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Herbal Processing and Extraction Technologies

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DOI: 10.1080/15422119.2016.1145395

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Separation & Purification Reviews

ISSN: 1542-2119 (Print) 1542-2127 (Online) Journal homepage: http://www.tandfonline.com/loi/lspr20

Herbal Processing and Extraction Technologies

Siti Nuurul Huda Mohammad Azmin, Zainuddin Abdul Manan, Sharifah


Rafidah Wan Alwi, Lee Suan Chua, Azizul Azri Mustaffa & Nor Alafiza Yunus

To cite this article: Siti Nuurul Huda Mohammad Azmin, Zainuddin Abdul Manan, Sharifah
Rafidah Wan Alwi, Lee Suan Chua, Azizul Azri Mustaffa & Nor Alafiza Yunus (2016):
Herbal Processing and Extraction Technologies, Separation & Purification Reviews, DOI:
10.1080/15422119.2016.1145395

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Download by: [Universiti Teknologi Malaysia] Date: 26 January 2016, At: 00:34
Herbal Processing and Extraction Technologies
Siti Nuurul Huda Mohammad Azmin1,2, Zainuddin Abdul Manan1,2, Sharifah Rafidah Wan
Alwi1,2, Lee Suan Chua3, Azizul Azri Mustaffa1,2 and Nor Alafiza Yunus1,2.
1
Process Systems Engineering Centre (PROSPECT), Research Institute of Sustainable

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Environment (RISE),

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2
Faculty of Chemical Engineering,

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Institute of Bioproduct Development (IBD), Universiti Teknologi Malaysia, 81310 UTM, Johor
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Bahru, Johor, Malaysia.

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Submitted Dec. 30, 2013; Revised Nov. 11, 2014 and Oct. 25, 2015; Accepted Jan. 14, 2016

Abstract:

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Herbs are widely utilized in food and health industries. Their beneficial effects to the human

body have been attributed to the presence of active phytochemical ingredients with some
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efficiency for disease treatment as well as for beauty and health enhancement. Public awareness

on the adverse effects of synthetic chemical products also increased the demand for herbal
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products. Highly efficient herbal processing and extraction technologies have been developed to

obtain the optimal amounts of active ingredients from herbs and cope with the rising demands
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for herbal products. This paper reviews the state-of-the-art development in herbal processing

and extraction methods from the year 1991 until 2015. The paper begins with a brief history of
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herbal usage, followed by descriptions of ten types of extraction processes and critical analysis
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of their relative advantages and disadvantages. Scale-up considerations of the extraction

methods are also presented. The paper concludes with a highlight of the current and future

challenges facing the herbal industry.

1
Keywords:

Extraction technologies, Herbs, Herbal processing, Natural products, Phytochemicals.

Corresponding author: Sharifah Wan Alwi, shasha@cheme.utm.my

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1 INTRODUCTION

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Throughout human history, herbs have been used in food, cosmetics and fragrances [1]. In

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addition, they are a source of traditional medicines for the treatment of various illnesses and

diseases [2]. Traditional medicine has been defined by the World Health Organization (WHO)
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as “health practices, approaches, knowledge and beliefs incorporating plant, animal and mineral-

based medicines, spiritual therapies, manual techniques and exercises, applied singularly or in
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combination, to treat, diagnose and prevent illnesses or maintain well-being” [3]. Herbal
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products have recently increased in importance in the treatment of health-related problems. A


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recent WHO report [3] stated that 5.6 billion people, or approximately 80% of the world’s

population, use herbal products for their primary health care [3-5]. Herbal products are currently
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being used as dietary supplements, nutraceuticals, health products, and traditional medicines.

These products also are being prescribed by Chinese and Indian national pharmacopeias [5]. The
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botanical dietary supplement market in the U.S. has expanded rapidly from US$ 2.9 billion in
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1995 [6] to US$ 4.8 billion in 2008 [7]. Over 42% of the U.S population has claimed to have

used botanical dietary supplements either to widen their current diet or to treat or to prevent

health-related issues [5]. European dietary supplements have contributed to a steady 4% growth

rate of the market between 2004 and 2011. The total market in 2004 was valued at US$ 6.2

2
billions [8]. With Malaysians consuming over US$ 1.44 billion worth of herbal-related products

(with over 80% imported) [9], the opportunity to increase herbal product processing in Malaysia

has expanded. From 2000 to 2005, annual sales of traditional medicines increased from US$ 385

million (RM1 billion) to US$ 1.29 billion (RM45 billion), as reported by Malaysian National

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News Agency, BERNAMA [10]. The expected growth of the herbal medicine industry is

between 15% and 20% per year [11].

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With the increased demand for herbal products, Malaysia is well-positioned to be a key global

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player in this field because of its rich biological resources, cultural background, and trade links

[1]. In addition, Malaysia is ranked fourth in Asia and twelfth in the world as the most
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biodiverse nation, with 3,000 species of medicinal plants and 15,000 species of flowering plants

[12]. Among the 3,000 known medicinal plants [13], the top Malaysian traditional medicinal
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plants are Tongkat Ali (Eurycoma longifolia), Kacip Fatimah (Labisia pumila), Hempedu Bumi
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(Andrographis paniculata), Dukung Anak (Phyllantus amarus), Misai Kucing (Orthosiphon


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stamineus), and Pegaga (Centella asiatica). Among these known plants, less than 50 traditional

medicine species have been scientifically investigated, with the remainder not yet characterized
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[1]. Worldwide, more than 35,000 plant species have been reported to be employed for medical

purposes [14]. Even with this extensive number of available plant species, Rates [15] has
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reported that only 121 active compounds from herbs have been utilized, with approximately 25%
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of prescribed drugs originating from these plants.

Medicinal plants have often been applied for a broad range of acute and chronic conditions [16].

This provides ample opportunity to gain a vast wealth of knowledge through exploration of these

3
plants. Phytochemical constituents in medicinal plants, such as flavonoids, phenolics, and

saponins [17], are believed to have numerous therapeutic abilities and are able to reduce the risk

of multiple diseases, including inflammatory conditions and cancer [18]. They contribute to the

protection of herbs from microbial and insect invasions [19]. Flavonoids have been utilized to

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improve human health via their multiple biological functions including anti-inflammatory [20],

antimicrobial [21], antioxidant [22], and anticancer activities [23] and the prevention of

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osteoporosis [24]. Tsao and Deng [25] have reported that phenolic acids from herbs have

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antioxidant activities that exceed the values exhibited by vitamins C and E. Polyphenols have

also been applied in the prevention of both cancer and heart disease [19]. Aqueous extracts of

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the Malaysian herb L. pumila, commonly known as Kacip Fatimah, have been demonstrated to

protect significantly human dermal fibroblasts from cell damage caused by ultraviolet irradiation
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[26], most likely as a result of the presence of flavonoids [27]. Ginseng, one of the most

commonly used herbs, contains saponins as active ingredients [28]. Ginseng exhibits a broad
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range of biological properties, including aphrodisiac and adaptogenic activities [29].


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With the high demand for herbal products that promote health advantages, the identification of
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the most effective methods [30] for extracting the active ingredients from plants has become

increasingly important. Traditionally, herbal extracts are prepared by boiling the roots, leaves, or
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the entire plant in water using a method known as tisane or decoction. These types of extracts
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can be consumed orally, but these methods are time-consuming and may not be the most

effective method for extracting the active ingredients from the herbs. This article provides a

review of the state-of-the-art on herbal processing techniques and discusses the effectiveness of

common extraction processes.

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1.1 A History of the Uses of Herbs

Herbs have been used for many purposes, including as ingredients for medicinal products, beauty

enhancers, fragrances, and food. In the case of beauty enhancers, the natural components in herb

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products are easily absorbed by the human skin [19] and are both safe and compatible with

human body, as natural ingredients that have demonstrated no known toxicity. Natural products

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in skincare formulations have been shown to exhibit significant antioxidant [100], emollient

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[101], and UV–B protection [102] properties.

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In the early nineteenth century, the first chemical analyses performed by scientists were utilized

to determine the active ingredients from plant extracts, which subsequently led to the
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development of natural (traditional) medicines that had been passed historically through

generations by words of mouth [2]. Many of the herbs and spices used for food seasoning also
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yield useful medicinal compounds [31, 32]. Simple preparation methods for processing the plant
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herbs by boiling either the entire plant or selected parts of the plant have been employed by

herbal medical practitioners for over 5,000 years [33].


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2.0 STEPS IN HERBAL PROCESSING


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Starting from the planting and harvesting stages, the steps practiced for processing the

natural products are very important. Every part of the plant matures at different times, which

suggests that the harvesting process should be optimized on the basis of the desired plant parts.

As shown in Table 1, the general guidelines for harvesting the three primary parts of the herbal

5
plants (i.e., leaves, stems, and roots) are presented to enable selection of the harvesting time on

the basis of the part of the plant that provides the optimal results in the extraction process.

Karimi et al. [34] showed that the leaves of L. pumila exhibited higher antioxidant activities and

total saponin amounts [35] than the plant roots and stems. Ramlan [36] classified four different

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stages of herbal processing to produce the final herbal products.

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Before processing starts, the harvested herbal plants must be pre-processed. At this stage, the
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plants must be dried to remove moisture for preservation, preventing bacteria activity and

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restricting fungal growth [37]. To increase the surface area of the dried herb plant materials for

improved contact with the solvent during the subsequent extraction process, the dried plant must

first be ground.
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An increased surface area of the dried plant materials will improve the

performance of the extraction process. The particle size of the milled plants is one of the factors
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that can affect the extraction yield.
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In the extraction processes, the operating conditions can greatly affect the efficiency of a
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particular technique. For solid–liquid extractions, important parameters include an appropriate


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solvent system, the solvent-to-herbs ratio, the particle sizes of ground and dried herbs materials,

the temperature, the duration, and the agitation rate, as discussed by Sim et al. [37]. Preliminary
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studies are necessary to determine these operating conditions prior to starting the extraction
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experiments. Literature studies can provide very useful information for determining the optimal

operating conditions.

