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Accepted Manuscript
Sourdough volatile compounds and their contribution to bread: a review
Cécile Pétel, Bernard Onno, Carole Prost
PII: S0924-2244(16)30275-8
DOI: 10.1016/j.tifs.2016.10.015
Reference: TIFS 1900
To appear in: Trends in Food Science & Technology
Received Date: 29 June 2016

Revised Date: 27 October 2016
Accepted Date: 27 October 2016
Please cite this article as: Pétel, C., Onno, B., Prost, C., Sourdough volatile compounds and
their contribution to bread: a review, Trends in Food Science & Technology (2016), doi: 10.1016/
j.tifs.2016.10.015.
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1 Sourdough volatile compounds and their contribution to bread: a review
2 Cécile Pétel1,2, Bernard Onno2, Carole Prost1*

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3 Flavor team, Matrix and Food, Process/properties – Structure/sensory, UMR CNRS 6144 GEPEA, Oniris, LUNAM university,
4 Nantes, France
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5 Food and Industrial Microbiology Laboratory, Oniris, Nantes, France
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7 corresponding author: Carole Prost, mail: carole.prost@oniris-nantes.fr, tel: +33 (0)2 51 78
8 55 17, fax: +33 (0)2 51 78 55 20
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10 Abstract
11 Background
12 Sourdough has been used in bread production for decades to improve its preservation,
13 texture and flavor. Today it is mostly used as a bread flavor improver. For many years, bread
14 volatile compounds have been referenced and more than 540 have now been reported. In
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15 contrast, sourdough volatile compounds have been less studied. No listing of these
16 compounds has been previously carried out and their origins have not been reported in a
17 review.
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18 Scope and Approach
19 The scope of this review is to detail the volatile compounds previously reported in sourdough
20 and sourdough bread in order to highlight the most common ones. Methods for studying
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21 volatiles in sourdough and sourdough bread are first listed. Then the volatile compounds
22 identified from previous papers about sourdough aroma are characterized to understand their
23 origins and their contribution to bread aroma.
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24 Key Findings and Conclusions
25 According to this review, the main extraction technique applied to sourdough and sourdough
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bread is headspace solid-phase micro-extraction. To date, 196 volatile compounds have
been reported in sourdough and sourdough bread including 43 aldehydes, 35 alcohols, 33
28 esters, 19 ketones, 14 acids, 13 furans, 11 pyrazines, 2 lactones, 2 sulfurs, 21 others and
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29 alkanes. The most recent characteristics of most of these volatile compounds (origins, odors
30 and odor thresholds) are reported as well as their presence in sourdough, sourdough bread
31 or bread. This report underlines the production levers that could modify sourdough and bread
32 aroma.
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33 Key words (6)

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34 Sourdough; sourdough bread; volatile compounds; bread; origin; extraction
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36
37 1. Introduction
38 Sourdough is a mixture of flour and water that is fermented using yeast and lactic acid
39 bacteria (LAB). Sourdough has been used in bread production for dough leavening (Roussel
40 & Chiron, 2002), but it also extends shelf life, improves nutritional properties, increases
41 bioactive compound contents and makes bread flavor better (Banu, Vasilean, & Aprodu,
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42 2011; De Vuyst et al., 2013; Gänzle & Gobbetti, 2013). Today, sourdough is mainly used as
43 an aroma improver and to confer typicality on wheat and rye breads. Flavor, as a
44 combination of smell and taste, is undoubtedly the most important attribute determining
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45 consumption (Hansen & Schieberle, 2005). Smell is characterized by volatile compounds
46 with different olfactory characteristics while taste is due to aromatic and sapid compounds.
47 Volatile compounds have been extensively studied in bread products and more than 540
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48 volatiles have been reported in different papers (Quilez et al., 2006; Pico et al., 2015).
49 Reviews on bread aroma have previously been published by Cho & Peterson (2010), Grosch
50 & Schieberle (1991, 1997), Maga (1974, 1978), Pico et al. (2015), Pozo-Bayon et al. (2006),
51 Rothe (1974) and Schieberle (1996). In contrast, sourdough has generally been studied in
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52 terms of its microflora diversity or its textural and sensory effects on bread (Charmaine et al.,
53 2005; Chavan & Chavan, 2011; Corsetti & Settanni, 2007; De Vuyst & Neyssens, 2005).
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Sourdough volatile compounds have been less studied than those of bread and no recent
review has included the diversity of volatiles in sourdough or sourdough bread (SD-bread).
56 To our knowledge, the latest review on sourdough aroma was published by Hansen and
57 Schieberle in 2005. Therefore, the aim of this paper is to review sourdough volatile
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58 compounds, including their possible origins, odor, and contribution to bread aroma, as well
59 as the most recent methods for studying them.
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61 Sourdough is a complex ecosystem in which lactic acid bacteria (LAB) and yeast interact
62 together and with the ingredients depending on the process parameters (Zotta, Piraino,
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63 Ricciardi, McSweeney, & Parente, 2006). In addition to flour and water, some extra
64 ingredients can be added to boost the microflora fermentation such as sugar or enzymes.
65 Depending on the proportion of these ingredients and on the bread process parameters
66 (fermentation and baking), SD-bread has a specific volatile profile. The proportion of
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67 sourdough added in SD-bread is a major factor influencing the bread volatile profile.
68 Spontaneous and inoculated sourdough can also be distinguished. In spontaneous
69 sourdough, fermentation is due to wild flour microflora, which is well adapted to this
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70 ecosystem and evolves during fermentation, while in inoculated sourdough selected starters
71 are added to the mixture. The spontaneous sourdoughs are generally specific to a region
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72 because LAB and yeast species depend on ecological factors (De Vuyst & Neysens, 2005).
73 In spontaneous sourdoughs, alcohols from yeast fermentation occur in greater
74 concentrations compared to those in inoculated sourdoughs (Hansen & Lund, 1987).
75 Temperature, time and the number of backsloppings influence the yeast and lactic acid
76 bacteria (LAB) fermentations and lipid oxidation and hence the volatile profile of sourdough.
77 Clearly, the sourdough volatile profile influences that of SD-bread and thus its sensory
78 properties. In recent sourdough development, it has been dried to obtain a specific aroma
79 (Brandt et al., 2006). Many factors impact the sensory properties of sourdough bread. The
80 effects on volatile compounds and the sensory profile variation of sourdough and SD-bread
81 production parameters are described in Figure 1.
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82 Figure 1 – Sourdough and sourdough-bread volatile compounds: variations in parameters
83 The evaluation of the volatile compound profile requires the extraction, identification and
84 quantification of the compounds. To explain the sensory evaluation, gas-chromatography-
85 olfactometry (GC-O) (also named “GC-sniffing”) is generally used to identify volatile
86 compound odors. These results are then compared to sensory evaluation to understand the
87 impact of all the parameters on bread sensory properties.
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88 The objectives of this review are: to name all the volatile compounds reported in wheat
89 sourdough, rye sourdough and sourdough breads, to list their origin and to understand the
90 variation levers in their processing. The volatile compound extraction methods used for
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91 sourdough and SD-bread evaluation and the associated identification and quantification
92 methods are also listed and compared. This approach is descriptive and also aimed to
93 identify the origin of the volatile compounds. Lastly, the impacts of these volatile compounds
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94 on SD-bread aroma and its sensory characteristics are described.
95 2. Methods for studying volatiles in sourdough and sourdough bread
96 Table 1 – Extraction methods used for sourdough and bread analysis and the parameters
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97 used for HS-SPME when relevant.
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Preliminary isolation remains an essential step in such extraction procedures despite rapid
developments in measurement techniques. Depending on the study objectives, different
100 extraction methods are used. Each one has some advantages and some limitations and
101 extracts preferentially one kind of volatile. According to 28 studies on bread, SD-bread and
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102 sourdough (Table 1), 3 major extraction methods are used: solvent extraction, purge and
103 trap, and headspace solid-phase microextraction.
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104 2.1. Extraction methods based on solvent affinity
105 The first extraction methods were vacuum distillation and solvent extraction. In this kind of
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106 method, solvents are used to extract volatile compounds from the matrix (Grosch, 2007;
107 Prost et al., 2012). This method is based on the diffusion of volatiles from the food matrix to
108 the solvent and thus the extracted volatiles have a high affinity for the solvent used. This
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109 method enables the extraction of a large variety of volatile compounds (Side, Robards &
110 Helliwell, 2000) but has some limitations. Firstly, the solvent can limit the identification of
111 volatile compounds and secondly, solvent elimination requires a heating process that can
112 lead to thermal decomposition artifacts (Side et al., 2000). Solvent extraction has notably
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113 been used for the extraction of bread volatiles by Frasse et al. (1992), Schieberle & Grosch
114 (1993), Gassenmeier & Schieberle (1995) and Zehentbauer & Grosch (1998) and for
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115 sourdoughs by Hansen et al. (1989) and Hansen & Hansen (1994). Today, solvent extraction
116 methods are less used due to their constraints and limitations.
117 2.2. Extraction methods based on compound volatility
118 Headspace extraction methods have been developed to avoid the drawbacks of the solvent
119 method. In this case, the gaseous phase above the product is collected and hence the
120 volatile compounds collected are more likely to represent the odor perceived by the
121 consumer (Grosch, 2007; Prost et al., 2012). Although headspace samples are generally
122 cleaner, they contain fewer compounds than those obtained by solvent extraction (Side et al.,
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123 2000). These solvent-free methods also enable volatile compound odors to be studied
124 directly. Dynamic and static methods are available.
125 In static extraction, the sample is placed in a hermetic vial until equilibrium is obtained in the
126 headspace. Then the headspace is collected and analyzed. The principal limitations of static
127 extraction are its lack of sensitivity and the collection of only the most volatile and major
128 compounds (Galey et al., 1994; Side et al., 2000). In dynamic extraction, the volatiles are
129 continually sent to the headspace through gaseous flow and are then collected and
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130 analyzed. This method is more sensitive than static methods.
131 Dynamic extraction collects a large variety of volatile compounds (Prost et al., 2012). For
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132 example, the purge and trap method involves passing an inert gas through the sample and
133 collecting the stripped volatile constituents in a trap. The equilibrium between the food and
134 headspace is constantly removed resulting in improved sensitivity (Side et al., 2000). This
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135 method was used by Gobbetti et al. (1995) and Damiani et al. (1996) for wheat sourdough
136 analysis and by Heinio et al. (2003) for rye samples. Birch et al. (2013) used dynamic
137 headspace extraction for wheat bread analysis.
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138 Lastly, headspace solid phase microextraction (HS-SPME) has become the most common
139 method for food products as it is simple and easy to use. It is also more sensitive than
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conventional static extraction for volatile and semi-volatile compounds (Side et al., 2000). For
HS-SPME, the sample is placed in a hermetic vial with shaking. Then, an SPME fiber
constituted of a very thin polymer coating on which volatile compounds will be absorbed is
143 inserted. The absorbance capacity differs according to the polarity and thickness of the fiber
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144 coating. Two kinds of method are used. The first is an immersive method in which the fiber is
145 inserted into the liquid sample. In the second method, named headspace solid phase
146 microextraction (HS-SPME), the fiber is inserted above the sample. Equilibrium is reached
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147 faster in HS-SPME than in immersion SPME (Side et al., 2000). The HS-SPME method is
148 sensitive and selective according to its coating and semi-quantitative. Achieving good
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149 reproducibility, selectivity and sensitivity with HS-SPME requires careful method
150 development.
151 2.3. Headspace solid-phase micro-extraction: parameter selection and optimization