In some processes, solvents are mixed with herbal raw materials (normally in the dry

powder form) and then subjected to forces such as heat, pressure or microwave power to enable

6
the phytochemicals to diffuse out of the herb cells into the solvent medium. The mixture of

solvent and extracted phytochemicals can exist in a miscible form, or can produce two liquid

layers (if essential oil is produced). The solvents are then removed from the mixture, typically

via evaporation in a rotary evaporator. Then, the crude extract is further processed into natural

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products.

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3.0 STATE OF THE ART IN HERBAL
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EXTRACTION METHODS

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With herbal processing, the type of extraction process can greatly affect the final natural

products obtained. Suitable extraction processes are needed to extract the desired active
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ingredients from herbs. Fig. 1 shows ten possible extraction methods that will be detailed

thereafter. In Table 2, the advantages and disadvantages of the available extraction methods are
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presented. The biggest advantage is when the extraction method can be used to extract plant
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compound in a short time with the minimum solvent consumption. Short extraction time is
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desirable due to the associated reduced electricity consumption and the ability to minimise any

potential degradation of active components.


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3.1 Supercritical Fluid Extraction (SFE)

Supercritical fluid extraction (SFE) is one of the extraction methods in herbal processing

due its ability to extract the valuable ingredients from herbs with high yield and good quality

[38]. Its favorable features include the ability to perform extractions at near-ambient

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temperatures, which prevents thermal degradation of the substance of interest [39]. SFE is also

being extensively studied as an alternative to conventional extraction methods [38]. Among the

possible SFE solvents, carbon dioxide (CO 2 ) is the most established and widely used solvent

[40]. CO 2 has unique properties, which include non-toxicity, non-flammability, lack of solvent

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residue in the final product, and lack of reactivity with extraction materials and equipment.

These behaviors make it commonly used in numerous extraction processes. In addition, this gas

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is less expensive than most common solvents, which reduces the cost of the extraction process.

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One of the most important benefits of CO 2 in the SFE processes is the reduction in the

environmental and health concerns that arise from the use of organic solvents [41, 42].

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In the SFE environment, only one fluid phase exists; the properties of this fluid resemble an

intermediate phase between gas and liquid. Carbon dioxide at the supercritical state has a critical
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temperature and pressure of 31.1 °C and 73.8 bar, respectively. Under these conditions, CO 2
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exhibits both gas-like characteristics, with high diffusion coefficients and low viscosities, and
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liquid-like characteristics, with high solvating power properties. These features make

supercritical CO 2 a good fluid solvent [43]. Both viscosity and diffusivity are factors that affect
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the penetration of solvent into the herbal materials. The decreased viscosity and increased

diffusivity of solvent facilitate the penetration of solvent into porous solid materials, resulting in
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increased mass transfer and reduced extraction times in SFE [63]. The solvation power, which
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changes with temperature and pressure, is another factor that can determine the effectiveness of

the SFE method. Modification of the solvent solvation power can be employed to achieve high

selectivity of the extraction product from herbs. In addition, modification of the solvent

solvation may be useful in the extraction of complex samples, such as plant materials [44, 45].

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One of the advantages of SFE is that the system operates at low temperatures, which is an ideal

technique for studying temperature-sensitive compounds [46-48] and may possibly lead to the

discovery of new natural compounds [49]. To minimize waste generation, the spent CO 2 can be

recycled and reused, even for large-scale system. SFE is very useful for removing pesticides

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from herbal medicines [50].

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Unmodified CO 2 may lead to a limited selectivity of this apolar solvent. Thus, a polar solvent
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modifier can be used to overcome this drawback. Significant losses of the desired compounds

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can occur if an inappropriate solvent modifier is applied. These losses can occur for desired

compounds that are removed with the solvent or via undesired reactions facilitated by the solvent
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itself [51]; such losses represent two of the major disadvantages of the SFE process. The most

commonly-used solvent modifiers are methanol, ethanol, acetonitrile, acetone, water, ethyl ether
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and dichloromethane. Methanol is a popular choice due to its effectiveness as a polar modifier
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(up to 20% miscible with CO 2 ). However, the use of methanol as a modifier could be
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disadvantageous when thermolabile compounds are involved because of the slightly higher

temperature required for methanol to reach its supercritical state. In addition, a major obstacle is
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the cost of purchasing the equipment compared with other methods.


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3.2 Microwave-Assisted Extraction (MAE)


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Microwave-assisted extraction (MAE) is a process that uses a liquid solvent, such as

water or alcohol, to extract the active ingredients from herbs. In MAE, the enhanced extraction

occurs as the result of changes in the vegetable cell structure caused by electromagnetic waves in

MAE [52]. On the other hand, in conventional extractions, the mass transfer of the

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phytochemicals occurs from inside (herbal particle) to the outside (solvent), although the heat

transfer occurs from the outside (heat source) to the inside (herbal particle) [53]. Generally,

microwaves are electromagnetic radiations with a frequency from 0.3 to 300 GHz [54]. The

microwave energy is delivered directly to the herbal particle through molecular interactions with

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the electromagnetic field via conversions of electromagnetic energy into thermal energy [55].

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Thus, MAE typically results in a short extraction time and high extraction yield. Besides, the

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combination of two transport phenomena; heat and mass gradients working in the same direction

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[53] also contribute to the high yield and short extraction time of MAE.

MAE has been applied to extract the ingredients from the leaves and roots of L. pumila [18].
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Abdul Qayoom et al. [56] used MAE to extract ingredients from the leaves and flowers of C.

angustifolia. The parameters that affect the extraction efficiency of this extraction method are
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the power and frequency of the microwaves, the duration of the microwave irradiation, the
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moisture content and particle sizes of the plant samples, the type and concentration of the
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solvent, the ratio of solid to liquid, the extraction temperature, the extraction pressure, and the

number of extraction cycles [57]. Among these factors, solvent selection is the most important
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parameter because the solvent affects the absorbance of the microwave energy, as determined by

the dissipation factor [58, 59]. The solvent must have an affinity for the target compound and an
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ability to absorb microwave energy [60]. Another critical factor in MAE is the ratio of the solid
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herbs to the amount of solvent. The bioactive ingredients in the herbs can effectively dissolve

when large amounts of solvent are used, thereby leading to improved extraction yields [60, 61].

Gao et al. [61] and Li et al. [62], who applied a high solvent ratio with MAE, reported consistent

results. However, their results differed from those of other studies by Guo et al. [63], Li et al.

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[64], and Spigno & Faveri [65], who found that when large quantities of solvent were utilized,

the extraction yield initially increased and then decreased as the solid-to-liquid ratio decreased.

When the amount of solvent was reduced (high-solid herbal materials), microwave energy may

have been absorbed and dispersed by the large amount of plant materials [61], thereby increasing

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the solid mass, and decreasing the surface area available for solvent to penetrate the plant

materials and solubilize the target molecules [66]. Agitation or shaking of the sample–solvent

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mixture may also have become inadequate when the microwaves were applied to the large-

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volume sample [67].

One of the advantages of MAE is the applicability of this process for both large-scale
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(industrial) and small-scale (laboratory) systems. This method is believed to be more efficient in

extracting active ingredients with less time compared to conventional methods. Oil that is
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extracted using MAE contains increased concentration of oxygenated compounds, and have been
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demonstrated to exhibit antibacterial and antifungal activities [68-70].


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The primary disadvantage of MAE is the reduction of efficiency in the microwave


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techniques for nonpolar target compounds or solvents and with highly viscous solvents [57, 71].

In addition, MAE is not appropriate for the extraction of temperature sensitive compounds [72].
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3.3 Sonication Extraction


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In this extraction method, conditions such as the time and the ratio of herbs to solvent share

similarities with the MAE processes, except the intensity of the ultrasonic equipment is replaced

instead with the microwave power to facilitate the extraction processes. Chua et al. [19] applied

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a sonication extraction technique to extract the dried leaves of L. pumila. The correct choice of

solvent coupled with appropriate agitation and/or heat characteristics are also the major factors in

optimizing this type of extraction process. The solvent extraction of herbal materials can be

improved through the use of ultrasonic power because of the mechanical effects resulted from

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the ultrasound process. This effect results in improved solvent penetration into the cellular

materials via improved mass transfer within the herbal cells. In addition, the mechanical effects

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disrupt the biological cell walls, thereby resulting in the release of the cell contents such as

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herbal oils [83].

In sonication processes, longitudinal waves are created as a sonic wave encounters a


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liquid medium, which creates regions of alternating compression and rarefaction (expansion)

among the molecules of the medium. In these regions of changing pressure, cavitation of formed
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gas bubbles occurs. During the rarefaction cycle, the surface area of these bubbles increases,
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which results in increased gas diffusion and an expansion of the bubble. In the compression
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cycle (i.e., when insufficient ultrasonic energy is provided), these vapor phases cannot remain in

an expanded state, which results in rapid condensation and the release of large amounts of energy
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[73-75]. The shock waves created with high temperatures (550°C) and pressures (50 MPa) [73,

75] are a consequence of the condensation process. Both high temperatures and pressures
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generate microjets directed toward solid surfaces (i.e., the herbs or the container wall) as the
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bubbles collapse onto those surfaces. These microjets are responsible for the degreasing effect

of ultrasound on metallic surfaces, and this technique is commonly used to clean materials [76].