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152 Many parameters are interrelated and the performance of this method depends not only on
153 individual variables but also on their combined effects (Stashenko & Martinez, 2007). The
154 dependent parameters are: sample preparation, equilibrium time, equilibrium temperature,
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155 extraction time, extraction temperature and fiber coating. These notably depend on the
156 studied matrix (Grosch, 2007; Kataoka et al., 2000; Prost et al., 2012) and the sample
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157 preparation (Side et al., 2000).
158 HS-SPME has been widely used for sourdough and bread analysis (Aponte et al., 2013;
159 Guerzoni et al., 2007; Kaaseleth et al., 2011; Ravyst & De Vuyst, 2011; Rizzello et al., 2010;
160 Settanni et al., 2013). However each study used its own parameters.
161 Regarding sourdough analysis, sample preparation is always different. Sometimes the
162 sourdough is diluted (Ravyst & De Vuyst, 2011; Aponte et al., 2013), sometimes it is not, and
163 sourdough quantity and vial size also vary between the referenced studies.
164 With regard to the fiber, the majority of the studies use a DVB/Car/PDMS fiber (Alfonzo et al.,
165 2013; Guerzoni et al., 2007; Montanari et al., 2014; Plessas et al., 2011; Ravyst & De Vuyst,
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166 2011; Ripari et al., 2016; Rizello et al., 2010; Settanni et al., 2013; Ventimiglia et al., 2015;
167 Vernocchi et al., 2008) but the coating thickness differs in each case: 65 µm (Guerzoni,
168 Vernocchi, Ndagijimana, Gianotti, & Lanciotti, 2007) and 50/30 µm (Plessas et al., 2008;
169 Rizzello, Nionelli, Coda, De Angelis, & Gobbetti, 2010). Others use Car/PDMS (Aponte et al.,
170 2013; Kaseleht, Paalme, Mihhalevski, & Sarand, 2011) with an 85 µm coating.
171 Equilibrium and extraction are generally carried out between 24 and 60°C and from 10 min to
172 1 h. During heating, Maillard compounds may be generated. However, the equilibrium phase
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173 is not always mentioned, thus some studies could have been carried out before equilibrium
174 was reached (Alfonzo et al., 2013; Aponte et al., 2013; Maire et al., 2013; Pacynski et al.,
175 2015; Plessas et al., 2008; Plessas et al., 2011; Quilez et al., 2006; Raffo et al., 2015; Ravyst
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176 & De Vuyst, 2011; Ripari et al., 2016; Settanni et al., 2013; Ventimiglia et al., 2015; Wu et al.,
177 2012).
178 From this comparison, HS-SPME seems to be the most convenient method to extract
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179 volatiles from bread products. Nevertheless, as sourdough is not directly consumed, the
180 number of studies about its volatile composition is limited and no parameter optimization has
181 been done for sourdough HS-SPME extraction. Bread HS-SPME parameters have been
182 optimized twice (Poinot et al., 2008; Raffo et al., 2015). However, even with optimization, the
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183 parameters may differ as illustrated by Poinot et al. (2008), who wanted to obtain a
184 representative odorant extract of bread, and Raffo et al. (2015), who wanted to extract the
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highest number of volatile compounds in bread. These studies selected different fibers:
Car/PDMS 75 µm (Poinot et al., 2008) and DVB/Car/PDMS 50/30 mm (Raffo et al., 2015),
187 and different extraction parameters: 5 min equilibrium plus 30 min extraction at 35°C for
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188 Poinot et al. (2008) and 60 min extraction at 50°C for Raffo et al. (2015). Moreover, some
189 publications mention the evaluation of rye and sourdough bread according to the same
190 extraction parameters (Aponte et al., 2013; Ravyst & De Vuyst, 2011). However, these
191 authors do not indicate if they checked that their HS-SPME parameters were adapted for
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192 both products. It is possible that the results differ depending on the sourdough used (wheat,
193 rye or other flour). On one hand, it can be assumed that optimization is required for each kind
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194 of sourdough and each objective. On the other hand, parameter optimization could limit the
195 comparison of the results. Thus, optimization of parameters requires some compromise to
196 obtain the best parameters for most sourdoughs while a first standardization could simplify
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197 the comparison of studies.
198 2.4. Extracted volatile compound analysis
199 Regarding the analysis of extracted volatile compounds, there is a consensus. This step is
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200 systematically performed with GC-MS with a polar column for sourdough volatiles extracted
201 through headspace methods. However, authors rarely indicate if they have reported all
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202 compounds or only a selection. Usually they mention volatiles according to their content
203 (peak area) or only odorous volatile compounds (Table 1). Hence, as differences occur
204 between studies, the comparison of their results is distorted. According to Table 1, the
205 number of volatile compounds reported in sourdough is always lower than in bread. These
206 differences may result from (i) different extraction methods since volatile compounds are
207 generally extracted according to their affinity for the extraction solvent or coating, (ii) the
208 selection of volatile compounds reported by the authors or (iii) a real difference in volatile
209 compounds between both products.
210 2.5. Conclusion about volatile compound extraction techniques
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211 To conclude about the volatile compound extraction and analysis methods, this review
212 underlines the need to develop a standardized representative method of extraction for
213 sourdough and bread volatiles and to define the selection criteria for reported volatile
214 compounds. These details would enable different studies to be compared and sourdough
215 and bread volatile profiles to be precisely defined. HS-SPME seems to be the most
216 convenient method to develop a standardized extraction method for sourdough studies. First,
217 it is a simple and inexpensive method and secondly, it has already been optimized for bread
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218 and so could presumably be optimized for sourdough. With regard to the parameters, some
219 points must be checked such as the extraction temperature, which should not generate a
220 Maillard reaction, and the equilibrium time, which must be sufficient to obtain volatile
221 compound partition in the headspace. However, each cited parameter has its own impact
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222 and thus its own importance for extraction, and should be optimized. Thus, it must be
223 underlined that it is probably impossible to generate only one method for all sourdoughs.
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224 3. Volatile compounds in sourdough
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226 3.1. Volatile compound diversity
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227 Publications about sourdough volatile compounds are incomplete. No global review has
228 previously been published reporting all the volatile compounds cited in sourdough.
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93 volatile compounds have been identified in wheat or rye sourdoughs and in wheat
sourdough or rye sourdough breads. Their classification by chemical group, their CAS
231 number and their characteristics are given in Table 2. Table 2 also reports whether the
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232 volatile compound has been identified in wheat sourdough, rye sourdough, wheat sourdough
233 bread, rye sourdough bread or in several, as well as in wheat bread.
234 Table 2 – Volatile compounds reported in sourdough and sourdough-bread aroma with their
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235 main associated characteristics.

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236 Table 3 – Occurrence of major volatile compounds in Sourdough (SD), Sourdough Bread
237 (SD-B) or Non-Sourdough Bread (Non SD-B) based on Table 2 and taking into account
238 volatile compounds reported by at least 3 authors at the sourdough step.
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239 According to our review, 98 and 71 volatile compounds have been reported in wheat and rye
240 sourdoughs, respectively (Table 2). The most reported volatile compounds (cited in more
241 than 3 papers (Table 3)) in both wheat and rye sourdoughs are hexanal, nonanal, 1-
242 pentanol, 1.4-butanediol, 6-methyl-5-hepten-2-one and octyl acetate. Some volatile
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243 compounds are more reported in rye sourdough than in wheat sourdough, such as 2-
244 methylbutanal, 3-methylbutanal, 1-hexanol, 2-pentanone and 2-acetylfuran. One volatile
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245 compound is only reported in rye sourdough (1-octanol). In contrast, 13 volatile compounds
246 are more cited in wheat sourdough than in rye sourdough (benzaldehyde, ethanol, 1-
247 propanol, 2-methylpentanol, 2-propen-1-ol, phenol, 2-methylbutanol, 2-octanone, formic acid,
248 octanoic acid, methyl acetate, 2-phenylethyl acetate) while only γ-nonalactone is specific to
249 wheat sourdough. Investigating the amount of volatile compounds in rye sourdoughs,
250 Kaseleth et al. (2011) and Lund et al. (1988), described ethanol, isoalcohols, hexanol, acetic
251 acid, hexanoic acid, dimethyltrisulfide, ethyl acetate, ethyl lactate, ethyl hexanoate,
252 pentanone and 2.3-butanedione as the main volatile compounds. However, they also
253 demonstrated that these results depended on the inoculated microflora and on the water
254 content in sourdough. This kind of result is limited because very few publications include the
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255 amount of volatile compounds. It would be interesting to obtain more numerical data to
256 complete this study and to understand the role of microflora, process parameters and
257 ingredients.
258 Moreover, Table 2 reports 82 and 68 volatile compounds in wheat and rye sourdough
259 breads, respectively. The most reported volatile compounds (cited in more than 3 papers) in
260 both these breads are 3-methylbutanal, 1-pentanol and 1.4-butanediol. Several volatile
261 compounds are more cited in rye SD-bread (hexanal, phenylacetaldehyde, (E)-2-octenal,
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262 methional, (E)-2-nonenal, (E,E)-2.4-decadienal, (Z)-2-nonenal, 6-methyl-5-hepten-2-one, 3-
263 hydroxy-2-butanone) while 3 volatile compounds are specific to rye SD-bread ((E,Z)-2,6-
264 nonadienal, 4-(Z)-heptenal, 1-nonanol). Only ethanol is specific to wheat SD-bread while 1-
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265 propanol and formic acid are more cited in wheat SD-bread than in rye SD-bread. Among the
266 common major volatile compounds, 1-pentanol and 1.4-butanediol are reported in both
267 sourdoughs and SD-breads (wheat and rye). 1-propanol and formic acid are more cited in
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268 wheat sourdough and wheat SD-bread than in rye products. Hansen et al. (1988) found that
269 2-propanone, 3-methylbutanol, benzyl alcohol, 2-phenylethanol, 2- and 3-methylbutanol and
270 2-methylpropanol are the major volatile compounds in wheat SD-breads in terms of
271 concentration. However, they underlined that the content of each volatile compound depends
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272 on the inoculated microflora. Investigating the major volatile compounds in rye SD-breads,
273 Hansen & Hansen (1996) determined that the amounts of ethanol, 2- and 3-methylbutanol, 2-
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phenylethanol, acetic acid, 2-methylpropanoic acid and 3-methylbutanoic acid are higher in
rye SD-breads than in bread, but these characteristics depend on the LAB and yeasts used.
276 The specificity of sourdoughs seems to be hidden in the corresponding breads. However, as
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277 the extracted volatile compounds depend on the methods and the products used, this
278 comparison is only descriptive. Moreover, none of these differences can be attributed to one
279 route of volatile formation because of the complexity of the latter. By modifying the
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280 microflora, not only the fermentative volatiles are modified, but also the precursors of lipid
281 oxidation and the Maillard reaction, and the same can be observed with the use of rye flour
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282 instead of wheat flour. This complexity makes understanding sourdough aroma formation
283 more difficult and points out the need for more precise analysis of each route throughout the
284 sourdough and bread process.
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285 By comparison, wheat bread contains 144 volatile compounds, significantly more than those
286 found in sourdough or SD-bread. However, bread aroma has been much more studied than
287 sourdough or SD-bread and thus the number of publications dealing with bread volatile
288 compounds is higher than those for sourdough. This difference probably explains the higher
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289 number of reported volatile compounds. According to the literature, sourdough and especially
290 SD-bread should have more volatile compounds than bread, or at least higher volatile
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291 contents (Hansen & Hansen, 1996; Plessas et al., 2008). It is known that only a small part of
292 bread volatile compounds has an impact on bread aroma, which is also probably the case for
293 sourdough. This impact mainly depends on the content and the perception threshold of
294 volatile compounds. Perception thresholds in water are reported in Table 2 for volatile
295 compounds that are referenced in Leffingwell et al. (online). However, this value depends on
296 the matrix and is therefore just an indication of the relative importance of each volatile
297 compound. GC-O analysis enables the detection of volatile compound odor and also, by
298 following the AEDA method, the detection of its perception threshold (Grosh & Schieberle,
299 1987). This method has been much more used for bread evaluation than for sourdoughs.
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300 Thus, the odor characterization is specified in Table 2 as an illustration but will not be
301 commented on further.
302 3.2. Main origins of volatile compounds
303 Figure 2 - Sourdough and sourdough-bread: major origins and main influential factors
304 Odorants are generated in sourdough mainly due to enzymatic and microbial processes
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305 during sourdough fermentation. These compounds belong to different chemical classes such
306 as aldehydes, acids, alcohols, ketones, esters and pyrazines, which are the most cited.
307 However, some compounds are already present in the flour. Bread and sourdough volatile
308 compounds originate in the same ways (Figure 2) from raw materials or processes. Those
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309 brought by raw materials are negligible compared to the total volatile compound content
310 (Kirchoff & Schieberle, 2002) and thus are not mentioned in this part. Other compounds are
311 mainly due to the fermentation process, lipid oxidation and Maillard and caramelization
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312 reactions (Drapon & Richard-Molard, 1979; Pozo-Bayon et al., 2006; Prost et al., 2012). In
313 sourdough, lactic acid bacteria (LAB) and yeast fermentations are the major routes of volatile
314 compound production. Moreover, no pyrazine has been reported in wheat or rye sourdoughs,
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315 which indicates the limitation of the Maillard reaction in sourdough.
316 The 3 major routes of volatile compound formation are briefly described below and the
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volatile compounds generated are listed. It is often difficult to establish a link between a given
compound and a single-generation pathway, as the same compound can originate from
319 several pathways. In the following sections, some compounds are reported in one or more
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320 paragraphs or its origin is denominated as “unknown”.
321 3.2.1. From fermentation processes