12
Sonication extraction is inexpensive, an efficient tool for large-scale commercial

applications, including emulsification, homogenization, extraction, crystallization, low-

temperature pasteurization, degassing, defoaming, both activation and inactivation of enzymes,

particle-size reduction, and modification of viscosity [77, 78]. This extraction technique, which

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is easy to use, features numerous advantages, including reduced working time, increased yield,

improved solvent consumption, and possibly improved quality of the extract. Ultrasound has

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weak effects on both yield and kinetics for the extraction of oil such as wood seed [79]. The

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effects of ultrasound on the extraction yield and kinetics may be linked to the nature of the plant

matrix [57]. The presence of a dispersed phase contributes to the ultrasound wave attenuation

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whereby the active part of ultrasound inside the extractor is restricted to a zone located in the

vicinity of the ultrasonic emitter. The two factors mentioned must be considered carefully in the
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design of ultrasound-assisted extractors.
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3.4 Soxhlet Extraction


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Soxhlet extraction serves not only as a technique for extraction of phytochemicals, but also as a
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reference to compare the newer extraction techniques [80]. Soxhlet extraction involves the use

of a Soxhlet apparatus (as shown in Fig. 2) for the extraction of herbs. The sample is placed in a
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thimble holder that is gradually filled with fresh solvent from a distillation flask (see Fig. 2). As
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the liquid reaches the over-flow level, a siphon aspirates the solute from the thimble holder,

moving the aliquot back into the distillation flask and carrying the extracted analytes into the

bulk liquid. This process continues until the extraction process has been completed. The system

operates in a continuous mode as the solvent is recirculated through the sample. With this

13
method, the extracts are isolated by being filtered and the solvent is removed at defined

temperatures under reduced pressure in a rotary evaporator [81]. This extraction technique can

maintain a high system temperature (at solvent boiling point) via a heat source applied directly to

the distillation flask. This method is also very simple and inexpensive [82].

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Soxhlet extractions are limited by the time required for the extraction process and by the large

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volumes of extractant (solvent) required. The solvents can be expensive to remove, and can
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cause environmental problems [83]. Note that in general, the compound boiling point is lower

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than that of the solvent. Due to the fact that the extraction process is usually performed at the

boiling point of the solvent for extended periods of time, thermal decomposition of the target
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compounds may also occur. In Soxhlet extraction, it is also necessary to choose the most

suitable solvent for extracting the targeted compounds because different solvent polarity will
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dissolve different compounds [84]. Hexane, which has a narrow boiling point (65°C) is the most
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widely applied solvent. However, this solvent is listed as an hazardous air pollutant by the US
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Environmental Protection Agency [85]. Thus, solvent substitution is commonly performed. As

examples, instead of using hexane, d-limonene was used by Mamidipally and Liu [85], while
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water was applied by Hanmoungjai [86] to extract oil from the rice bran. The alternative

solvents, however, result in less recovery due to the lower molecular affinity between the
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alternative solvents and the solute. Sometimes, co-solvent is added to match the polarity of the
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targeted compounds. This may increase the solvent cost.

3.5 Marinated Extraction

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Marinated extraction is an ancient extraction method conducted at room temperature. For this

technique, the parameters to be considered include the type of solvent, the ratio of dried herbs to

solvent, and the extraction time. This method requires a prolonged extraction time because it

does not use heat or other forces. The extraction products are commonly obtained by filtering

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the extracts first. The advantage of this method is that it requires neither special equipment nor a

special location such as a laboratory. The commonly cited disadvantage of this method is the

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long extraction time [87]. As an example, Laghari et al. [56] extracted flowers of Cassia

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angustifolia while Zhu [88] extracted Portulaca oleracea L. within 48 hours at room

temperature using this method.

3.6 Hydro-distillation Extraction


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Hydro-distillation extraction techniques use water as solvent. The mechanism for hydro-

distillation extraction is similar to that of the Soxhlet extraction process. Both methods are
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commonly used to isolate volatile and non-volatile polar components from aromatic plants [89],
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with small variations in the type of solvent applied and the equipment arrangement. In hydro-
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distillation extraction, the sample and water solvent are placed in a retort (Fig. 3). Heat is

applied to heat and vaporize the mixture. Water vapor causes small sacs in the raw plant
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material containing essential oil to burst. Extracted oil is then transported by steam in the vapor
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phase into the condenser where the condensate liquid mixture formed. The liquid mixture then

flows into a separator where water and the essential oil are separated by density difference. The

water-rich phase, which contains some plant essence is called ‘hydrosol’. As an example, when

roses are extracted using this method, the hydrosol is retained for use as a mild antiseptic and as

15
fragrance for floral aromatherapy. The experimental hydro-distillation extraction equipment

commonly used for herbal extraction is shown in Fig. 3. As a precaution, the temperature limit

inside the retort of a hydro-distillation extractor must be strictly observed in order to prevent

thermal compound degradation. As an example, lavender essential oil must be extracted at

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temperatures between 373 to 391 K (100-118°C). Operation at temperatures higher than 391 K

will result in the extract containing more chemicals than the targeted aroma, causing the

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therapeutic effect to be reduced. In addition, hydro-distillation extraction must be performed

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within a specified duration in order to ensure that the oil components are completely released.

One advantage of the hydro-distillation extraction method is that it does not require
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expensive organic solvent. Nonetheless, the method involves a separation step to separate the

liquid extract from water. This processing step may require a long period of time or the use of an
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additional solvent to facilitate separation [90].
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3.7 Steam-distillation Extraction


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Fig. 4 shows the steam-distillation extraction setup. Steam-distillation includes a steam


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generation apparatus to supply steam to the mixture of solvent and plant raw material. Steam
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maybe supplied at a pressure and the corresponding saturation temperature that is sufficiently
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higher than the boiling point of the mixture in order to allow evaporation to take place at lower

temperatures. Next, the evaporated mixture of water and compound flows into a condenser

where it is condensed into a liquid mixture and later collected in a separator. The solvent is

finally evaporated and separated from the compound using a rotary evaporator. Note that, a

preliminary study is typically performed to select a suitable solvent to extract the phytochemicals

16
of interest [91]. A solvent with a polarity value that is close to that of the specific compound of

interest in a herb, has a better chance of attracting the compound.

The steam distillation-extraction method is commonly applied for the extraction of

essential oils. As steam passes through the plant material, tiny pockets in the plant cell holding

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the essential oil will open and release the essential oil without damaging the oil structure. Thus,

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steam-distillation is a special extraction technique that can prevent the decomposition of organic
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compound due to high temperature as its temperature could be controlled. So that it could be

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operated below the decomposition temperature of the compounds.

3.8 Ultra-high Pressure Extraction an


M
High pressure in this type of extraction method refers to cold, isostatic ultra-high hydraulic

pressure. The Ultra-high pressure extraction technique involves three steps: i) mixing herb with
d

solvent, ii) extraction of the desired phytochemicals at high pressure, and iii) filtering of
te

supernatant to remove solid particles (herbal residual).


ep

Jun [92] showed the experimental set up of this method. Raw herbs and solvent were placed

together in a polyethylene bag and sealed after removing bubbles. Then, the bag was placed in a
c

pressure vessel that was equipped with a temperature controller (at the top and the bottom of the
Ac

vessel) and pressure valve (to release the excess pressure). Fluid was used to apply pressure to

the vessel using an ultrahigh pressure booster pump. Extraction was carried out at high pressure

(100 MPa to 1,000 MPa) and at room temperature for a specified duration (5 to 15 minutes). As

17
in the case of other methods, after the extraction process, the mixture was filtered and

concentrated by using a rotary evaporator.

Under high pressure, the solubility of natural compounds in any solvent is enhanced [93]. This

leads to the faster diffusion time of compounds into the solvent medium. The pressure range

t
ip
used for the UHPE method, between 100 MPa to 1000 MPa, is the highest among the extraction

cr
methods. For example, the pressure used in supercritical fluid extraction is about 100 MPa,
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while in other extraction methods used atmospheric pressure. The ultra-high pressure applied in

us
UHPE leads to the increase in the compound solubility and shorter extraction time. Xi [94]

compared the times needed for the extraction of green tea leaves using different extraction
an
methods. In their investigation, high pressure extraction method gave the shortest time (1 min)

to extract 30% of polyphenols from green tea leaves in water. Other methods which involved
M
extraction at room temperature, ultrasonic extraction and heat reflux extraction needed 20 hours,
d

90 minutes and 45 minutes, respectively. The results prove that the high pressure extraction
te

method can extract the needed compound within the shortest extraction time. Note that, even

though the UHPE method is operated at high pressure, it requires no electrical power supply
ep

during pressure holding. Power supply is only required when pressure has to be increased.
c

Organic compounds in herbs are typically heat-sensitive [95]. Application of heat may cause the
Ac

organic compounds to denature, lose biological activity or decompose to other compounds.

Compound decomposition can be avoided using UHPE that operates at room temperature [95].

The extract impurity is, however, a main issue and drawback of the UHPE method. As high

pressure is applied to the extraction system, extract purity is slightly changed.

18
3.9 Accelerated Solvent Extraction (ASE)

Accelerated solvent extraction (ASE) is performed at elevated temperatures (50 to 200°C)

and at pressures between 10 and 15 MPa maintaining the solvent in liquid form. These

t
conditions tend to enhance the solvent diffusivity and accelerate the extraction process.

ip
Giergielewicz-Możajska [96] shows the ASE equipment used in experimental work. There is a

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pressurization system that creates and applies pressure to the pressure vessel. The temperature

us
and pressure in this system are set to be constant. The sample, together with the solvent are

placed in the closed container inside the pressure vessel. The container is connected to a
an
thermocouple to detect temperature change in the sample container. If temperature change

occurs, the heating and cooling jacket (surrounding the sample container) will operate in order to
M
keep constant the temperature inside the sample container. The pressure, on the other hand, is

controlled by the pressure relief valve. When the pressure increases, the pressure relief valve
d

will be opened to prevent pressure from building up. When the pressure decreases, the
te

pressurization system will apply pressure to the vessel. Note that, pressure is only created when
ep

the pressure inside the vessel drops below the set pressure, thereby saving the pressurization

energy during the extraction process.


c
Ac

Note that the ASE method is normally applied for thermally-stable organic pollutants from

environmental matrices. The ASE is not suitable for thermally labile compounds because the

high temperature needed in the ASE method may lead to degradation of heat-sensitive

compounds. This is perhaps the reason why very few applications of ASE have been published

in the field of nutraceuticals.

19
The performance of ASE was proven effective by Kaufmann and Christen [97] who compared

the ASE method with the Soxhlet extraction for isolating steroids from the leaves of Lochroma

gesnerioides. In addition, the findings showed that both methods could produce the same results

in terms of recovery, repeatability and selectivity. The extraction time and solvent consumption

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ip
may be reduced by using the ASE [57, 97].

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3.10 Hot Water Extraction
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Hot water extraction (HWE) belongs to the same category as the ASE process. The HWE

however uses hot water for extraction instead of an organic solvent. The use of water as a
an
solvent results in lower operating cost for the in HWE method because water is a cheaper

solvent. As a solvent, water is also relatively easier to treat and recover, and poses relatively less
M
environmental issue. Ayala and De Castro [98] proved that, the isolation of oregano essential oil

using HWE is quicker, cheaper and more effective than using hydro-distillation extraction
d

method. Besides, Ozel [99] found that the HWE method can extract the most valuable
te

antioxidants (carvacrol and thymol) from essential oils of Thymbra spicata at high concentration
ep

(~90%).
c

Carvacrol and thymol are valuable nutrients in the food industry. Eikani [100] also compared the
Ac

efficiency of HWE, hydro-distillation and Soxhlet extraction in extracting essential oils from

coriander seeds (Coriandrum sativum L.). Their findings showed that hydro-distillation and

Soxhlet extraction showed higher extraction efficiencies than the HWE. However, the HWE

showed better results in the extraction of more concentrated and valuable oxygenated

components in essential oils (used in food industry). The extraction of essential oil from

20
marjoram leaves was done by Jimenez-Carmona [101]. The authors compared the performances

of HWE and hydro-distillation extraction processes and found that the volume of essential oil

extracted using HWE was 5.1 times the volume extracted using hydro-distillation. The authors

also reported that the extracted essential oil contained high amount of oxygenated components.

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ip
Besides, the HWE is capable of extracting the same amount of essential oil within 15 minutes

compared to hydro-distillation extraction which took 3 hours as reported by Jimenez-Carmona et

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al. [101], Saim [102]]. Findings by the authors suggest that the HWE method is better for

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extracting essential oils.

4.0 COMPARISON OF
an THE EXTRACTION

PROCESSES
M
Comparison of the extraction processes in the previous section reveals that SFE is a well-
d

established technique for the extraction and separation [39] of both essential oils and its
te

derivatives for the food, cosmetic, pharmaceutical, and other related industries. SFE processes
ep

also result in high-quality essential oils with commercially viable compositions, as compared to

the products obtained using conventional steam-distillation processes [103, 104]. In the SFE
c

method, the physicochemical properties of the extraction fluid, such as its density, diffusivity,
Ac

dielectric constant, and viscosity, can be easily controlled by varying the pressure or temperature

without crossing the phase boundaries [105]. Over the past four decades, supercritical CO2 has

been applied for the extraction and isolation of multiple valuable compounds from natural

products [106]. The use of CO 2 as a solvent in SFE has provided an excellent alternative to

21
chemical solvents to extract the bioactive components from herbs and other medicinal plants.

The use of supercritical CO 2 is also more environmentally friendly than most extraction

techniques that use organic and liquid solvents. For example, the MAE processes use organic

solvents, such as methanol and ethanol that are relatively less environmentally friendly than

t
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CO 2 . Hawthorne et al. [107] extracted essential oils from savory, peppermint, and dragonhead

using both SFE and steam-distillation processes. They determined that SFE and steam-

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distillation extracts had similar distributions of volatile components. The results of their study

us
suggested that steam-distillation did not result in significant losses of the more volatile essential

oil components. In addition, SFE was determined to be a rapid and quantitative method for

an
extracting essential oils from aromatic plants. Rezazadeh et al. [108] extracted lavender oil and

compared the efficiencies of both SFE and steam-distillation. They determined that the
M
extraction yield of SFE was approximately six times higher than those obtained using the steam-

distillation process. The extraction time with SFE was considered suitable for the processing of
d

high quality lavender oil, compared to the products obtained using steam-distillation processes.
te

Abdul Qayoom et al. [56] studied the extraction of the leaves and flowers of Cassia
ep

angustifolia using four different extraction methods including microwave, sonication, marinated,

and Soxhlet extraction processes. Among these four extraction methods, the microwave
c

extraction method was found to be the best technique on the basis of its ease of use, robust
Ac

processing, and minimal time required to process the materials and to efficiently extract large

amounts of the desired phytochemicals. The extracts obtained by this method also exhibited an

increase in antioxidant activities. The other methods investigated were effective for extracting

phytochemicals, but exhibited low efficiencies. In addition, these other methods were found to

22
be very difficult to handle and needed longer periods of processing steps as compared to the time

required by the microwave extraction method.

A comparison between the sonication extraction and the MAE indicated that the

sonication extraction method was simpler even though both methods require the same amount of

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solvent. MAE, on the other hand, needed less extraction time as compared to the sonication

cr
extraction methods. In addition, the MAE apparatus and equipment are expensive and difficult
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to operate, as stated in a number of studies [57, 60, 109].

us
Ayala and De Castro [98], Ozel et al. [99], Eikani et al. [100] and Jimenez-Carmona et al.

an
[101] compared the performances of hydro-distillation and HWE techniques for the extraction of

essential oils from different plants. Compared to the hydro-distillation extraction process, they
M
found that the HWE offers many more advantages, including the ability to perform separation

that is:
d
te

• Quicker, (the HWE is capable of producing the same amount of extract within 15 minutes

as compared to 3 hours for the hydro-distillation extraction),


ep

• Cheaper (the HWE uses less electricity and power supply during the extraction process)
c

and,
Ac

• More effective (the HWE is able to produce more concentrated and valuable oxygenated

components).

When comparing the conventional steam-distillation, Soxhlet, and MAE methods, Chen et al.

[67] suggested that MAE had distinct advantages of decreased extraction time, increased

23
extraction yields, improved selectivities and of producing superior quality targeted extract

materials. In addition, MAE was relatively cost-effective as compared to the accelerated Soxhlet

extraction process [97, 110].

Xi et al. [94] compared three extraction methods which are sonication, marinated and ultra-high

t
ip
pressure to extract polyphenols from green tea leaves. Their investigation found that ultra-high

cr
pressure extraction method is suitable for fast extraction of polyphenols from green tea leaves as
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compared to other methods. Shouqin et al. [95] also compared the three methods for extracting

us
compounds from Epimedium, green tea, propolis and Scutellaria herbs. They found that, ultra-

high pressure extraction is a very useful tool for the extraction of natural products. The shorter
an
extraction time (5 to 10 minutes) is needed as the high pressure will quickly break the plant cell

and the solvent will permeate very fast through the broken solvent. This will increase the mass
M
transfer rate of compound to the solvent area. Besides, ultra-high pressure extraction helps save
d

a lot of energy because the energy is generated only when the pressure is lower than the set
te

pressure.
ep

Kaufmann and Christen [97] extracted natural compound from nine different herbs using ASE

and MAE. They found that the MAE can reduce the extraction time and solvent volume needed
c

while ASE can increase the diffusivity of solvent which leads to increase in the extraction speed
Ac

and efficiency.

From the comparison of methods in extracting various phytochemicals, it can be seen that

researchers have been searching for the potential methods that could result in higher extraction

yield, better selectivity, less solvent and energy requirement, faster extraction time, as well as

24
environmentally friendly process. However, there have been works that have compared the ten

extraction methods together. The comparison provides useful guides for future researcher and

process design engineers who may be interested to know the relative advantages and

disadvantages of the methods.

t
ip
5.0 CHALLENGES FOR THE HERBAL INDUSTRY

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Phytochemicals are very important constituents of herbal products because these active

us
components can often determine the safety and effectiveness of herbal products. Data on

an
phytochemical processing can be difficult to obtain, particularly the physical and chemical

properties [36], including solubility values, partition coefficients, and heat transfer coefficients,
M
are not available. These critical data are required to develop an effective process model that can

be integrated into process design methods similar to those that have been established for the
d

petrochemical and palm-oil-based oleochemical industries. The physico-chemical property data


te

can be obtained through either experimental studies or mathematical modeling efforts.

Determining the physical and chemical properties can be challenging because herbal materials
ep

contain multiple phytochemical components, and each component contributes to these properties.

Even with a full characterization of the phytochemical components, the components may have
c
Ac

isomers with different properties. For example, the components of L. pumila (Kacip Fatimah)

are still uncharacterized. In the herb extraction studies available in the literature, analysis using

gas chromatography (GC) or high-performance liquid chromatography (HPLC) have indicated

that the components varied with the method and solvent applied during the extraction process.

This lack of standardization has limited the number of scientific studies reported for L. pumila,

25
with a dearth of published data on the chemical properties and pharmacological activities of the

plant extracts [81, 111].

6.0 SCALE-UP METHODS

t
ip
Scale-up of extraction equipment enables the commercial production of herbs at larger

cr
scale to meet customer demands. Before scaling up, the laboratory-scale method should be
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tested in order to make sure that the selected method can extract the optimum amount of

us
phytochemicals. According to Santos [115] and Prado [116], the scale-up procedure assumed

an
that the industrial-scale unit has the same performance as the laboratory-scale unit when the ratio

between the mass of solid and solvent, size of raw material plant and the operating conditions are
M
kept constant. In validating scale-up criteria, it is necessary to assess their applicability to

different types of raw materials, as the mass transfer mechanisms may differ among species and
d

parts of the plant used for extraction [117]. In a scale-up plant, there is typically a huge amount
te

of waste either from solvent or solid waste. Thus, in scaling up the extraction method, reusing of

the waste can be very profitable [116]. As an example, grape seeds are considered a disposable
ep

waste material by the majority of wineries. The seeds are usually discarded, burned or used as

an animal feed [118].


c
Ac

Santos et al. [115] compared the performances of Soxhlet and ultra-high pressure

extractions to extract phenolic compounds from jabuticaba skins at laboratory scale. They found

that the ultra-high pressure extraction was more efficient than the Soxhlet extraction method.