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322 Figure 3 – Simplified contribution of sourdough microbiota to volatile compound generation
323 Fermentation is the major route for volatile formation in sourdough and bread crumb. It
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324 produces mainly acids, alcohols, aldehydes, esters and ketones (Pico et al., 2015) (Figure
325 2). Yeast and LAB fermentations can be distinguished. They differ from metabolic and kinetic
326 ways and lead to the formation of specific volatile compounds (Figure 3). Competition
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327 between yeast and LAB also has an impact on volatile compound production (Hansen &
328 Schieberle, 2005). Moreover, homofermentative and heterofermentative LAB can be
329 distinguished. The former can convert hexoses almost completely into lactic acid whereas
330 heterofermentative LAB degrade hexoses into lactic acid, acetic acid, ethanol and CO2
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331 (Hansen & Schieberle, 2005). LAB also liberate aroma precursors such as free amino acids,
332 which are degraded into aldehydes or into the corresponding alcohols (Hansen & Schieberle,
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333 2005). To be more specific, monosaccharides are used for glycolysis and form pyruvic acid,
334 which is the basis of LAB and yeast fermentations. From pyruvic acid, several compounds
335 are generated such as lactic acid, propanoic acid, propanol, ethyl lactate, ethanol, acetic
336 acid, 2.3-butanedione, 2-butanone or butanol. Then the generated volatile compounds
337 depend on the microflora. For example, LAB produce hexanoic acid (goat), hexanol (floral),
338 pentanol (sweet), 2- and 3-methylbutanol (malty), 2-pentylfuran (fruity) and dimethylsulfide
339 (sulfurous), whereas yeasts produce more ethanol and isoalcohols (Gobbetti et al., 1995,
340 Damiani et al., 1996). In addition, while LAB fermentation requires more than 12 h to produce
341 a sufficient amount of volatiles, this is achieved in a few hours with yeast fermentation
342 (Chavan & Chavan, 2011; Hansen & Schieberle, 2005).
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343 [For details concerning fermentation routes, please refer to Drapon & Richard-Molard
344 (1979), Kaseleth et al. (2011) and Prost et al. (2012) for yeast fermentation and to Gänzle et
345 al. (2007), Prost et al. (2012), Schieberle (1996) and Vermeulen (2006) for LAB
346 fermentation.]
347 Yeasts are naturally present in sourdough or are added (mainly S. cerevisiae in bread
348 products) and contribute to developing the dough and generating volatile compounds. CO2
349 and ethanol are the main outcomes of yeast fermentation. However, the ethanol content is
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350 strain-dependent (Hansen & Hansen, 1994). The LAB starter type modifies the variety and
351 quantity of volatiles, but acetic acid is the major volatile compound resulting from LAB
352 fermentation (Hansen & Hansen, 1994). Heterofermentative LAB fermentation generates
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353 mainly ethyl acetate, hexyl acetate, ethyl hexanoate and isopentyl acetate, while
354 homofermentative fermentation produces 2,3-butanedione (butter-like), acetaldehyde
355 (aldehydic) and 2- and 3-methylbutanol (fruity) (Gerekovà et al., 2011). The largest difference
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356 is in 3-methylbutanol content, which varies mainly according to species and strains (Settanni
357 et al., 2013).
358 As seen in Table 2, 36 volatile compounds from LAB and yeast fermentation are common to
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359 wheat and rye sourdoughs. Among these, hexanal (green), acetaldehyde, hexanoic acid
360 (fatty), 1-hexanol (ethereal), 1-pentanol (oil), 2- and 3-methylbutanol, 2-pentylfuran (fruity)
361
362
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and dimethylsulfide (sulfurous) are due to LAB fermentation (Gobbetti et al., 1995; Kaseleth
et al., 2011). 2,3-butanedione is mainly due to homofermentative LAB (Damiani et al., 1996),
363 while acetic acid and ester production is specific to heterofermentative LAB (ethyl acetate,
364 ethyl lactate (caramel-like), ethyl octanoate (fruity), ethyl hexanoate (fruity), 3-methylbutyl
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365 acetate (fruity), 2-methylbutyl acetate (overripe fruit)) and their content depends on the LAB
366 species but not their diversity, which is linked to the metabolism (Hansen & Lund, 1989;
367 Damiani et al., 1996; Kaseleth et al., 2011). These compounds, and mostly acetic acid,
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368 confer sourdough specific aroma characteristics. Some volatile compounds are only due to
369 some specific LAB such as benzaldehyde (almond-like), which is only reported for Lb.
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370 helveticus (Kaseleth et al., 2011), or 2-heptenal (sour), which is produced by Lb. plantarum
371 and Lb. farciminis (Damiani et al., 1996). In contrast, the same volatile compounds can be
372 produced by homo- and heterofermentative LAB, but their content differs. For example, the
373 reduction of aldehydes occurs more in hetero- than in homofermentative species (Kaseleth et
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374 al., 2011).
375 Yeasts produce ethanol, aldehydes, iso-alcohols and ethyl acetate and are therefore mainly
376 responsible for ethanol (alcohol), 2-methyl-1-propanol (ethereal), 3-methylbutanol (alcohol),
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377 2-phenylethanol (rose), 2-methylbutanol (roasted), aldehyde (acetaldehyde, hexanal,

378 octanal, nonanal…), 3-hydroxy-2-butanone (sweet), benzyl alcohol (floral) or octanoic acid
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379 (fatty) production (Damiani et al., 1996; Hansen & Schieberle, 2005; Pozo-Bayon, 2006).
380 Some other volatile compounds are due to amino acid conversion by yeast such as
381 benzaldehyde (almond-like) and 2-phenylethanol (rose) (from phenylalanine), methional
382 (potato) (from methionine), 2-methylpropanal (aldehydic) (from valine), 2-methylbutanal
383 (musty) and 2-methylbutanoic acid (acidic) (from isoleucine), 3-methylbutanal (ethereal) and
384 2-methylbutanoic acid (acidic) (from leucine), 2,3-butanedione (from asparagines) or acetic
385 acid (vinegar) (from asparagines, glycine, serine or alanine) (Maga, 1974).
386 Nevertheless, wheat and rye sourdoughs do not share all their volatile compounds. In wheat
387 sourdough, 16 additional volatile compounds of fermentation origin are reported (Table 2):
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388 decanal (sweet), octanal (floral), 3-methylhexanal (sweet), 2-methylpentanol, 1-nonanol

389 (fresh), 2-hexanol (chemical), 6-methyl-5-hepten-2-one (citrus), butanoic acid (sharp),
390 pentanoic acid (stinky), 2-furanmethanol (alcohol), ethyl benzoate (fruity), 2-phenylethyl
391 acetate (floral), ethyl decanoate (sweet), methyl salicylate (mint), γ-butyrolactone (creamy)
392 and γ-nonalactone (coconut). As shown in Table 2, 2-methylbutanal (musty) is more often
393 reported in rye sourdough (Heiniö et al., 2003; Lund, Hansen & Lewis, 1989; Kaseleth et al.,
394 2011) than in wheat sourdough (Damiani et al., 1996) while phenylacetaldehyde (green) is
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395 only found in rye sourdough bread (Cho & Peterson, 2010; Schieberle & Grosch, 1994;
396 Schierbele, 1996) and less often in wheat sourdough bread (Pozo-Bayon, 2006). According
397 to Pozo-Bayon (2006), rye flour is an important source of 2-methylbutanal and
398 phenylacetaldehyde. Both of these compounds are reported in bread (Birch et al., 2013; Cho
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399 & Peterson, 2010; Poinot et al., 2007; Pozo-Bayon et al., 2006; Gassenmeier & Schieberle,
400 1995; Raffo et al., 2015; Pico et al., 2015; Zehentbauer & Grosch, 1998). Finally, 2-
401 methylpropanal (aldehydic), 2-butanone (acetone) and 2-methylpropanoic acid (sweet) are
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402 specific to rye sourdough and are also due to fermentation. The mechanism of the flour type
403 effect varies and could be (i) direct by cereal-specific volatile compounds, (ii) indirect by input
404 of precursors, or (iii) indirect by increasing microflora activity and metabolite content.
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405 This first part indicates that both microflora and flour have a strong impact on the volatile
406 profiles of sourdough and SD-bread, conferring multiple aromas specific to the generated
407
408
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volatile compounds and thus to the microflora, but these are not the only parameters. The
impact of sourdough microflora on aroma depends on multiple factors. First, the type and
409 content of volatiles from fermentation depend on the microflora used (Gobbetti et al., 1995).
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410 As briefly shown above, there are differences between homofermentative and
411 heterofermentative LAB, according to the strain and species. These can be observed on one
412 volatile compound or on a chemical class (Damiani et al., 1996). For example,
413 heterofermentative LAB produce mainly acetic acid and ethanol but they also produce
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414 specific esters and reduce aldehydes to the corresponding alcohols (Kaseleht et al., 2011).
415 Moreover, non-specific differences between heterofermentative species have been detected.
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416 In contrast, more diversity is observed between homofermentative species. In addition, the
417 sourdough volatile profile is more balanced with the association of heterofermentative and
418 homofermentative LAB. Fermentation with LAB produces more esters than with yeast
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419 (Plessas et al., 2008). Moreover, the association of yeast and LAB modifies the volatile
420 profile of sourdough by increasing volatiles due to yeast fermentation and decreasing the
421 content of LAB volatile compounds (Damiani et al., 1996). Other factors are due to process
422 parameters. According to the rise in fermentation temperature, LAB and then yeasts are
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423 favored up to 35°C (Gobbetti et al., 1995). The fermentation time can also change the volatile
424 profile: under 3 h of fermentation, yeasts are in the majority in sourdough then the iso-
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425 alcohols dominate; between 5 and 9 h of fermentation, the total volatile content increases
426 and is stable for 24 h. After 24 h of fermentation, Gobbetti et al. (1995) observed a decrease
427 in volatile content. Finally, the flour ash content modifies microflora activity and notably the
428 content of organic acids (acetic acid and lactic acid) (Hansen & Hansen, 1994). Besides its
429 impact on organic acid content, the flour ash content modifies the content of volatile
430 compounds but this effect depends on the microflora used. Hansen and Hansen (1994)
431 demonstrated that the flour type had a significant effect on the production of ethyl acetate
432 and ethanol in sourdoughs fermented with heterofermentative cultures but there is more
433 often a higher content of alcohols with high-grade flour.
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434 This short presentation of the parameters of sourdough volatile content variation underlines
435 the complexity of this ecosystem. In fact, the fermentative compounds produced depend on
436 numerous parameters, which undergo multiple interactions (Figures 1 and 3).
437 3.3. From lipid oxidation
438 Lipid oxidation begins during mixing but the presence of active enzymes, such as
439 lipoxygenase, in the raw material as well as air incorporated during beating can induce early
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440 oxidation (Maire et al., 2013). Moreover, lipid oxidation can be influenced by the addition of
441 fatty ingredients and the kind of fatty matter in the recipe. It is due to lipoxygenase action
442 during kneading and storage. This enzyme oxidizes polyunsaturated fatty acids into free
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443 radicals, peroxides and hydroperoxides (Drapon & Richard-Molard, 1979; Galey et al., 1994),
444 which are then converted into volatile compounds during baking. In sourdough and bread
445 crumb, lipid oxidation mainly leads to aldehydes ((E)-2-octenal, hexanal, heptanal, octanal,
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446 nonanal, 2-heptenal…), ketones (2-octanone…), alcohols and esters depending on the initial
447 fatty acid (Birch et al., 2013; Maire et al., 2013; Drapon & Richard-Molard, 1979; Martinez-
448 Anaya, 1996).
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449 [For more information about lipid oxidation in baked products, please refer to Frankel, 1991]
450 11 volatile compounds from lipid oxidation are reported in wheat and rye sourdoughs (Table
451
452
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2): hexanal (green), acetaldehyde (aldehydic), benzaldehyde (almond-like), nonanal
(aldehydic), (E)-2-octenal (fresh), (E)-2-heptenal (sour), (E)-2-nonenal (fatty), 1-pentanol
453 (oil), 1-hexanol (ethereal), 1-heptanol (musty), 1-octen-3-ol (mushroom), and 2-pentylfuran
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454 (fruity) while 5 volatile compounds are only cited in wheat sourdough (decanal, octanal,
455 (E,E)-2,4-decadienal, (Z)-2-nonenal, γ-nonalactone) and 2 only in rye sourdough (1-penten-
456 3-ol, 2-butanone). These differences are probably mainly due to the recipe and the process
457 used.
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458 Lipid oxidation is significantly reduced during sourdough fermentation (Czerny & Schieberle,
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459 2002; Gänzle et al., 2007) and some LAB can convert some lipid oxidation compounds into
460 their corresponding alcohols (Vermeulen et al., 2013). For example, 3-methylbutanoic acid is
461 derived from the oxidation of 3-methybutanal by aldehyde dehydrogenase (Guerzoni et al.,
462 2007).
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463 Lipid oxidation is not specific to the sourdough or bread process, but it modifies volatile
464 compound formation by changing the amount of precursors and generating new volatile
465 compounds. Thus, it is necessary to control lipid oxidation through the ingredients, mixing
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466 parameters and storage conditions to monitor the volatile profiles of sourdough and SD-
467 bread.
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468 3.4. From the Maillard reaction
469 Volatile compounds created during baking (bread) or drying (sourdough) depend directly on
470 the dough precursors: sugar and amino acids. Bread crust color and the roasted aroma are
471 due to these Maillard compounds (Drapon & Richard-Molard, 1979). The Maillard reaction is
472 mainly due to temperature; hence the number of Maillard compounds in sourdough is very
473 low. Only 3 volatile compounds are found in wheat and rye sourdoughs (2-methylbutanal, 3-
474 methylbutanal and 2,3-butanedione) while Heiniö et al. (2003) reported only furfural in rye
475 sourdough (Table 2). However, 2- and 3-methylbutanal and 2,3-butanedione can also be
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476 derived from LAB and yeast fermentation. Therefore, the Maillard reaction will not be fully
477 described in this paper.
478 [For details of the Maillard reaction, please refer to Nursten, 2005]
479 More sugary ingredients could promote Maillard reactions and the corresponding pleasant
480 volatile compounds would be developed. LAB activity also has an impact on the Maillard
481 reaction as they liberate amino acids as precursors for this reaction and decrease dough pH
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482 (El Dash, 1971). However, in sourdough, the drying process is the most efficient way to
483 create more Maillard compounds. Yet, dried sourdough is inactive and cannot confer the
484 “sourdough bread” denomination. Moreover, this kind of sourdough is not described in this
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485 paper because only one publication deals with its aroma (Brandt et al., 2006).
486 3.5. Impact of ingredients and processes
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487 To influence sourdough aroma, ingredients and parameters have to be controlled. By
488 studying volatile compounds, their origins and the complexity of interactions between
489 ingredients, process and volatile compound production routes are underlined.
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490 The volatile profile depends on sourdough ingredients and processes such as pH,
491 fermentation temperature, enzyme addition and selected starters (Damiani et al., 1996;
492
493
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Gobbetti et al., 1995; Johnson & Sanchez, 1973; Plessas et al., 2011). As seen in Table 2,
wheat and rye sourdoughs have different aromatic profiles with only 43 similar volatile
494 compounds. Hence flour has an impact on the aromatic profile. According to the cereal and
495 ash content of flour, different types and contents of nutrients and precursors are available
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496 (Gobbetti et al., 1995). Sourdough with an elevated ash content is characterized by a higher
497 total concentration of volatile compounds (Gobbetti et al., 1995). In wheat flour, the increase
498 in ash content and a dough yield between 135 and 175 increase the volatile content
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499 (Gobbetti et al., 1995). Moreover, the addition of fructose or citrate can modify the sourdough
500 volatile profile or content as well as the bread volatile profile (Gobbetti et al., 1995). The
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501 amount of free amino acids also increases during sourdough fermentation (Hansen, Lund, &
502 Lewis, 1989). However, more publications deal with wheat sourdoughs than with rye
503 sourdoughs, which could partly explain this difference.
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504 In bread, the addition of fatty ingredients can contribute to a major production of desirable
505 carbonyl compounds during baking as well as an increase in aroma compounds from lipid
506 oxidation (Pozo-Bayon, 2006). However, fatty ingredients with sugary ingredients increase
507 the quantity of 5-hydroxymethyl-furfural, which exhibits an undesirable smell (Pozo-Bayon,
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508 2006).
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509 This brief evaluation of the variation parameters shows the importance of monitoring all
510 production steps, from ingredients to final product, because there are many interactions
511 between each parameter. Thus, the control of the sourdough volatile profile is very complex.
512 Moreover, due to the diversity of aromas generated by each pathway, the interactions
513 between all volatile compounds, the matrix and the content of each volatile, it is very hard to
514 conclude precisely about the sensory effect of each pathway.
515 4. Impact of sourdough on bread