Then, the scale up was done for ultra-high pressure extraction. This scale-up method used

26
aqueous ethanol (a mixture of 70:30 v/v ethanol and water) as solvent. Other conditions were

0.045 g/cm3 of feed to solvent ratio, temperature of 353K, pressure of 5MPa and an extraction

time of only 9 minutes. Using these conditions, the extraction resulted in 13.3% of extraction

yield. The unit was designed to operate for 8,000 hours in a year, which corresponds to 330 days

t
ip
per year of continuous 24-h-per-day shift. Note that the actual operating hours of 330 instead of

365 days a year allowed for at least two days per month for the process and plant maintenance

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[119].

us
Fiori [120] scaled up the SFE equipment for extracting grape seed. In this plant, CO 2

was used as solvent. The set operating conditions include pressure at 50 MPa, temperature at
an
373.15 K, ratio of solvent to feed at 4 kg CO 2 /kg grape seed and an extraction time at 2 hours.

The SFE unit includes three extraction vessels. The first vessel is for the extraction finishing,
M
the second is to conclude the extraction semi-cycle, and the third is a backup vessel.
d

Prado et al. [116] also performed a 17-fold scale-up for the Supercritical Fluid Extraction
te

of grape seed. The scaled-up conditions include a temperature of 313K, pressure of 35 MPa,
ep

ratio of CO 2 solvent to feed of 8.21 kg CO 2 /kg grape seed and an extraction time of 300 minutes.

The plant was designed to operate for 24 hours with three daily shifts for 330 days, or a total of
c

7920 hours of operation per year (the rest hours was used for process and plant maintenance). In
Ac

their study, they found that higher solvent velocity tend to cause mechanical dragging

(entrainment of oil not solubilized in CO 2 ), ultimately resulting in a low yield for the scale-up

plant. In scaling-up SFE, increasing the solvent mass flow will increase the entrained solvent

27
condensed phase. In order to prevent this phenomenon, an optimal ratio of solvent to raw

material must be maintained [121].

The 15-fold scale-up of SFE for extracting clove and sugarcane was successfully done by

Prado [122]. In this design, carbon dioxide is utilized as a solvent. All of the conditions in the

t
ip
laboratory scale were set to be constant. For the extraction of clove, the temperature is set at

cr
313K, pressure at 15 MPa, the ratio of solvent to feed is 3.59 kg CO 2 /kg clove and the extraction
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time is 130 minutes. For sugarcane residue, the extraction conditions are at temperature of

us
333K, pressure of 35 MPa, ratio of solvent to feed of 30 kg CO 2 /kg sugarcane residue and an

extraction time of 360 minutes. The scale-up yield was found to be slightly higher than that of
an
the laboratory scale (i.e., 20% higher at 130 min for clove and 15% higher at 180 min for

sugarcane residue).
M
Microwave-assisted extraction was scaled up by Filly [123] to extract essential oil from
d

rosemary. At first, the laboratory scale extraction was performed for microwave-assisted and
te

hydro-distillation extractions. The result showed that, the same extraction yield was obtained
ep

within 30 minutes of microwave-assisted extraction and 2 hours for hydro-distillation extraction.

Both methods actually have their unique advantages in that, microwave gives a good yield while
c

hydro-distillation gives qualitative aromatic profile. In order to acquire both advantages,


Ac

microwave-assisted hydro-distillation was designed and scaled up. This technique is a

combination of microwave heating and dry distillation performed at atmospheric pressure

without any added solvent or water. The objective of the study is to extract the essential oil from

rosemary on a laboratory scale and apply the same conditions to a pilot scale. The conditions

28
applied in the study included the use of 3 kg of dried rosemary, 30 W of microwave power and

30 minutes of extraction time without the use of any solvent. The microwave-assisted hydro-

distillation is a rapid technique that consumes less energy and no solvent. It is therefore

advantageous from an environmental point of view because no waste will be produced. The

t
ip
extraction schematic is shown in Fig. 5 [123].

cr
As per 2015, there are only SFE, microwave-assisted extraction and ultra-high pressure
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extraction methods in extracting plant/ herb that have been scaled up. Another method such as

us
HWE was scaled up by Kilpelainen [124] to extract sawdust. The scale-up techniques require

many considerations on why the scale-up must be done. Only promising techniques, i.e. those
an
that could yield a reasonably large amount of extracts within a short time will be chosen for

scale-up in order to make economic sense and to produce a good return on investment.
M
7.0 CONCLUSIONS
d
te

The demand for herbal products has been increasing with the increased awareness of
ep

possible side effects of using products made from chemicals. The effectiveness of natural

products has been attributed to the presence of phytochemicals as the active compounds in herbs.
c

Extraction processes are required to obtain the active ingredients that will be used in the
Ac

formulation of natural products. Appropriate solvents and cost-effective extraction processes

must be chosen to obtain the active ingredients.

Herbal/plant extraction techniques have been typically designed to achieve one or more

of the following goals – shortened extraction time, decreased solvent consumption, increased

29
extraction yield, and enhanced extract quality [57]. The most suitable method must therefore be

chosen to perform a particular extraction task. The extraction techniques described in this

review are suitable for the solid-liquid extraction of plant constituents. Among the common

methods to extract the essential oil are hydro-distillation, steam-distillation, Soxhlet and

t
ip
marinated extraction methods. These methods are effective, but can be time-consuming and

require high operating costs. For example, Soxhlet extraction, which uses a large amount of

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solvent not only requires a high operating cost but also causes additional environmental

us
problems. Some other methods described in the review required longer time to extract the

needed compound from the herbs. For instance, the traditional method of boiling herbs to obtain

an
phytochemicals requires longer extraction time. Thus, more advanced extraction methods such

as sonication-assisted extraction [125], microwave assisted extraction [97], SFE [126], ultra-high
M
pressure extraction [94, 95], hot water extraction [98, 99] and ASE [97, 127] have been used as

alternatives for to perform faster extraction and obtain higher quality yield. These techniques
d

operate at higher temperatures and/or pressures and greatly decrease the extraction time.
te

However, these specialized extraction techniques have found application in limited occasions as
ep

they require higher capital investment for the complex equipment. ASE, for example, has been

performed at high temperatures for the extraction of organic compounds that are more stable at
c

high temperature relative to other compounds that tend to denature. Research is in progress to
Ac

better understand the various extraction mechanisms with the aim to improve their efficiencies

and cost-effectiveness, to remove their limitations and to perform scale up of these techniques

for commercial-scale applications.

30
FUNDING

This work was supported by the Ministry of Education, Fundamental Research Grant Scheme

(Vote number: R.J130000.7809.4F488), Universiti Teknologi Malaysia and the Ministry of

t
ip
Education, Malaysia MyPhD scholarship. This support is gratefully acknowledged.

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CONFLICT OF INTEREST STATEMENT

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The authors have declared no conflict of interest.

REFERENCES an
M
[1] Kumoro A.C., Hasan M. (2008) Extraction of herbal components–the case for supercritical

fluid extraction. Teknik;29(3):180-183.


d

[2] Nadia M., Nazrun A., Norazlina M., Isa N., Norliza M., Ima Nirwana S. (2012) The anti-
te

inflammatory, phytoestrogenic, and antioxidative role of Labisia pumila in prevention of

postmenopausal osteoporosis. Adv. Pharmacol. Sci.;2012: article 706905, 7 pages.


ep

[3] WHO. (2003) Traditional Medicine, WHO, Geneva, Switzerland.


c

[4] Gias U. (1998) Standardization of Herbal Preparation. The Independent, Monday; May 30.
Ac

[5] Khan I.A., Smillie T. (2012) Implementing a “Quality by Design” Approach to Assure the

Safety and Integrity of Botanical Dietary Supplements. J. Natural Products;75(9):1665-1673.

[6] Aarts T. (1998) Industry Overview. Nutrition Business Journal;3(9):1-5.

31
[7] Nahin R.L., Statistics N.C.f.H. (2009) Costs of complementary and alternative medicine

(CAM) and frequency of visits to CAM practitioners. US Department of Health and Human

Services, Centers for Disease Control and Prevention, National Center for Health Statistics

Hyattsville, MD.

t
ip
[8] Frost & Sullivan. (2005) European Dietary Supplements: Health is Wealth.

https://www.frost.com/sublib/display-market-insight.do?id=38076249 consulted on Jan. 15,

cr
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

2016.

us
[9] Puteh. (1999) In A Two and Half Day course of Herbal and Phytochemical Processing. CEPP

short course notes Chemical Engineering Pilot Plant, UTM Skudai, Malaysia.
an
[10] http://www.bernama.com.my/bernama/v3/news-busines.php?id=150892 consulted on May
M
2, 2014.. .

[11] http://www.bernama.com.my/bernama/v3/news-busines.php?id=219357 Malaysian


d

National News Agency, Local Herbal Market to Hit RM8 Billion by 2010, consulted on May 2,
te

2014. .
ep

[12] Chua S.K. (2008) Monitoring the quality of essential oil from etilingera SP. 4

(Zingiberaceae) by gas chromatography-mass spectrometry (GC-MS): PhD dissertation,


c

Universiti Malaysia Pahang.


Ac

[13] Arif M.T. (2002) Traditional/Complementary Medicine in the Malaysian Healthcare

System,. Poster presented at the 4th International Conference for Traditional/Complementary

Medicine, Sunway Convention Centre, Kuala Lumpur, Indonesia.

32
[14] Lewington A. (1993) Medicinal Plants and Plant Extracts: A review of their importation

into Europe. Traffic International, Cambridge, UK.

[15] Rates S. (2001) Plants as source of drugs. Toxicon;39(5):603-613.

[16] Diallo D., Hveem B., Mahmoud M.A., Berge G., Paulsen B.S., Maiga A. (1999) An

t
ip
ethnobotanical survey of herbal drugs of Gourma district, Mali. Pharmaceutical

cr
Biology;37(1):80-91.
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

[17] Kris-Etherton P., Lefevre M., Beecher G., Gross M., Keen C., Etherton T. (2004) Bioactive

us
compounds in nutrition and health-research methodologies for establishing biological function:

an
the antioxidant and anti-inflammatory effects of flavonoids on atherosclerosis. Annual Reviews

Nutrition;24:511-538.
M
[18] Karimi E., Jaafar H.Z., Ahmad S. (2013) Antifungal, anti-inflammatory and cytotoxicity

activities of three varieties of labisia pumila benth: from microwave obtained extracts. BMC
d

Complement Altern Med; jan. 24:13-20.


te

[19] Chua L.S., Latiff N.A., Lee S.Y., Lee C.T., Sarmidi M.R., Aziz R.A. (2011) Flavonoids and
ep

phenolic acids from Labisia pumila (Kacip Fatimah). Food Chem.;127(3):1186-1192.

[20] Yamamoto Y., Gaynor R.B. (2001) Therapeutic potential of inhibition of the NF-κB
c

pathway in the treatment of inflammation and cancer. J. Clin Invest;107(2):135-142.


Ac

[21] Cushnie T., Lamb A.J. (2005) Antimicrobial activity of flavonoids. Int. J. antimicrob agents;

26(5):343-356.

33
[22] Shahidi F., Janitha P., Wanasundara P. (1992) Phenolic antioxidants. Critical Rev. Food Sci.

Nutr.;32(1):67-103.

[23] Wei H., Tye L., Bresnick E., Birt D.F. (1990) Inhibitory effect of apigenin, a plant

flavonoid, on epidermal ornithine decarboxylase and skin tumor promotion in mice. Cancer

t
ip
res;50(3):499-502.

cr
[24] Migliaccio S., Anderson J. (2003) Isoflavones and skeletal health: are these molecules ready
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

for clinical application? Osteoporosis Int.;14(5):361-368.

us
[25] Tsao R., Deng Z. (2004) Separation procedures for naturally occurring antioxidant

an
phytochemicals. J. Chromatogr B;812(1–2):85-99.

[26] Choi H.-k., Kim D.-h., Kim J.W., Ngadiran S., Sarmidi M.R., Park C.S. (2010) Labisia
M
pumila extract protects skin cells from photoaging caused by UVB irradiation. J. Biosci.

Bioeng.;109(3):291-296.
d

[27] Norhaiza M., Maziah M., Hakiman M. (2009) Antioxidative properties of leaf extracts of a
te

popular Malaysian herb, Labisia pumila. J Med Plant Res;3:217-223.


ep

[28] Sparg S., Light M., Van Staden J. (2004) Biological activities and distribution of plant

saponins. J. ethnopharmacol.;94(2):219-243.
c
Ac

[29] Emilia Nocerino M.A., Angelo A. Izzo. (2000) The aphrodisiac and adaptogenic properties

of ginseng. J Fitoterapia 71:S1-S5.

34
[30] Abdullah F., Ling S.K., Man S., Tan A.L., Tan H.P., Abdullah Z. (2012) Characterization

and identification of Labisia pumila by multi-steps infrared spectroscopy. Vibr. Spec.;62:200-

206.

[31] Tapsell L.C., Association A.M. (2006) Health benefits of herbs and spices: the past, the

t
ip
present, the future: Australasian Medical Publishing Company, Melbourne, Australia.

cr
[32] Diarmuid, J. (2004) Aspirin: The Story of a Wonder Drug. Bloomsbury publishing, London,
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

ISBN 0747570779.

us
[33] Nunn J.F. (2002) Ancient Egyptian medicine. University of Oklahoma Press, Red River

books, London.
an
[34] Karimi E., Jaafar H.Z. (2011) HPLC and GC-MS Determination of Bioactive Compounds in
M
Microwave Obtained Extracts of Three Varieties of Labisia pumila Benth.

Molecules;16(8):6791-6805.
d

[35] Karimi E., Jaafar H.Z., Ahmad S. (2011) Phytochemical analysis and antimicrobial
te

activities of methanolic extracts of leaf, stem and root from different varieties of Labisa pumila
ep

Benth. Molecules;16(6):4438-4450.

[36] Ramlan A.A., Sivakumar K., Chwan D.Y.F. (2005) Engineering aspects of herbal and
c

phytochemical processing: A Malaysian perspective. http://eprints.utm.my/5583/ consulted on


Ac

Jan. 15, 2016.

[37] Sim C., Kumaresan S., Sarmidi M.R. (2004) Mass transfer coefficients of eurycoma

longifolia batch extraction process. http://eprints.utm.my/6026/ consulted on Jan. 16, 2016.

35
[38] Bernardo-Gil M.G., Roque R., Roseiro L.B., Duarte L.C., Gírio F., Esteves P. (2011)

Supercritical extraction of carob kibbles (Ceratonia siliqua L.). The J. Supercritical

Fluids;59(0):36-42.

[39] Karale Chandrakant K., Dere Pravin J., Dhonde S., Honde Bharat S., Kote Amol P. (2011)

t
ip
A overview of supercritical fluid extraction for herbal drugs. Pharmacologyonline 2:575-596.

cr
[40] Eller F. (2002) Supercritical carbon dioxide extraction of fat. Business Briefing: Food
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

Technol:1-4.

us
[41] E. Martinelli, K. Schulz and G.A. Mansoori. (1991) Supercritical Fluid Extraction /

an
Retrograde Condensation with Applications in Biotechnology. 451-478, in "Supercritical Fluid

Technology", Edited by Bruno TJ and Ely JF. CRC Press, Boca Raton, FL.
M
[42] Geng Y., Liu J., Lv R., Yuan J., Lin Y., Wang X. (2007) An efficient method for extraction,

separation and purification of eugenol from Eugenia caryophyllata by supercritical fluid


d

extraction and high-speed counter-current chromatography. Sep Purif Technol, 57(2):237-241.


te

[43] Clifford A.A. (1993) Introduction to Supercritical fluid Extraction in Analytical Science, S.
ep

A Westwood (ed.), Supercritical fluid Extraction and Its Use in Chromatographic Sample

Preparation. CRC Press, Boca Raton, Florida:1-39.


c

[44] Lang Q., Wai C.M. (2001) Supercritical fluid extraction in herbal and natural product
Ac

studies—a practical review. Talanta; 53(4):771-782.

[45] Reverchon E., Donsi G., Sesti Osseo L. (1993) Modeling of supercritical fluid extraction

from herbaceous matrices. Ind. Eng. Chem. Res. 32(11):2721-2726.

36
[46] Polesello S., Lovati F., Rizzolo A., Rovida C. (1993) Supercritical fluid extraction as a

preparative tool for strawberry aroma analysis. J. High Res Chromatogr. 16(9):555-559.

[47] Dron A., Guyeru D.E., Gage D.A., Lira C.T. (1997) Yield and quality of onion flavor oil

obtained by supercritical fluid extraction and other methods. J. Food Proc. Eng. 20(2):107-124.

t
ip
[48] Pan W.H., Chang C.-C., Su T.-T., Lee F., Fuh M.-R.S. (1995) Preparative supercritical fluid

cr
extraction of pyrethrin I and II from pyrethrum flower. Talanta; 42(11):1745-1749.
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

[49] Fuh M.-R., Pan W., Hsieh I., CHUO C.-M. (1995) Preparative-scale supercritical fluid

us
extraction of essential oils from Syzygium aromaticum (clove bud). Am. Lab.. 27(18):36-41.

an
[50] Frenich A.G., Romero-González R., del Mar Aguilera-Luiz M. (2014) Comprehensive

analysis of toxics (pesticides, veterinary drugs and mycotoxins) in food by UHPLC-MS. TrAC
M
Trends Anal. Chem 63:158-169.

[51] Marsili R., Callahan D. (1993) Comparison of a liquid solvent extraction technique and
d

supercritical fluid extraction for the determination of α-and β-carotene in vegetables. J.


te

Chromatogr. Sci. 31(10):422-428.


ep

[52] Veggi P.C., Martinez J., Meireles M.A.A. (2013) Fundamentals of Microwave Extraction

Microwave-assisted Extraction for Bioactive Compounds: Springer; Berlin, p. 15-52.


c
Ac

[53] Chemat F., Abert-Vian M., Zill-e-Huma Y. (2009) Microwave assisted separations: green

chemistry in action. Green chemistry research trends Nova Science Publishers, New York,

pp.33-62.

37
[54] Camel V. (2001) Recent extraction techniques for solid matrices—supercritical fluid

extraction, pressurized fluid extraction and microwave-assisted extraction: their potential and

pitfalls. Analyst;126(7):1182-1193.

[55] Thostenson E., Chou T.-W. (1999) Microwave processing: fundamentals and applications.

t
ip
Composites Part A: Applied Sci. Manufact. 30(9):1055-1071.

cr
[56] Laghari A.Q., Memon S., Nelofar A., Laghari A.H. (2011) Extraction, identification and
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

antioxidative properties of the flavonoid-rich fractions from leaves and flowers of Cassia

us
angustifolia. American J. Anal. Chem.;2(8):871-878.

an
[57] Wang L., Weller C.L. (2006) Recent advances in extraction of nutraceuticals from plants.

Trends in Food Sci. Technol. 17(6):300-312.


M
[58] Chen L., Jin H., Ding L., Zhang H., Li J., Qu C., Zhang H. (2008) Dynamic microwave-

assisted extraction of flavonoids from Herba Epimedii. Sep. Purif. Technol. 59(1):50-57.
d

[59] Azmin S.N.H.M., Yunus N.A., Mustaffa A.A., Wan Alwi S.R., Chua L.S. (2015) A
te

Framework For Solvent Selection Based on Herbal Extraction Process Design. J. Eng. Sci.
ep

Technol. (Special Issue on SOMCHE 2014 Conference) 1:25-34

[60] Zhang H.-F., Yang X.-H., Zhao L.-D., Wang Y. (2009) Ultrasonic-assisted extraction of
c

epimedin C from fresh leaves of Epimedium and extraction mechanism. Innovative Food Sci.
Ac

Emerg. Technol. 10(1):54-60.