516
517 4.1. Bread aroma and sourdough impact: generalities
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518 The impact of sourdough on bread aroma depends on the proportion of sourdough in bread
519 dough (Plessas et al., 2008). Previous studies have shown that some volatile compound
520 contents in SD-bread are related to their concentrations in the corresponding sourdough
521 (Hansen & Schieberle, 2005) but are usually lower. This can be explained by the proportion
522 of sourdough in bread dough and by the impact of bread processes. Sourdough bread
523 volatile profiles are more complex with LAB fermentation than with yeast fermentation only,
524 notably for the ester content (Plessas et al., 2008). Moreover, the aromatic profile of wheat
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525 bread is simpler than that of wheat sourdough bread (Plessas et al., 2008), whose major
526 characteristic is the high content of acids. In sourdough bread, the contents of 2-
527 methylpropanol, 2-methylbutanol, 3-methylbutanol, ethyl acetate, and ethyl lactate are linked
528 to their contents in the corresponding sourdough (Hansen & Schieberle, 2005). However, as
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529 sourdough is generally added at less than 50% of the flour content and then goes through
530 the baking process, volatiles from sourdough are diluted. For example, from sourdough to
531 SD-bread, the majority of esters disappear (Hansen & Schieberle, 2005). By contrary the
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532 amount of volatile compounds which have different origins can increase during baking. For
533 example, the content of 3-methylbutanal increases (Hansen & Schieberle, 2005). This
534 increase in bread is probably due to the free amino acids (leucine) brought by sourdough into
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535 bread, which then contribute to the Maillard reaction during baking. Then as 3-methylbutanal
536 is also generated during baking process its amount is higher in bread compared with its
537
538
539
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amount in sourdough. In rye sourdough bread, heterofermentative cultures result in bread
with a higher content of acetic acid while homofermentative cultures in bread lead to a higher
content of iso-alcohols (Hansen, Lund, & Lewis, 1989). The sourdough rye bread crumb
540 generally has the highest content of 2-propanone, 3-methylbutanal, benzylalcohol and 2-
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541 phenylethanol (Hansen, Lund, & Lewis, 1989).
542 [For more information about bread aroma, please refer to Pozo-Bayon, Guichard & Cayot,
543 2006; Pico et al., 2015]
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544 In the next section (4.2), volatile compounds reported for sourdough and sourdough bread
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545 are compared to observe the evolution from sourdough to bread. Then the difference
546 between volatile compounds reported in wheat sourdough bread and wheat bread are
547 described in 4.3.
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548 4.2. Volatile compound evolution from sourdough to bread
549 82 volatile compounds have been reported for wheat sourdough bread (Table 2). By
550 comparison with wheat bread (without sourdough), 72 volatile compounds are common and
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551 thus probably due to the bread matrix (Table 2). By comparing wheat sourdough bread and
552 wheat bread (without sourdough), 10 volatile compounds seem to be specific to wheat
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553 sourdough bread ((E,E)-2.4-heptadienal, 4-nonenal, ethyl-2-methylpropanoate, 3-methylbutyl

554 acetate, indene, carvone, p-cymene, styrene, vanillin, estragole) but these were only
555 reported by Seitz et al. (1998). Thus, by considering the 2nd part of this review (2. Methods
556 for studying volatiles in sourdough and sourdough bread), this difference could only be due
557 to differences in volatile extraction or analysis. These will not be further investigated here.
558 However, sections 4.2.1. and 4.2.2. describe the differences between volatile compounds
559 reported for (i) wheat sourdough and wheat sourdough bread and (ii) rye sourdough and rye
560 sourdough bread.
561 4.2.1. From wheat sourdough to wheat sourdough bread
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562 51 volatile compounds are reported in wheat sourdough but not in wheat sourdough bread
563 (Table 2). Among these, there are 9 aldehydes, 15 alcohols, 3 acids, 16 esters, 1 lactone
564 and 5 ketones. More precisely, 17 are due to the fermentative process, such as 1-heptanol,
565 pentanoic acid and 2-phenylethyl acetate, 2 are due to lipid oxidation or fermentation (2-
566 methylpentanol, γ-nonalactone) and 1 is due to the Maillard reaction or fermentation (6-
567 methyl-5-hepten-2-one). The origins of the others, such as dodecanal, 2-
568 methylbenzaldehyde, (E,E)2,4-octadienal, (Z)2-hexen-1-ol, 1-octen-3-ol, 3-hydroxy-2-
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569 butanone or 3,5-octadien-2-one, are not reported in previous publications. These differences
570 underline the large role of fermentation in volatile production but also the modification of the
571 sourdough volatile profile notably through bread processes and volatile evaporation.
572 According to this result, it seems that most evaporated volatiles originate from fermentation.
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573 Alcohols and acids are the main chemical classes produced during fermentation and are the
574 most volatile compounds. The monitoring of sourdough volatile compounds throughout all
575 sourdough and sourdough bread processes could be helpful to understand all the
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576 implications of these processes and to indicate the key parameters to control in order to
577 guide the volatile and thus sensory profile of SD-bread.
578 4.2.2. From rye sourdough to rye sourdough bread
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579 Focusing on rye products, 39 volatiles are reported in rye sourdough but not in rye bread
580
581
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(Table 2) with 15 aldehydes, 7 alcohols, 3 acids, 4 esters, 4 ketones, 4 furans and 2 sulfurs.
The main origins of these compounds are fermentation for 7 volatile compounds such as
582 pentanal, 2-phenylethanol, 2-octanone or octanoic acid, lipid oxidation for 2 compounds (1-
583 heptanol, and 1-octanol), and 1 compound is from the Maillard reaction (propanal). Other
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584 compounds are due to fermentation or lipid oxidation as for the 6 volatile compounds
585 (benzaldehyde, heptanal, or 2-butanone), from fermentation or the Maillard reaction (2-
586 methylpropanal) or may due to all 3 ways such as acetaldehyde. However, the origin of 21
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587 volatiles is not known.

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588 4.2.3. Impact of the recipe on volatile compounds
589 According to the comparisons of wheat sourdough with wheat sourdough bread and rye
590 sourdough with rye sourdough bread, volatiles from fermentation are the main variation
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591 factors between these products. However, there are some differences between wheat and
592 rye products: alcohols and esters are more described in wheat products whereas aldehydes,
593 furans and sulfurs are more cited in rye products.
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594 4.3. Differences in volatile compounds between wheat sourdough bread and bread
595 By comparison with wheat bread, wheat sourdough bread contains almost the same volatiles
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596 but at higher contents (Hansen & Hansen, 1996). In sourdough bread, ethanol is mainly
597 evaporated. However, 10 volatile compounds are reported in SD-bread but not in wheat
598 bread (Table 2): (E,E)-2,4-heptadienal, 4-nonenal, 2-ethylhexyl acetate, acetonyl acetate,
599 indene, carvone, styrene, 1,4-dichlorobenzene, estragole, 1-phellandrene. The origin of all of
600 these compounds is unknown. Nevertheless, these compounds are only cited by Seitz et al.
601 (1998), and could be due to experimentation artifacts. According to Table 3, all the main
602 volatile compounds found in sourdoughs are also found in bread. As these compounds are
603 not specific to LAB fermentation, this result is not surprising.
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604 Only a relatively small proportion of volatile compounds seem to have an impact on the final
605 aroma of bread or bread products (Grosch & Schieberle, 1997; Pozo-Bayon et al., 2006).
606 The study of odorants in sourdough and SD-bread could underline the modification of the
607 potent odorants from sourdough in bread and determine which volatile compounds are
608 responsible for SD-bread aroma. This kind of study would help understand the real role of
609 sourdough addition in bread aroma.
610 Sourdough is used to confer a specific aroma to bread crumb thanks to volatile profile
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611 modification and sourness through acetic acid. The flavor of SD-bread is richer and more
612 aromatic than in bread, which can be attributed to the long fermentation time of sourdough
613 (Clarke & Arendt, 2005). According to Hansen & Schieberle (2005), sourdough bread has a
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614 higher content of volatiles and achieves a higher score in sensory tests compared to bread
615 chemically acidified with lactic and acetic acids. Moreover, Callejo (2011) lists 22 odor
616 attributes divided into 14 odor classes for bread, 4 of which are specific to SD-bread
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617 (“wheaty”, “dark beer”, “butter-like”, “toasted grain”), and 43 for taste and aroma divided into
618 32 flavor classes for bread while SD-breads have 35 additional attributes (divided into 24
619 classes), 4 of which are common with ordinary bread (“wheat”, “astringent”, “sweety”, “yeast”)
620 (Callejo, 2011). According to this study, the sourdough sensory impact has already been
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621 highlighted and described. However, the SD-bread characteristics mainly depend on
622 sourdough production parameters such as ash content, fermentation temperature, microbiota
623
624
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and sourdough yield (Katina, 2005). However, as underlined by Callejo (2011), the lack of a
universal vocabulary for bread flavor description limits the comparison of sensory study
625 results and most studies deal with the taste of SD-bread more than its odor. Thus, the
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626 contribution of sourdough to bread aroma could be further examined and linked with the
627 qualitative and quantitative profiles of volatiles to understand the real impact of sourdough on
628 bread.
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629 5. Future aspects