[61] Gao M., Huang W., RoyChowdhury M., Liu C. (2007) Microwave-assisted extraction of

scutellarin from Erigeron breviscapus Hand-Mazz and its determination by high-performance

liquid chromatography. Anal. Chim. Acta 591(2):161-166.

38
[62] Li H., Pordesimo L., Weiss J., Wilhelm L. (2004) Microwave and ultrasound assisted

extraction of soybean oil. Transactions of the ASAE;47(4):1187-94.

[63] Guo Z., Jin Q., Fan G., Duan Y., Qin C., Wen M. (2001) Microwave-assisted extraction of

effective constituents from a Chinese herbal medicine Radix puerariae. Anal. Chim. Acta

t
ip
436(1):41-47.

cr
[64] Li J., Zu Y.-G., Fu Y.-J., Yang Y.-C., Li S.-M., Li Z.-N., Wink M. (2010) Optimization of
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

microwave-assisted extraction of triterpene saponins from defatted residue of yellow horn

us
(Xanthoceras sorbifolia Bunge.) kernel and evaluation of its antioxidant activity. Innovative

Food Sci. Emerg. Technol. 11(4):637-643.


an
[65] Spigno G., De Faveri D. (2009) Microwave-assisted extraction of tea phenols: A
M
phenomenological study. J. Food Engin. 93(2):210-217.

[66] Ballard T.S., Mallikarjunan P., Zhou K., O’Keefe S. (2010) Microwave-assisted extraction
d

of phenolic antioxidant compounds from peanut skins. Food Chem. 120(4):1185-1192.


te

[67] Chen Y., Xie M.-Y., Gong X.-F. (2007) Microwave-assisted extraction used for the
ep

isolation of total triterpenoid saponins from Ganoderma atrum. J. Food Engin. 81(1):162-170.

[68] Sandri I., Zacaria J., Fracaro F., Delamare A., Echeverrigaray S. (2007) Antimicrobial
c

activity of the essential oils of Brazilian species of the genus Cunila against foodborne pathogens
Ac

and spoiling bacteria. Food Chem. 103(3):823-828.

[69] Sökmen A., Vardar‐Ünlü G., Polissiou M., Daferera D., Sökmen M., Dönmez E. (2003)

Antimicrobial activity of essential oil and methanol extracts of Achillea sintenisii Hub.

Mor.(Asteraceae). Phytotherapy Res. 17(9):1005-1010.

39
[70] Deba F., Xuan T.D., Yasuda M., Tawata S. (2008) Chemical composition and antioxidant,

antibacterial and antifungal activities of the essential oils from Bidens pilosa Linn. var. Radiata.

Food control; 19(4):346-352.

[71] Cravotto G., Boffa L., Mantegna S., Perego P., Avogadro M., Cintas P. (2008) Improved

t
ip
extraction of vegetable oils under high-intensity ultrasound and/or microwaves. Ultrason.

Sonochem. 15(5):898-902.

cr
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

[72] Huie C.W. (2002) A review of modern sample-preparation techniques for the extraction and

us
analysis of medicinal plants. Anal. Bioanal Chem. 373(1-2):23-30.

an
[73] Soria A.C., Villamiel M. (2010) Effect of ultrasound on the technological properties and

bioactivity of food: a review. Trends in Food Sci. Technol. 21(7):323-331.


M
[74] Pico Y. ( 2012) Chemical Analysis of Food: Techniques and Applications, . Elsevier,

Oxford, UK.
d

[75] Chemat F., Khan M.K. (2011) Applications of ultrasound in food technology: processing,
te

preservation and extraction. Ultrason. Sonochem. 18(4):813-835.


ep

[76] Awad T., Moharram H., Shaltout O., Asker D., Youssef M. (2012) Applications of

ultrasound in analysis, processing and quality control of food: A review. Food Res. Int.
c

48(2):410-427.
Ac

[77] Patist A., Bates D. (2008) Ultrasonic innovations in the food industry: from the laboratory to

commercial production. Inn. Food Sci. Emerg. Technol. 9(2):147-154.

40
[78] Chandrapala J., Oliver C.M., Kentish S., Ashokkumar M. (2013) Use of Power Ultrasound

to Improve Extraction and Modify Phase Transitions in Food Processing. Food Rev. Int.

29(1):67-91.

[79] Romdhane M., Gourdon C. (2002) Investigation in solid–liquid extraction: influence of

t
ip
ultrasound. Chem. Engin. J. 87(1):11-19.

cr
[80] Tatke P., Jaiswal Y. (2011) An overview of microwave assisted extraction and its
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

applications in herbal drug research. Res. J Med. Plant. 5:21-31.

us
[81] Pihie L., Hawariah A., Zakaria Z.A., Othman F. (2012) Antiproliferative and Proapoptotic

an
Effects of Labisia pumila Ethanol Extract and Its Active Fraction in Human Melanoma HM3KO

Cells. Evidence-Based Complementary and Alternative Medicine; article ID 123470,


M
doi:10.1155/2012/123470.

[82] Luque de Castro M., Garcıa-Ayuso L. (1998) Soxhlet extraction of solid materials: an
d

outdated technique with a promising innovative future. Anal. Chim. Acta 369(1):1-10.
te

[83] Luque de Castro M., Priego-Capote F. (2010) Soxhlet extraction: Past and present panacea.
ep

J. Chromatogr. A. 1217(16):2383-2389.

[84] Zarnowski R., Suzuki Y. (2004) Expedient Soxhlet extraction of resorcinolic lipids from
c

wheat grains. J. Food Comp. Anal. 17(5):649-663.


Ac

[85] Mamidipally P.K., Liu S.X. (2004) First approach on rice bran oil extraction using

limonene. Eur. J. Lipid Sci. Technol. 106(2):122-125.

41
[86] Hanmoungjai P., Pyle L., Niranjan K. (2000) Extraction of rice bran oil using aqueous

media. J. chem. Technol. Biotechnol. 75(5):348-352.

[87] Wu X., Ge X., Liang S., Lv Y., Sun H. (2014) A Novel Selective Accelerated Solvent

Extraction for Effective Separation and Rapid Simultaneous Determination of Six

t
ip
Anthraquinones in Tartary Buckwheat and Its Products by UPLC–DAD. Food Anal.

Methods:7(2):1-9.

cr
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

[88] Zhu H., Wang Y., Liu Y., Xia Y., Tang T. (2010) Analysis of flavonoids in Portulaca

us
oleracea L. by UV–vis spectrophotometry with comparative study on different extraction

technologies. Food Anal. Methods;3(2):90-97.


an
[89] Grosso C., Cardoso M.T., Figueiredo A., Moldão-Martins M., Burillo J., Urieta J., Barroso
M
J., Coelho J., Palavra A. (2007) Supercritical fluid extraction, Hydrodistillation and Soxhlet

extraction of the aerial part of winter savory. Proceedings 528 of European Congress of
d

Chemical Engineering (ECCE-6) Copenhagen, 16-20 September 2007.


te

[90] Gao X., Yani S., Wu H. (2014) Pyrolysis of Spent Biomass from Mallee Leaf Steam
ep

Distillation: Biochar Properties and Recycling of Inherent Inorganic Nutrients. Energy &

Fuels;28(7):4642-4649.
c

[91] Ridgway K., Lalljie S.P., Smith R.M. (2007) Sample preparation techniques for the
Ac

determination of trace residues and contaminants in foods. J. Chromatogr. A;1153:36-53.

[92] Jun X., Deji S., Ye L., Rui Z. (2011) Micromechanism of ultrahigh pressure extraction of

active ingredients from green tea leaves. Food Control. 22(8):1473-1476.

[93] von Rohr P.R., Trepp C. (1996) High pressure chemical engineering: Elsevier, Amsterdam.

42
[94] Xi J., Shen D., Zhao S., Lu B., Li Y., Zhang R. (2009) Characterization of polyphenols from

green tea leaves using a high hydrostatic pressure extraction. Int. J. Pharm. 382:139-143.

[95] Shouqin Z., Junjie Z., Changzhen W. (2004) Novel high pressure extraction technology. Int.

J. Pharm. 278:471-474.

t
ip
[96] Giergielewicz-Możajska H., Dąbrowski Ł., Namieśnik J. (2001) Accelerated solvent

cr
extraction (ASE) in the analysis of environmental solid samples—some aspects of theory and
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

practice. Critical Rev. Anal. Chem. 31(3):149-165.

us
[97] Kaufmann B., Christen P. (2002) Recent extraction techniques for natural products:

an
microwave-assisted extraction and pressurized solvent extraction. Phytochem. Anal. 13(2):105-

113.
M
[98] Ayala R.S., De Castro M.L. (2001) Continuous subcritical water extraction as a useful tool

for isolation of edible essential oils. Food chem.. 75(1):109-113.


d

[99] Ozel M.Z., Gogus F., Lewis A.C. (2003) Subcritical water extraction of essential oils from
te

Thymbra spicata. Food Chem. 82(3):381-386.


ep

[100] Eikani M.H., Golmohammad F., Rowshanzamir S. (2007) Subcritical water extraction of

essential oils from coriander seeds (Coriandrum sativum L.). J. Food Eng. 80(2):735-740.
c
Ac

[101] Jimenez-Carmona M., Ubera J., de Castro M.L. (1999) Comparison of continuous

subcritical water extraction and hydrodistillation of marjoram essential oil. J. Chromatogr. A.

855(2):625-632.

43
[102] Saim N., Osman R., Yasin W.A.H.M., Hamid R.D. (2008) Subcritical water extraction of

essential oil from coriander (Coriandrum sativum L.) seeds. The Malaysian J. Anal. Sci.

12(1):35-41.

[103] Ehlers D., Nguyen T., Quirin K., Gerard D. (2001) Analysis of essential basil oils-CO2

t
ip
extracts and steam-distilled oils. Deutsche Lebensmittel-Rundschau;97(7):245-250.

cr
[104] Özer E.f.Ö., İin S.P., Akman U., Hortaçsu Ö. (1996) Supercritical carbon dioxide
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

extraction of spearmint oil from mint‐plant leaves. The Canadian J. Chem. Eng. 74(6):920-928.

us
[105] Bravi E., Perretti G., Montanari L., Favati F., Fantozzi P. (2007) Supercritical fluid

an
extraction for quality control in beer industry. J. supercritic. Fluids 42(3):342-346.

[106] Mansoori G.A., Schulz K., Martinelli E.E. (1988) Bioseparation using supercritical fluid
M
extraction/retrograde condensation. Nature Biotech. 6(4):393-396.

[107] Hawthorne S.B., Rickkola M.-L., Screnius K., Holm Y., Hiltunen R., Hartonen K. (1993)
d

Comparison of hydrodistillation and supercritical fluid extraction for the determination of


te

essential oils in aromatic plants. J. Chromatogr. A;634(2):297-308.


ep

[108] Rezazadeh Sh B.-a.B.Z.B.F., Vatanara A, Behbahani B, Rouholamini Najafabadi A,

Maleky-Doozzadeh M, Yarigar-Ravesh M, Pirali Hamedani M. , . (2008) Comparison of Super


c

Critical Fluid Extraction and Hydrodistillation Methods on Lavander‘s Essential Oil


Ac

Composition and Yield. . J. Med. Plants; 7 (Supplement No. 4,):63-68.

[109] Zhang H.-F., Yang X.-H., Wang Y. (2011) Microwave assisted extraction of secondary

metabolites from plants: Current status and future directions. Trends Food Sci. Technol.

22(12):672-688.

44
[110] Sticher O. (2008) Natural product isolation. Natural product reports;25(3):517-554.

[111] Abdul Kadir A., Nik Hussain N.H., Wan Bebakar W.M., Mohd D.M., Wan Mohammad

W.M.Z., Hassan I.I., Shukor N., Kamaruddin N.A., Wan Mohamud W.N. (2012) The Effect of

Labisia pumila var. alata on Postmenopausal Women: A Pilot Study. Evidence-Based

t
ip
Complementary and Alternative Medicine; article ID 216525, doi:10.1155/2012/216525.

cr
[112] Binic I., Lazarevic V., Ljubenovic M., Mojsa J., Sokolovic D. (2013) Skin ageing: natural
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

weapons and strategies. Evidence-Based Complementary and Alternative Medicine; article ID

us
827248, doi:10.1155/2013/827248.

an
[113] Shiffman M.A., Mirrafati S.J., Lam S.M. (2008) Simplified facial rejuvenation: Springer,

Berlin.
M
[114] Hunt K.J., Hung S.K., Ernst E. (2010) Botanical Extracts as Anti-Aging Preparations for

the Skin. Drugs & aging; 27(12):973-985.


d

[115] Santos D.T., Veggi P.C., Meireles M.A.A. (2012) Optimization and economic evaluation
te

of pressurized liquid extraction of phenolic compounds from jabuticaba skins. J. Food Eng.
ep

108(3):444-452.

[116] Prado J.M., Dalmolin I., Carareto N.D., Basso R.C., Meirelles A.J., Oliveira J.V., Batista
c

E.A., Meireles M.A.A. (2012) Supercritical fluid extraction of grape seed: process scale-up,
Ac

extract chemical composition and economic evaluation. J. Food Eng. 109(2):249-257.

[117] Reverchon E., Marrone C. (1997) Supercritical extraction of clove bud essential oil:

isolation and mathematical modeling. Chem. Eng. Sci. 52(20):3421-3428.

45
[118] Molero Gómez A., Pereyra López C., Martinez de la Ossa E. (1996) Recovery of grape

seed oil by liquid and supercritical carbon dioxide extraction: a comparison with conventional

solvent extraction. Chem. Biochem. Eng. J. 61(3):227-231.

[119] Rosa P.T., Meireles M.A.A. (2005) Rapid estimation of the manufacturing cost of extracts

t
ip
obtained by supercritical fluid extraction. J. Food Eng. 67(1):235-240.

cr
[120] Fiori L. (2010) Supercritical extraction of grape seed oil at industrial-scale: plant and
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

process design, modeling, economic feasibility. Chem. Eng. Proc.: Process Intensification.

us
49(8):866-872.

an
[121] del Valle J.M., Rivera O., Mattea M., Ruetsch L., Daghero J., Flores A. (2004)

Supercritical CO 2 processing of pretreated rosehip seeds: effect of process scale on oil


M
extraction kinetics. J. supercritical fluids. 31(2):159-174.

[122] Prado J.M., Prado G.H., Meireles M.A.A. (2011) Scale-up study of supercritical fluid
d

extraction process for clove and sugarcane residue. J. Supercritical Fluids.56(3):231-237.


te

[123] Filly A., Fernandez X., Minuti M., Visinoni F., Cravotto G., Chemat F. (2014) Solvent-
ep

free microwave extraction of essential oil from aromatic herbs: From laboratory to pilot and

industrial scale. Food chem.. 150:193-198.


c

[124] Kilpelainen P.O., Hautala S.S., Byman O.O., Tanner L.J., Korpinen R.I., Lillandt M.K.J.,
Ac

Pranovich A.V., Kitunen V.H., Willfor S.M., Ilvesniemi H.S. (2014) Pressurized hot water flow-

through extraction system scale up from the laboratory to the pilot scale. Green Chem.

16(6):3186-3194.

46
[125] Vinatoru M. (2001) An overview of the ultrasonically assisted extraction of bioactive

principles from herbs. Ultrason. Sonochem. 8(3):303-313.

[126] Meireles M.A.A. (2003) Supercritical extraction from solid: process design data (2001–

2003). Cur. Op. Solid State Mat. Sci. 7(4):321-330.

t
ip
[127] Smith R.M. (2002) Extractions with superheated water. J. Chromatogr. A. 975(1):31-46.

cr
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

Figure 1: The 10 extraction

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methods described in the

text.

an
M
d
te
c ep
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47
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Soxhlet

apparatus
Figure 2:

extraction
Ac
cep
te
d

48
M
an
us
cr
ip
t
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Ac
cep
te
d

49
M
an
us
cr
ip
t
Figure 3: Hydro-distillation extraction equipment.

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cr
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an
M
d
te
ep
c

Figure 4: Steam distillation extraction set-up.


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50
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Ac
cep
te
d

51
M
an
Figure 5: Solvent-free microwave extraction: from laboratory to pilot scale.
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cr
ip
t
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Ac
cep
te
d

52
M
an
us
cr
ip
t
Table 1: General guidelines for harvesting various plant parts

Plant part to be collected Harvesting stage

Whole plant or aerial part Initial flowering.

t
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Full maturity. The maturity stage of the species must be first

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Roots or rhizomes
determined.

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Leaves Fully developed leaves.

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At the beginning of the rainy season. The maturity stage of the
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Stems or bark
species must first be determined.
d

Wood Toward the end of the rainy season.


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Flowers At the beginning of the blooming period.


ep

Fruit Fully matured.


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Seeds Fully matured fruit.

53
Table 2: Advantages and disadvantages of various extraction methods

Type of
Advantages Disadvantages
Extraction

t
ip
Solvent (CO 2 ) is inexpensive
Supercritical
Loss of desired compounds with

cr
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fluid Solvent recycling can be achieved for


improper solvent selection

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extraction, all methods
Specialized equipment is required
SFE
Pure extraction yield can be attained
an Efficiency of microwaves is very poor
M
for nonpolar target compounds or
Applicable for both industrial and
solvents or for extremely viscous
d

Microwave
laboratory scales
solvents
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Assisted
Less time consuming than
extraction, Not appropriate for heat sensitive
ep

conventional methods
MAE compounds
c

Can provide high returns on capital


Expensive equipment and difficult to
Ac

investment
operate

Sonication Efficient tool for large-scale The active part of ultrasound is only

54
extraction commercial applications the vicinity of the ultrasonic emitter

Reduced working time and easy to Presence of a dispersed phase

handle contributes to the ultrasound wave

attenuation

t
Increased yield, reduced solvent

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consumption, and high extract quality Weak effect on the extraction of oil

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us
Requires excessive extraction times

Uses large amounts of extractants

Soxhlet
an
Very simple and inexpensive method (solvent)
M
Temperature in the extraction system No agitation that can accelerates the
extraction
can be maintained process
d

Thermal decomposition of heat


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sensitive compound
ep

No specific place is needed


Marinated Prolonged time period is required to
c

extraction obtain the products


Heat supply is not needed
Ac

Prolonged time period is necessary to


Hydro-
separate water from product
distillation Inexpensive method because of no

55
extraction organic solvent is required No agitation to accelerate the process

Risk of thermal degradation

Energy consuming

t
ip
Steam-

cr
Can extract water insoluble No agitation needed to accelerate the
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

distillation
compound process

us
extraction

Ultra-high

pressure Short extraction time


an Compound impurity issue
M
extraction
d

Potential alternative technique to SFE


te

for the extraction of Only suitable for the extraction of high


Accelerated
ep

temperature stable compound.


solvent polar compounds

extraction
Reduce solvent consumption and
c

extraction time
Ac

Hot water Inexpensive method because no Not suitable for heat sensitive

extraction organic solvent is required compounds.

56
Extract essential oil with high

oxygenated components

Substantial saving of both energy and

investment cost

t
ip
cr
Downloaded by [Universiti Teknologi Malaysia] at 00:34 26 January 2016

us
an
M
d
te
c ep
Ac

57

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