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630 The first requirement in sourdough volatile compound analysis is to select and optimize one
631 extraction method in order to standardize studies. This will enable study results and
632 conclusions to be compared. However, each sourdough has its own volatile profile. Thus, the
633 optimization of the extraction method would probably not be the same for all sourdoughs if
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634 the objective is to obtain an extract representative of sourdough odor. Nevertheless, if the
635 objective is to extract the highest number of volatile compounds then this homogenization is
636 possible. This constraint is due to the numerous parameters that must be optimized in the
637 case of the HS-SPME technique (temperature, fiber, duration) and the diversity of sourdough
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638 product volatile profiles. Moreover, if the objective is to compare sourdough and SD-bread
639 then the methodology would be optimized for only one product (sourdough or bread) but
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640 applied to both in order to compare them. This constraint is due to the differences between
641 bread and sourdoughs in terms of structure, volatile compounds and preparation. This
642 standardization is thus a crucial issue in the comparison of sourdough and bread volatile
643 profiles.
644 In addition, considering the increasing use of dried sourdough in bread, more studies should
645 pay attention to dried sourdough and its advantages. Numerous precursors of the Maillard
646 reaction are generated during the liquid sourdough process, which may create new flavors
647 during the drying process. An analysis and understanding of the production of dried
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648 sourdough volatile compounds and their impact on bread would clarify its interest in the
649 bread industry.
650 To go further, the parameters that guide the volatile profile of sourdough and sourdough
651 bread need to be determined, taking into account all the interactions between parameters
652 (microflora, flour, fermentation parameters, etc.). This kind of study requires the monitoring of
653 volatile compounds from ingredients to final sourdough bread with a standardized extraction
654 method for all these steps.
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655 Despite the knowledge accumulated regarding the biological reactions (microbial, enzymatic)
656 during cereal fermentation, and the link between metabolite production at this level and the
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657 final product aroma, integrating all the parameter effects and their interactions is still a
658 challenge for research in order to identify clearly the levers to direct the sensory properties of
659 the final product. The complete explanation of the contribution of volatiles to odor and aroma
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660 requires some recombination or association analysis. Moreover, interactions between volatile
661 and sapid compounds and with texture need to be studied to define the impact of sourdough
662 on bread flavor.
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664 Acknowledgement
665 Cécile Petel would like to thank Soufflet Biotechnologies (Nogent sur Seine, France) for her
666 PhD contract which led to this review, and especially Dr J. Rouille and Dr M. Nlandu-Mputu
667 for their supervision during it.
668
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669 References
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672 of wheat flours. Food Microbiology 36, 343-354.
673 Aponte, M., Boscaino, F., Sorrentino, A., Coppola, R., Masi, P., and Romano, A. (2013).
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674 Volatile compounds and bacterial community dynamics of chestnut-flour-based sourdoughs.
675 Food Chemistry, 141(3), 2394–2404.
676 Banu I., Vasilean I. and Aprodu I. (2011). Effect of select parameters of the sourdough rye
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677 fermentation on the activity of some mixed starter culture. Food Biotechnology, 25, 275-291.
678 Birch, A. N., Petersen, M. A., and Hansen, Å. S. (2013). The aroma profile of wheat bread
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684 validation process of a sensory panel for bread analysis: Influence of cultivar on the quality of
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686 Chavan, R. S., and Chavan, S. R. (2011). Sourdough Technology-A Traditional Way for
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689 Cho, H., Peterson, D. G. (2010). Chemistry of bread aroma: A review. Food Science and
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691 Clarke I. C. and Arendt E. K. (2005). A review of the application of sourdough technology to
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824 application to analysis of volatiles in foods. Trends in Analytical Chemistry, 19(5), 322-329.
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827 235-242.
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831 and cereal enzymes to the generation of amino acids in dough relevant for bread flavor.
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842 Science, 56(2), 127–133. http://doi.org/10.1016/j.jcs.2012.03.007

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843 Zehentbauer, G., Grosch, W. (1998). Crust aroma of baguettes. I. Key odorants of baguettes
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847 2574.
848
849
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850 Figure Captions
851 Figure 1 – Sourdough and sourdough-bread volatile compounds: variations in parameters
852 Figure 2 – Sourdough and sourdough-bread: major origins and main influential factors
853 Figure 3 – Simplified contribution of sourdough microbiota to volatile compound generation
Table 1 – Extraction methods used for sourdough and bread analysis and the parameters
PT
854
855 used for HS-SPME when relevant.
856 Table 2 – Volatile compounds reported in sourdough and sourdough-bread aroma with their
RI
857 main associated characteristics.
858 Table 3 - Occurrence of major volatile compounds in Sourdough (SD), Sourdough Bread
859 (SD-B) or Non-Sourdough Bread (Non SD B) based on Table 2 and taking into account
SC
860 volatile compounds reported by at least 3 authors at the sourdough step (Numbers
861 correspond to the number of publications mentioning the volatile compounds).
862
U
AN
M
D
TE
C EP
AC
23
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Table 1 – Extraction methods used for sourdough and bread analysis and parameters used for HS-SPME when it is relevant (in grey : sourdoughs)
Number of described Volatiles

Extraction Analyze technique compounds and selection criterion
Authors Year Product Sample preparation HS-SPME Parameters
technique (column polarity) Sourdo
Bread Selection criterion
ugh
Vacuum desorption and Solvent
Major peak or
extraction (dichloromethane)
Frasse et al. 1992 Wheat bread bread crumb ND GC-MS (apolar) - 25
PT
sufficiently resolved
Schieberle P. Rye sourdough HRGC-MS , HRGC-O

1993 bread crumb or crust ND - 28 Odorant (8<FD<512)
RI
& Grosch W. bread (polar and apolar)
Gassenmeier
HRGC-MS (polar and
K. & 1995 Wheat bread bread crumb ND - 20 FD≥8
SC
apolar)
Schieberle P.
Zehentbauer
1998 HRGC-MS , HRGC-O
G. & Grosch Baguette bread crumb or crust ND - 47 -
(a,b) (polar and apolar)
U
W.
AN
Purge and Trap and
solvent extraction
50 g rye sourdough +
Sourdough rye
Hansen et al. 1989 50 mL water + 1 mL 4- ND GC-MS (polar) - 53 -
bread crumb
methyl-1*pentanol
M
Hansen A. &
D
1994 Wheat sourdough No details ND GC-MS (polar) 19 - -
Hansen B.
Gobbetti et al. 1995

TE
190g homogeneized
Wheat sourdough 40g of ice + 60 mL of ND
HRGC-MS (non
10 -
High match quality
polar) ≥5 times of noise
Purge and Trap Injector
distilled water
190g homogeneized High match quality
EP
HRGC-MS (non
Damiani et al. 1996 Wheat sourdough 40g of ice + 60 mL of ND 25 -
polar) ≥3 times of noise
distilled water
0.5 g extruded rye
C
samples + 49.5ml 30%

sodium chloride
AC
Heinio et al. 2003 Rye samples solution equilibrated ND GC-MS (polar) - 27 Odorous
overnight at room
temperature in vials
sealed with a septum
15 g frozen bread Equilibrium : 10 min 40 °C
DHE
2013
Birch et al. Wheat bread crumb in pieces in 500 Purge : Nitrogen 5 min and 60 GC-MS (polar) - 46 -
(a,b)
mL glasses min
HS
SP
M
Quilez et al. 2006 Baguette 0,25 g of bread crumb SPME Fiber: Car/PDMS (75 GC-MS (polar) - 65 -
E
-
ACCEPTED MANUSCRIPT
powder +9,9 mL NaCl µm)

solution + 0,1 mL of
internal standard in 20 Equilibrium : non mentionned -
mL vial Extraction: 60 min 50 °C -
SPME Fiber: DVB/Car/PDMS
-
3 g sourdough or (65 µm)
PT
Guerzoni et al. 2007 Wheat sourdough culture media in 10 mL Equilibrium : 10 min 60°C GC-MS (polar) 52 - -
vial
Extraction: 20 min -
RI
(2 cm, 50/30 mm)
Sourdough wheat 2 g of sourdough-bread
Plessas et al. 2008 Equilibrium : non mentionned GC-MS (polar) - 32 -
bread in 20 mL vial
SC
Extraction: 60 min 60 °C
SPME Fiber: Car/PDMS (75
6 g of homogenised µm)
U
Poinot et al. 2008 Wheat bread crushed bread in 125 Equilibrium : 5 min 35°C GC-MS (polar) - 46 Optimisation
mL vial
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(65 µm)
Vernocchi et 3 g sourdough in 10
2008 Wheat sourdough GC-MS (polar) 19 - -
M
al. mL vial Equilibrium : 10 min 60°C
Extraction: 20 min
D
(50/30 µm)
Wheat germ 10 g sourdough in 50
Rizzello et al. 2010 TE Equilibrium : 30 min 40°C GC-MS (polar)
sourdough mL vial
SPME Fiber:
EP
DVB/Car/PDMS (2 cm, 50/30
Kefir sourdough 2 g of sourdough-bread mm)
Plessas et al. 2011 GC-MS (polar) - 38 -
bread in 20 mL vial Equilibrium : non mentionned
C
AC
Ravyts E. & Wheat and rye 5 g sourdough + 1g

2011 Equilibrium : non mentionned GC-MS (polar) 17 - ≥3 times of noise
Devuyst L. sourdough NaCl solution
SPME Fiber: 75µm
Chinese DVB/Car/PDMS
5 g of bread in 15 mL
Wu et al. 2012 sourdough Equilibrium : non mentionned GC-MS (polar) - 77 -
vial
steamed bread
ACCEPTED MANUSCRIPT

Sterile flour
Alfonzo et al. 2013 extract fermented 5 mL SFE Equilibrium : non mentionned GC-MS (polar) 18 - Identified
by LAB
SPME Fiber: Car/PDMS (85
Wheat, rice, 2 g of sourdough + 2
µm)
buckwheat, mL of distilled water +
PT
Aponte et al. 2013 Equilibrium : non mentionned GC-MS (polar) 59 - -
maize, chesnut 5 µL 4-methyl-2-
flour sourdough pentnol in 20mL vial Extraction: 30 min 40 °C
RI
(1 cm, 75 µm)
3 g of sample in 15 mL
Maire et al. 2013 Cake Equilibrium : non mentionned GC-MS (polar) - 70 Optimisation
vial
SC
(50/30 mm)
U
Settanni et al. 2013 Wheat sourdough 5 g of sourdough Equilibrium : non mentionned GC-MS (polar) 51 - -
AN
Extraction: 40 min 60°C
(50/30 mm)
Montanari et Pandoro 3 g sourdough in 10 Identified with
2014 GC-MS (polar) 26 30
M
al. sourdough mL vial Equilibrium : 10 min 47°C concentration >0.1%
Extraction: 40 min
D
0,25 g of bread powder
(50/30 mm)
(slice or crust) + 5 mL
Raffo et al. 2015 Wheat bread TE Equilibrium : non mentionned GC-MS (polar) - 134 -
of internal standard
solution in 15 mL vial Extraction: 60 min 50°C
SPME Fiber: Car/PDMS
GC-MS (polar and
EP
3 g of powder bread
Pacynski et al. 2015 Gluten-free bread Equilibrium : non mentionned apolar) GC*GC- - 77 -
(crust or crumb)
TOFMS
C

(50/30 mm)
Ventimiglia et
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2015 Wheat sourdough 5 g of sourdough Equilibrium : non mentionned GC-MS (polar) 31 - -

al.
(50/30 mm)
2 g of sourdough in 5
Ripari et al. 2016 Sourdough Equilibrium : non mentionned GC-MS (non polar) 54 - -
mL vial
ACCEPTED MANUSCRIPT
Table 2 – Volatile compounds reported in sourdough and sourdough-bread aroma with their main associated characteristics.
Origins Reported for…
Perception threshold in water (ppb) β
PT
Also found in Wheat bread

Sourdough (SD) SD-breads
(without sourdough)
Maillard reaction
Lipid oxidation
Fermentative
RI
SD and SD-Bread
N°C A S Odour (from littérature) α
Volatile compounds
SC
wheat rye others wheat rye
U
AN
Aldehydes
Fresh, Green, Fatty, Aldehydic, Grass,
Hexanal 66 25 1 4,5-5 b,d,g b,e,g,q - d,s,t,w m,k,l,s a o,q j,q,u b,p,q,r,z,n
M
Leafy, Fruity, Sweaty
Acetaldehyde 75 07 0 Pungent, Ethereal, Aldehydic, Fruity 15-120 d d q d,t l a o - q,n
D
Fresh, Aldehydic, Floral, Green, Overipe
2-Methylpropanal 78 84 2 0,1-2,3 d - z - l a q - p,q,r,z,n
fruit, Fruity, Roasted, Malty
2-Methylbutanal 96 17 3
TE
Musty, Cocoa, Coffee, Nut, Malty, Fruity,
1 d - q,x,z d m,k,l - q j,q q,r,z,n
Sweet, Roasted
Almond, Strong, Sharp, Sweet, Bitter, 350-
EP
Benzaldehyde 100 52 7 b,d,g,h b,g,h - d,h,y,t,w m,l a i,o - b,p,r,n
Cherry 3500
2-Propenal 107 02 8 Fruity, Almond, Cherry - - - - - l - - - n
C
Pentanal 110 62 3 Fermented, Bread, Fruity, Nutty, Berry 12-42 e - - - K - q - q,n

Fresh, Aldehydic, Fatty, Green, Burgundy,
AC
Heptanal 111 71 7 3 d b,e,n - d l a o,q - b,r,n

Ozone, Grass
Sweet, Aldehydic, Waxy, Fat, Soap, Zeste

Decanal 112 31 2 0,1-2 b,y b - y,t - - q - b,n
d'orange, Citrus, Floral
Soapy, Waxy, Aldehydic, Citrus, Green,

Dodecanal 112 54 9 - - - - w - - - - n
Floral
Green, Sweet, Floral, Hyancinth, Cocoa, b,c,q,f,r,z,
Phenylacetaldehyde 122 78 1 4 b - b - - - q c,u,v
Fatty, Waxy n
ACCEPTED MANUSCRIPT
Earthy, Alcohol, Wine, Whiskey, Cocoa,

Propanal 123 38 6 9,5-37 - - q - l - - - q,n
Nutty
Butanal 123 72 8 Acre, Cacao, Moisi, Vert, Malté, Pain 9-37,3 - - - - K - - - q,n
Melon, Grass, Floral, Orange, Fatty, Green,
Octanal 124 13 0 0,7 b,d,g b,g - d,t - - q - b,r,n
Citrus, Waxy, Aldehydic,
PT
Aldehydic, Rose, Waxy, Citrus, Orange,
Nonanal 124 19 6 1 d b,g - d,s,t,w m,l,s a o,q j b,q,z,n
Floral
RI
2-Methylbenzaldehyde 529 20 4 Fruity - - - - w - - - - -
(E,Z)-2,6-Nonadienal 557 48 2 Green, Fat, Cucumber, Violet, Leafy 0,01 - - - - - - c,q,u c,q,r,z,n
SC
Ethereal, Aldehydic, Chocolate, Peach,
c,j,q,u b,c,p,q,f,r,
3-Methylbutanal 590 86 3 Fatty, Sour, Roasted Bread, Fruity, 0,2-2 b - b,x,z d m,k,l,s a o,q,v
,v z,n
Fermented, Corn flakes
U
Pungent, Green, Ethareal, Sharp
2-Methyl-2-butenal 1115 11 3 - - - - - K - - - n
penetrating, Nutty, Anisic
AN
Pungent, Green, Fruity, Apple, Orange,
(E)-2-Pentenal 1576 87 0 - - - - - l - - - -
Tomato
M
2-Undecenal 2463 77 6 Fresh, Fruity, Orange peel - - - - t - - - - n
Fresh, Cucumber, Green, Fat, Waxy, Leafy,
D
(E)-2-Octenal 2548 87 0 Grass, Banana, Sweet, Nutty, Roasted, 3 - e,g,n - t,w l - q c,q,u q,n
Cereal
Pentadecanal 2765 11 9 Fresh, Waxy
TE - - - - w - - - - -
c,q,u,
Methional 3268 49 3 Potatoe, Musty, Earthy, Vegetable 0,2 - - x,z - - - q,v c,q,f,r,z,n
v
EP
2-Butenal 4170 30 3 Floral - - - - - m - - - q,r

Fatty, Green, Oil, Aldehydic, Cake,
(E,E)-2,4-Heptadienal 4313 03 5 - - - - - m - q - -
Cinamon
C
(E,E)-2,4-Nonadienal 5910 87 2 Fatty, Nutty, Violet, Leafy, Waxy, Fried 0,09 - - t - - q q,u c,q,r,z,n
AC
Green, Banana, Aldehydic, Fatty, Cheesy,

(E)-2-Hexenal 6728 26 3 17 - - - t l - q - r,n
Soap
Oil, Fatty, Green, Dairy product, Milky,
4-(Z)-Heptenal 6728 31 0 0,8-10 - - - l - - c,q,u c,q,z,n
Creamy,
(E,Z)-2,4-Nonadienal 6750 03 4 Fatty, Green, Cucumber, Honey 0,09 - - - - - - - q,u c,q,z,n
ACCEPTED MANUSCRIPT
1048 Fresh, Clean, Aldehydic, Soapy, Citrus,

Tridecanal 19 8 - - - - w - - - - -
6 Petal, Waxy, Grapefruit peel
1882
(E)-2-Heptenal 55 5 Sour, Green, Vegetable, Fresh, Fatty 13 d n - h,w l - q - q,n
9
1882 c,q,u, b,c,q,f,r,z,
(E)-2-Nonenal 56 6 Fatty, Green, Aldehydic, Citrus 0,08-0,1 - b,q,x z y,w l - q,v
9 v n
PT
1926
3-Methylhexanal 28 4 Sweet, Green - d - - d - - - - -
9
2515
RI
(E,Z)-2,4-Decadienal 83 4 Fatty, Fried, Geranium, Green, Waxy - x - - - - - q,u c,q,r,z,n
2
2515 Oil, Cucumber, Melon, Citrus, Pumpkin, c,q,u,
(E,E)-2,4-Decadienal 84 5 0,007 - e,x z s,w - - q,v c,q,r,z,n
2 Nutty, Meat, Fried v
SC
3036
(E,E)-2,4-octadienal 28 5 Green, Fatty, Reminiscent of pear, Melon - - - - t - - - - -
1
3742
U
4-Nonenal 42 0 - - - - - - - q - -
3
5726
AN
(Z)-2-Heptenal 86 1 13 d n - d,t m - - - -
6
6078
(Z)-2-Nonenal 31 8 Iris, Fatty, Waxy, Cucumber, Metallic 0,08-0,1 - x - y - - v c,q,u c,q,z,n
4
M
1344
4,5-Epoxy-(E)-2-decenal 31 2 Citrus, Metallic, Green, Aldehydic, Fatty - - - - - - - v q,u q,f,r,z,n
54
p-Phtalaldehyde Unknown - - - - w - - - - -
D
iso-Phtalaldehyde Unknown - - - - w - - - - -
Alcohols
2-Phenylethanol 60 12
TE
8 Floral, Fade rose, Rose, Rose water, Honey
750-
e,q - - y,w - a - - n
1100
b,p,q,f,r,z,
EP
Ethanol 64 17 5 Strong, Alcohol, Ethereal, Medicinal 100000 b,g,x - - y,s,t,w s a i,o,q,v -
n
1-Propanol 71 23 8 Alcohol, Fermented, Musty, Fusel 9000 p p - h,i,t,w m,l a i,o,q j,q b,p,q,r,n
1-Butanol 71 36 3 Oil, Sweet, Balsamine 500 - - - d m a i j b,p,q,r,n
C
1-Pentanol 71 41 0 Oil, Sweet, Balsamine, Chemical mint 4000 b,h b,h,q - h,t,w m,k,l a b,i,q b,j,q b,p,r,n
AC
2-Methyl-1-propanol 78 83 1 Ethereal, Winey, Alcohol 7000 b,h,q - - h m a i j b,q,r,n

Benzyl alcool 100 51 6 Floral, Rose, Phenolic, Vinegar, Balsamine 10000 o - - d,h m,l a i,o j b,p,q,r,n
2-Ethylhexanol 104 76 7 Citrus, Fresh, Floral, Oily, Sweet - - - - w - - i,o - q,n
2-Methylpentanol 105 30 6 - b,d,g,h b,g,h - d,h,y,t,w m,l a i,o j b,p,q,r,n
2-Propen-1-ol 107 18 6 Alliaceous, Pungent, Mustard - b,d,g,h b,g - d,h,y,t,w m - - - b,q,n
Phenol 108 95 2 Phenol, Plastic, Rubber - b,d - - d,y,t,w m a o - b,q,r,n
1,4-Butanediol 110 63 4 - b,d,g,h, - - d,h,y,s,t,w m,k,l,s a i,o,v j,q,u p,q,r,n
ACCEPTED MANUSCRIPT
Ethereal, Oil, Alcohol, Green, Fruity, b,d,e,g,

1-Hexanol 111 27 3 2500 b - d,h m,k,l - i,q j p,q,r,n
Sweet, Woody, Floral h,x
Musty, Leaf, Woody, Peony, Violet, Grass,
1-Heptanol 111 70 6 3 - b - - - - q - p,q,n
Sweet
PT
Waxy, Green, Orange, Aldehydic, Rose,
1-Octanol 111 87 5 110-130 - b - - m,k,l a - j b,q,n
Mushroom, Citrus
RI
1-Dodecanol 112 53 8 Earthy, Soap, Waxy, Fat, Honey, Coconut - h - - h - - - - n
Oil, Alcohol, Fruity, Banana, Whiskey,
3-Methylbutanol 123 51 3 250-300 h,q - - h m - - - n
SC
Almond, Sweet
2-Methylbutanol 137 32 6 Roasted, Wine, Onion, Fruity - b,e,g,q b,g - y,t,w l - - j b,p,q,r,n
Fresh, Clean, Fatty, Floral, Rose, Orange,
U
1-Nonanol 143 08 8 50 - - - - - - - c,q,u n
Dusty, Wet, Oily
AN
2,3-Butanediol 513 85 9 Fruity, Creamy, Butter - - - - y,w - - o - b,q,r,n
3-Hexenol 544 12 7 Green, Leaf 70 - - - d m - - - b,n
3-Methyl-2-buten-1-ol 556 82 1 Sweet, Fruity, Alcohol, Green, Lavander - - - - - - - - - b,q,n
M
Earthy, Mushroom, Herbal, Melon, Citrus,
3-Octanol 589 98 0 - - - - - l - - - -
Woody, Spicy, Minty
D
Sour, Raifort, Tropical fruits, Green,
1-Penten-3-ol 616 25 1 400 - - - - l a - - b,n
Vegetable
3-Hexanol 623 37
TE
0 Alcohol, Medicine, Ethereal - - - - - - a - - -
2-Hexanol 626 93 7 Chemical, Wine - d - - d - - - - -
EP
6-Methyl-5-hepten-2-ol 1569 60 4 Sweet, Oily, Green, Coriander - - - - t,w - - - - -
(Z)-2-Hexen-1-ol 2305 21 7 Fruity, Green, Leaf - - - - t - - - - -
Mushroom, Earthy, Green, Oil, Raw
C
1-Octen-3-ol 3391 86 4 1 - b - t,w - - - - n

chicken, Mustyssure
AC
2-Pentanol 6032 29 7 Mild, Green, Fusel oil, Fermented - - - - w - - - - q,n

Spicy, Clove, Smoky, Phenolic, Pepper,
4-Vinyl-2-methoxyphenol 7786 61 0 3 - - - w - - - - n
Woody, Metallic
2027
2-Pentenol 24 9 Green - - - - w - - - - -
3
2600
(Z)-2-Octen-1-ol 58 1 Sweet, Floral - - - - w - - - - -
1
(E)-2-Heptenol 3346 76 4 Fatty, Pungent, Plastic, Green - g - - t - - - - q,n
ACCEPTED MANUSCRIPT
7
5149
3-Nonen-1-ol 28 1 - - - - - - a - - -
4
Ketones
Solvent, Ethereal, Apple, Pear, Blue cheese,
2-Propanone 67 64 1 500000 - - - - q j,q q,n
PT
Fruity, Acrid
2-Butanone 78 93 3 Aceton, Ethereal, Fruity, Camphor, Sweet 50000 g g - - k,l - q - p,q,r,n
RI
3-Pentanone 96 22 0 Ethereal, Acetone - - - - - - a - - q,n
3-Octanone 106 68 3 Fresh, Herbal, Lavender, Sweet, Mushroom - - - - - k - - - -
SC
Sweet, Fruity, Ethereal, Wine, Banana,
2-Pentanone 107 87 9 70000 - - - t m,k,l a q j b,q,r,n
Woody
U
Fruity, Spicy, Sweet, Grass, Coconut, 140-
2-Heptanone 110 43 0 - - - t m,l - - - b,q,n
Woody, Cinamon, Soap 3000
AN
c,j,q,u b,c,p,q,f,r,
6-Methyl-5-hepten-2-one 110 93 0 Citrus, Green, Musty, Apple, Lemongrass - b,d,h - b,h d,h,s,t m,k,l,s a i,v
,v z,n
2-Octanone 111 13 7 Earthy, Grass, Woody, Soap 50 b - - y,s,t,w s a - j b,p,q,r,n
M
Balsam, Rose, Metallic, Powdery,
Benzophenone 119 61 9 - - - - - - - q - q
Geranium
D
Musty, Mildew, Earthy, Chemical, Nutty,
4-Methyl-3-penten-2-one 141 79 7 - - - - a q - p,q,r,z,n
Chocolate, Woody
2,3-Butanedione 431 03 8
TE
Strong, Butter, Sweet, Creamy, Sour,
2,3-6,5 b,g - q - - - q - q,n
Caramel
EP
Sweet, Butter, Creamy, Dairy product, c,q,u,
3-Hydroxy-2-butanone 513 86 0 800 b - - s,t - - q,v c,q,f,r,z,n
Caramel, Fat v
2,3-Octanedione 585 25 1 Dill, Cooked broccoli, Butter - - - - - - - - q,u -
C
Acrid, Sweet, Butter, Caramel, Creamy,

2,3-Pentanedione 600 14 6 - - - - - - - - q,u c,q,n
AC
Nut, Cheesy
Earthy, Blueberry, Hay, Mushroom, Spicy,
3-Octen-2-one 1669 44 9 - - - - y,w - - - - r
Grass, Sweet, Rose
1-Octen-3-one 4312 99 6 Grass, Mushroom, Earthy, Musty 0,005 - q - - k - - - -
2369 Woody, Sweet, Fruity, Earthy, Green,
(E)-beta-Damascenone 85 7 0,002 - - - w - - - - N
6 Floral, Spicy
3,5-Octadien-2-one 3828 27 4 Fruity, Fat, Mushroom - - - - t - - - - -
ACCEPTED MANUSCRIPT
4
6521
(Z)-1,5-Octadien-3-one 86 7 Earthy - y - - y - - - - r,n
3
Acids
Formic acid 64 18 6 Acrid, Vinegar, Formyl 450000 b,g - - y,s,t,w l,s a i,o,q q,v b,p,q,f,r,n
PT
Acetic acid 64 19 7 Sharp, Acrid, Vinegar, Sour - - - - - - - - - q,n
Benzoic acid 65 85 0 Faint balsam, Urine - - w - - q - q,n
RI
Propanoic acid 79 09 4 Acrid, Acidic, Cheesy, Vinegar, Rancid 20000 b,g - - - s a i q b,p,r,n
2-Methylpropanoic acid 79 31 2 Sweet, Cheesy 8100 - - - - - - q q,n
Sweet, Honey, Floral, Waxy, Sour,
SC
2-Phenylacetic acid 103 82 2 10000 - - - - - - q q,f,r,n
Honeysuckle, Civette, Chocolate
Sharp, Acetic, Cheesy, Butter, Fruity,

Butanoic acid 107 92 6 240 b,g - - t - - i q b,p,q,f,n
U
Sweet, Sour, Sweat, Parmesan
Stinky, Putrid, Acidic, Sweat, Rancid,
Pentanoic acid 109 52 4 3000 b,y - - y,w - - - q b,q,r,n
AN
Acrid
2-Methylbutanoic acid 116 53 0 Acidic, Cheesy, Dirty, Fermented - g - - s s - o - q,r,n
Octanoic acid 124 07 2 Fat, Waxy, Rancid, Vegetable, Cheesy 3000 b,g,y - - y,s,t,w l,s - o - b,p,q,r,n
M
Hexanoic acid 142 62 1 Sour, Fat, Sweat, Cheesy 3000 - - - - - - - q N
Dodecanoic acid 143 07 7 Fat, Coconut, Oil, Berry 10000 - - - s,w s - - - -
D
2-Ethylhexanoic acid 149 57 5 - - - - w - - - - N
Sour, Dirty foot, Cheesy, Sweat, Tropical
TE
3-Methylbutanoic acid 503 74 2 120-700 - g - - - - i,v q,v p,q,f,r,n
fruits
Furans
EP
5-Hydroxymethylfurfural 67 47 0 Fat, Musty, Waxy, Caramel - - - q - - - q q q,n
Alcohol, Chemical, Bread, Coffee, Musty,
2-Furanmethanol 98 00 0 - - - b - k a o,q c b,p,r,n
Sweet, Caramel, Burnt, Oil , Earthy
C
3000-
Furfural 98 01 1 Sweet, Woody, Almond, Bread, Rancid e,y - e,q y - a i - p,q,r,n
23000
AC
2-Methylfuran 534 22 5 Ethereal, Acetone, Chocolate - - - h - - - c,u p,r,n

5-Methylfurfural 620 02 0 Spicy, Caramel, Maple, Almond - - - q - - - - q -
3-Hydroxy-5-ethyl-4-
698 10 2 Sweet, Fruity, Maple, Caramel 0,00001 - - - - - q q p,q,r,z,n
methyl-2(5H)-furanone
3-Methylfuran 930 27 8 - - - - - - - - q,v q,f,r,n
ACCEPTED MANUSCRIPT
Sweet, Balsamine, Almond, Cocoa,

2-Acetylfuran 1192 62 7 10000 - b - h,t m,k,l a q j b,p,q,r,n
Caramel, Coffee, Burnt
2-Ethylfuran 3208 16 0 Sweet, Burnt, Earthyk Malty - - - - - k - - - R
4-Hydroxy-2,5-dimethyl- Sweet, Cotton, Candy, Caramel,
3658 77 3 - - - - - k - - - R
3(2H)-furanone Strawberry, Sugar
PT
2-Pentylfuran 3777 69 3 Fruity, Green, Earthy, Bean, Metallic 6 h - - - l - - - r,n
2-Butylfuran 4466 24 4 Sweet, Wine, Fruity, Spicy - - - - - k,l - - - p,q,r,n
RI
3-Furancarboxyaldehyde Unknown - - - - - - - q - r,n
Esters
SC
Ethereal, Sweet, Fruity, Solvent, Wine,
Methyl acetate 79 20 9 - h - - h,t,w m a i,q j N
Cognac, Rum
Ethyl benzaote 93 89 0 Fruity, Dried mushroom, Green - - - - - a - - q,n
U
Ethyl-2-methylpropanoate 97 62 1 Sweet, Ethereal, Fruity, Alcohol 0,1 - - - - - - q - -
AN
Ethyl lactate 97 64 3 Sharp, Butter, Caramel, Fruit pie, Green 14000 - - - - m,b - - - N
2-Ethyl-hexyl acetate 103 09 3 Earthy, Grass, Humus, Woody - - - - - - - q - N
Floral, Rose, Sweet, Honey, Fruity,
2-Phenylethyl acetate 103 45 7 - b,h,y - - h,y,t,w m a q j b,q,f,r,n
M
Tropical
Sweet, Fruity, Rum, Fruit juice, Grape,
Ethyl propanoate 105 37 3 10 y - - y - - - - N
Pineeapple
D
Ethyl butyrate 105 54 4 Sweet, Fruity, Tutti-frutti, Cognac - - - - t - a - - N
Ethyl heptanoate 106 30
TE
9 Fruity, Pineeapple, Cognac, Rum, Wine - y - - y,t - - - - N
Fruity, Wine, Waxy, Apricot, Pear brandy,
Ethyl octanoate 106 32 1 - b - - t,w k,s a - j b,q,n
Banana, Sweet, Soap, Fresh
EP
Methyl hexanoate 106 70 7 Fruity, Pineeapple, Ethereal 70-84 - - - - - a - - N

Propyl acetate 109 60 4 Solvent, Sweet, Fruity, Peach, Raspberry - b,h - - h,t m,l a i,q q b,q,n
C
Isobutyl acetate 110 19 0 Sweet, Fruity, Ethereal, Apple, Banana - - - - t - a - - N

Sweet, Waxy, Fruity, Apple, Grape,
AC
Ethyl decanoate 110 38 3 - - - - m - o j N

Brandy, Oil
Octyl acetate 112 14 1 Green, Earthy, Mushroom, Herbal, Waxy - b,d,g,h - - d,h,s,t m,k,l,s a i,o j b,p,q,r,n
Octyl formate 112 32 3 Fruity, Rose, Orange, Waxy, Cucumber - - - - - - a - - -
Methyl salicylate 119 36 8 Mint, Green - - - - - - a - - -
Fruity, Rose, Waxy, Rum, Wine, Natural,
Ethyl nonanoate 123 29 5 - - - - - - a - - -
Tropical
ACCEPTED MANUSCRIPT
Sweet, Fruity, Waxy, Banana, Pineeapple,

Ethyl hexanoate 123 66 0 1 - - - - - a o - N
Green
Butyl acetate 123 86 4 Ethereal, Solvent, Fruity, Banana 66 - - - t m,l - q - n
3-Methylbutyl acetate 123 92 2 Sweet, Fruity, Banana, Solvent 2 - - - - - - q - -
Phenylmethyl acetate 140 11 4 - h - - h m - - j n
PT
Ethyl acetate 141 78 6 Ethereal, Fruity, Sweet, Grass, Green 5-5000 - - - t l - - j -
Hexyl acetate 142 92 7 Fruity, Green, Apple, Banana, Sweet 2 - - - - m - - - -
RI
Sweet, Fruity, Green, Apple, Pineeapple,
Ethyl pentanoate 539 82 2 - - - - - m - - - n
Acidic, Green, Tropical
SC
Butyl propanoate 590 01 2 Sweet, Banana, Tutti-Frutti, Rum - - - - w - - - - -
Acetonyl acetate 592 20 1 Fruity, Butter, Dairy product, Nut - - - - t - - - - n
Ethyl 2-furoate 614 99 3 Fruity, Floral - - - - t - - - - -
U
2-Methylbutyl acetate 624 41 9 Overripe fruit, Sweet, Banana, Fruit juice 5 - - - t - - - - n
AN
Pentyl acetate 628 63 7 Ethereal, Fruity, Banana, Apple, Pear - - - - w - - - - -
n-Pentyl acetate 628 63 7 Ethereal, Banana, Fruity, Peach, Apple - - - - w - - - - n
Ethyl hexadecanoate 628 97 7 Waxy, Fruity, Creamy, Milky, Basalmic - b,g - - t - - - - b,q,n
M
5208
Ethyl 2-hydroxyhexanoate 55 1 Fruity, Green - y - - y - - - - -
9
Lactones
D
γ-Butyrolactone 96 48 0 Creamy, Oil, Fat, Caramel - y - - y,w - a o - q,n
γ-Nonalactone 104 61 0
Coconut, Sweet,
Creamy, Fruity
TE
Butter, Waxy, Oil,
- b b - y,t,w - - - - b,c,q,r,z,n
Pyrazines
EP
100-
2,6-Dimethylpyrazine 108 50 9 Chocolate, Roasted, Nut, Coffee - - - - - a - - q,r,n
9000
Nut, Cocoa, Roasted, Chocolate, Green, 60-
C
2-Methylpyrazine 109 08 0 - - - - a q - p,q,r,n

Peanut, Burnt 105000
AC
Nut, Peanut, Musty, Earthy, Cocoa, 800-

2,5-Dimethylpyrazine 123 32 0 - - - - - a - - p,q,r,n
Roasted, Medicinal, Grass, Woody 1800
1336
2-Ethyl-5-methylpyrazine 64 0 Coffee, Bean, Nut 100 - - - - - - c c,q,n
0
2,5-Dimethyl-3- 1336
65 1 Cocoa, Roasted, Potatoe, Nut - - - - - - - q,u r,n
ethylpyrazine 0
1392 Butter de Peanut, Nut, Musty, Fermented, 6000-
2-Ethylpyrazine 00 3 - - - - - - q,u q,r,z,n
5 Coffee, Roasted, Cocoa, Meat, Woody 22000
ACCEPTED MANUSCRIPT
2-Ethyl-3,5- 1392 Burnt, Almond, Nut, Coffee, Pop Corn,

07 0 1 - - - - - q - p,q,r,n
dimethylpyrazine 5 Sour, Hay, Cooked potatoe
1570 Nut,Peanut, Musty, Maize, Earthy, Bread,

2-Methyl-3-ethylpyrazine 23 0 130 - - - - - - c,u r,z,n
7 Roasted, Potatoe
2,3-Diethyl-5- 1813 Musty, Nut, Earthy, Roasted, Potatoe,
PT
04 0 - - - - - - q c,u q,n
methylpyrazine 8 Green
1813
Diethyl-methyl-pyrazine 05 1 Nut, Meat, Vegetable - - - - - - - - q q,z,n
RI
8
Musty, Roasted, Maize, Popcorn, Nut,
2204
Acetylpyrazine 25 2 Potatoe, Bread crust, Chocolate, Nut, 62 - - - - - - c n
SC
7
Coffee
Sulfurs
U
Sulfurous, Onion, Sweet corn, Vegetable,
Dimethyl sulfide 75 18 3 0,3-1 h - - - k,l - - - q,r,n
Cabbage, Tomato, Green, Radish
AN
Dimehtyl disulfide 624 92 0 Sulfurous, Vegetable, Cabbage, Onion 0,16-12 - - - - k,l - - - n
Others
M
Fresh, Camphor, Sweet, Green, Woody,
α-Pinene 80 56 8 6 - - - - - - q - n
Earthy
D
Phenolic, Smoky, Spicy, Medicine,
Guaïacol 90 05 1 3-21 - - - - - a - q -
Vanillin, Meat, Woody
Indene 95 13 6
TE - - - - - - - q - -
Carvone 99 49 0 Mint, Licorice 50 - - - - - - q - -
p-Cymene 99 87 6 Fresh, Citrus, Terpene, Woody, Spice - - - - - - - q - -
EP
Sweet, Balsamine, Floral, Plastic, Solvent,

Styrene 100 42 5 - - - - - - - q - -
Rubber
C
p-Cresol 106 44 5 Phenol, Narcissus, Animal, Mimosa - - - - - - - - q,v q,f,n

1,4-Dichlorobenzene 106 46 7 - - - - - - - q - n
AC
m-Cresol 108 39 4 Medicinal, Wood, Leather, Phenol - - - - - - a q - q,n

Vanilline 121 33 5 Sweet, Vanillin, Creamy, Chocolate 20-200 - - - - - - q - -
β-Myrcene 123 35 3 Pepper, Spicy, Balsamine, Terpen, Plastic 13-15 - - - - - - q - q
l-Limonene 138 86 3 Citrus, Grass, Terpene, Camphor 10 - - - - - - q - n
Sweet, Sassafras, Anise, Spicy, Grass,
Estragole 140 67 0 - - - - - - - q - -
Fennel
ACCEPTED MANUSCRIPT
L-Borneol 464 45 9 Pine, Wood, Camphor - - - - - - - - v -

Nitrohexane 646 14 0 - - - - - - a - - -
Sabinene 3387 41 5 Woody, Terpen, Citrus, Pine, Spicy - - - - - - a - - -
1-Phellandrene 4221 98 1 Terpene, Medicine - - - - - - a - - -
2372 Apple, Rose, Honey, Tobacco, Sweet,
PT
(E)-Damascenone 93 4 - - - - t - - - - n
6 Boiled potate
8521
2-Acetyl-1-pyrroline 22 5 Nut, Roasted ham, Sweet - v - v - - - - q c,q,f,r,z,n
RI
3
Diethylphtalate Unknown - - - - w - - - - -
Methylnaphtalene Unknown - - - - w - - - - -
SC
Alkans - - - - d,y - - - - q,n
U
(a) Aponte et al., 2013 ; (b) Birch et al, 2013; (c) Cho et Peterson, 2010; (d) Damiani et al, 1996; (e) Frasse et al., 1992; (f) Gassenmeier et Schieberle, 1995; (g) Guerzoni et al,
AN
2007; (h) Hansen et Hansen, 1994; (i) Hansen et Hansen, 1996; (j) Hansen, Lund et Lewis, 1989b; (k) Heiniö et al., 2003; (l) Kaseleth et al., 2011; (m) Lund, Hansen & Lewis,
1989; (n) Pico et al., 2015 ; (o) Plessas et al, 2008; (p) Poinot et al, 2007; (q) Pozo-Bayon, 2006; (r) Raffo et al., 2015; (s) Ravyst & De Vuyst L.; (t) Ripari et al., 2016; (u)
Schieberle & Grosch, 1994; (v) Schieberle, 1996; (w) Settanni et al., 2013; (x) Thiele et al, 2002; (y) Ventimiglia et al, 2015; (z) Zehentbauer & Grosch, 1998
M
(α) The GoodScent Company; (β) Leffingwell et al.
D
TE
C EP
AC
ACCEPTED
Table 3 - Occurrence of major volatile compoundsMANUSCRIPT
in Sourdough (SD), Sourdough Bread (SD-B) or
Non-Sourdough Bread (Non SD B) based on Table 2 and taking into account volatile compounds
reported by at least 3 authors at the sourdough step (Numbers correspond to the number of
publications mentioning the volatile compounds)
Number of citations in…

SD and SD-Bread Sourdough (SD) Bread (B)
Odor (from littérature) α
Volatile compounds Wheat Rye Wheat Rye Non
SD SD SD B SD B SD B
Aldehydes
Fresh, Green, Fatty, Aldehydic, Grass,
Hexanal 4 4 2 3 5
Leafy, Fruity, Sweaty
PT
Musty, Cocoa, Coffee, Nut, Malty,
2-Methylbutanal Fruity, Sweet, Roasted
1 3 1 2 4
Almond, Strong, Sharp, Sweet, Bitter,

Benzaldehyde 5 2 2 - 4
RI
Cherry
Aldehydic, Rose, Waxy, Citrus,

Nonanal 4 3 2 1 4
Orange, Floral
SC
Ethereal, Aldehydic, Chocolate,
3-Methylbutanal Peach, Fatty, Sour, Roasted Bread, 1 4 3 5 8
Fruity, Fermented, Corn flakes
U
Alcohols
Ethanol Strong, Alcohol, Ethereal, Medicinal 4 1 4 - 7
1-Propanol
1-Pentanol
2-Methylpentanol
AN
Alcohol, Fermented, Musty, Fusel
Oil, Sweet, Balsamine, Chemical mint
4
3
5
2
3
2
3
3
2
2
3
1
5
4
5
2-Propen-1-ol Alliaceous, Pungent, Mustard 5 1 - - 3
M
Phenol Phenol, Plastic, Rubber 4 1 1 - 4
1,4-Butanediol 6 4 3 3 4
D
Ethereal, Oil, Alcohol, Green, Fruity,

1-Hexanol 2 3 2 1 4
Sweet, Woody, Floral
TE
Waxy, Green, Orange, Aldehydic,

1-Octanol Rose, Mushroom, Citrus
- 3 - 1 3
2-Methylbutanol Roasted, Wine, Onion, Fruity 3 1 - 1 5

Ketones
EP
Sweet, Fruity, Ethereal, Wine,

2-Pentanone Banana, Woody
1 3 1 1 4
Citrus, Green, Musty, Apple,
6-Methyl-5-hepten-2-one Lemongrass
4 4 2 5 8
C
2-Octanone Earthy, Grass, Woody, Soap 4 1 - 1 5

Acids
AC
Formic acid Acrid, Vinegar, Formyl 4 2 3 2 6

Octanoic acid Fat, Waxy, Rancid, Vegetable, Cheesy 4 2 1 - 5
Furans
Sweet, Balsamine, Almond, Cocoa,
2-Acetylfuran 2 3 1 1 5
Caramel, Coffee, Burnt
Esters
Ethereal, Sweet, Fruity, Solvent,
Methyl acetate Wine, Cognac, Rum
3 1 2 1 1
Floral, Rose, Sweet, Honey, Fruity,

2-Phenylethyl acetate Tropical
4 1 1 1 5
Green, Earthy, Mushroom, Herbal,
Octyl acetate 4 4 2 1 5
Waxy
ACCEPTED MANUSCRIPT
SOURDOUGH PROCESS BREAD-MAKING PROCESS
PT
Ingredients Dough yield Dough ingredients Fermentation parameters
flour type (ash, cereal), salt, Temperature flour (ash, cereal), salt, Baking temperature
RI
sugar/enzyme addition , water Time of fermentation enzymes/sugar/ amino acids, fat Storage conditions
proportion, substrates Backslopping (proportions, Mixing parameters
SC
(carbohydrate, nitrogen) time, frequency)
U
Sourdough Sourdough Bread
AN
Proportion of sourdough
Microflora
(LAB homo/heterofermentative,
M
yeasts, interactions between yeasts
and LAB)
D
Volatile compound profile TE Volatile compound
and precursors profile
C EP
Sensory properties
AC
Figure 1 – Sourdough and sourdough-bread volatile compounds: variations in parameters

ACCEPTED MANUSCRIPT
Dough Formulation
(Flour, microflora, enzymes, sugars, fat, salt …)
Volatile compound precursors
PT
RI
Carbohydrates , Aldehydes, Amino acids Lipids, Fatty acids Amino acids, Peptides, Carbohydrates
SC
Fermentation Lipid oxidation Maillard reaction
U
AN
Microflora, Fermentation process Mixing, Storage, Oxygen Cooking, Drying
M
Acids, Alcohols, Esters, Ketones Aldehydes, Ketones Pyrazines, Pyridines, Pyrroles, Furans,
Aldehydes, Lactones Sulfurs, Aldehydes, Ketones
D
TE
C EP
AC
Sourdough and bread volatile compounds
Figure 2 – Sourdough and sourdough-bread: major origins and main influential factors –
with Volatile compound origins; Variation factors; Volatile compound precursors; Major associated volatile compound chemical classes;
Secondary associated volatile compound chemical classes
ACCEPTED MANUSCRIPT
Sourdough FERMENTATION
Ingredients /
Microbial Interactions Lactic Acid Process
Yeast Physico-chemical parameters Bacteria
PT
(pH, temperature buffering capacity,
temperature, DY, substrates) Flour amylases
RI
Primary and secondary metabolites
(alcohols, aldehydes, organic acids, amino acids) LAB enzymes
SC
+
Chemical reactions (e.g. esterification)
Ehrlich pathway
Proteolysis Flour proteases
U
AN
Amino acids Lipid oxidation
M
Fusel
D
alcohols Maillard
TE reaction
EP
Bread volatile compounds

C
AC
Figure 3 – Simplified contribution of sourdough microbiota to volatile compound

generation (LAB: Lactic Acid Bacteria)
ACCEPTED MANUSCRIPT
Sourdough volatile compounds and their contribution to bread: a review
Cécile Pétel1,2, Bernard Onno2, Carole Prost1*

1
Flavor team, Matrix and Food, Process/properties – Structure/sensory, UMR CNRS 6144 GEPEA, Oniris, LUNAM university,
Nantes, France
2
Food and Industrial Microbiology Laboratory, Oniris, Nantes, France
PT
*
corresponding author: Carole Prost, mail: carole.prost@oniris-nantes.fr, tel: +33 (0)2 51 78
55 17, fax: +33 (0)2 51 78 55 20
RI
Highlights
• Comparison of volatile compounds extraction methods used on sourdough and bread.
• 540 volatile compounds previously reported in sourdoughs and in sourdough breads studies
SC
are listed.
• Origins, odor threshold and odor of most of the volatile compounds are reported as well as
their presence in sourdough, sourdough bread and bread.
U
AN
M
D
TE
C EP
AC

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Accepted Manuscript

Sourdough volatile compounds and their contribution to bread: a review

Cécile Pétel, Bernard Onno, Carole Prost

To appear in: Trends in Food Science & Technology

Received Date: 29 June 2016

1 Sourdough volatile compounds and their contribution to bread: a review

2 Cécile Pétel1,2, Bernard Onno2, Carole Prost1*

33 Key words (6)

34 Sourdough; sourdough bread; volatile compounds; bread; origin; extraction

82 Figure 1 – Sourdough and sourdough-bread volatile compounds: variations in parameters

95 2. Methods for studying volatiles in sourdough and sourdough bread

104 2.1. Extraction methods based on solvent affinity

117 2.2. Extraction methods based on compound volatility

151 2.3. Headspace solid-phase micro-extraction: parameter selection and optimization

157 preparation (Side et al., 2000).

197 the comparison of studies.

198 2.4. Extracted volatile compound analysis

210 2.5. Conclusion about volatile compound extraction techniques

235 main associated characteristics.

302 3.2. Main origins of volatile compounds

321 3.2.1. From fermentation processes

322 Figure 3 – Simplified contribution of sourdough microbiota to volatile compound generation

374 al., 2011).

377 2-phenylethanol (rose), 2-methylbutanol (roasted), aldehyde (acetaldehyde, hexanal,

388 decanal (sweet), octanal (floral), 3-methylhexanal (sweet), 2-methylpentanol, 1-nonanol

437 3.3. From lipid oxidation

468 3.4. From the Maillard reaction

486 3.5. Impact of ingredients and processes

515 4. Impact of sourdough on bread

548 4.2. Volatile compound evolution from sourdough to bread

553 sourdough bread ((E,E)-2.4-heptadienal, 4-nonenal, ethyl-2-methylpropanoate, 3-methylbutyl

561 4.2.1. From wheat sourdough to wheat sourdough bread

578 4.2.2. From rye sourdough to rye sourdough bread

587 volatiles is not known.

588 4.2.3. Impact of the recipe on volatile compounds

629 5. Future aspects

722 Grosch, W. (2007). Gas Chromatography-Olfactometry of aroma compounds, in Flavours

730 yeasts interactions. Food Microbiology, 24(2), 139–148.

760 Leffingwell and Associates. [on line]. www.leffingwell.com/odorthre.htm. Page consulted

806 205, 297-307.

810 Rothe M. (1974). Aroma of bread. Berlin: Akademie

813 Schieberle P. (1996). Odour-active compounds in moderately roasted sesame. Food

836 51, 57-68.

839 production by yeasts and lactobacilli. Food Chemistry, 108(4), 1217-1225.

842 Science, 56(2), 127–133. http://doi.org/10.1016/j.jcs.2012.03.007

850 Figure Captions

851 Figure 1 – Sourdough and sourdough-bread volatile compounds: variations in parameters

853 Figure 3 – Simplified contribution of sourdough microbiota to volatile compound generation

Number of described Volatiles

Frasse et al. 1992 Wheat bread bread crumb ND GC-MS (apolar) - 25

Schieberle P. Rye sourdough HRGC-MS , HRGC-O

Gobbetti et al. 1995

samples + 49.5ml 30%

powder +9,9 mL NaCl µm)

Ravyts E. & Wheat and rye 5 g sourdough + 1g

SPME Fiber: DVB/Car/PDMS

SPME Fiber: DVB/Car/PDMS

2015 Wheat sourdough 5 g of sourdough Equilibrium : non mentionned GC-MS (polar) 31 - -

Origins Reported for…

Perception threshold in water (ppb) β

Also found in Wheat bread

Pentanal 110 62 3 Fermented, Bread, Fruity, Nutty, Berry 12-42 e - - - K - q - q,n

Heptanal 111 71 7 3 d b,e,n - d l a o,q - b,r,n