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USP 40 Official Monographs / Eugenol 4125

ADDITIONAL REQUIREMENTS Analysis

PACKAGING AND STORAGE: Preserve in single-dose or mul-
tiple-dose containers of Type I glass.
LABELING: Label it to indicate that it must be diluted with
suitable parenteral vehicle before intravenous infusion.
USP REFERENCE STANDARDS 11
USP Endotoxin RS
USP Etoposide RS
USP Etoposide Resolution Mixture RS
.
Samples: Sample solution and Blank
[NOTEIdentify any peaks from the Sample solution that
correspond to those in the Blank by their retention
times.]
Calculate the percentage of eucalyptol (C10H18O) in the
portion of Eucalyptol taken:
Result = (rU/rT) 100
rU = peak response of eucalyptol from the Sample
solution
rT = sum of all peak responses from the Sample
solution, other than the responses

Eucalyptol corresponding to those of the Blank

Acceptance criteria: 98.0%100.0%
IMPURITIES
LIMIT OF PHENOLS
Analysis 1: Shake 5 mL with 5 mL of sodium hydroxide
C10H18O 154.25 TS.
1,3,3-Trimethyl-2-oxabicyclo[2.2.2]octane; Acceptance criteria 1: The volume of Eucalyptol is not
1,8-Epoxy-p-menthane [470-82-6]. diminished.
Analysis 2: Shake 1 mL with 20 mL of water and allow
DEFINITION the liquids to separate. To 10 mL of the water layer add
Eucalyptol is obtained from oil of eucalyptus and from other 1 drop of ferric chloride TS.
sources. It contains NLT 98.0% and NMT 100.0% of Acceptance criteria 2: The mixture develops no violet
C10H18O. color.
IDENTIFICATION SPECIFIC TESTS
A. INFRARED ABSORPTION 197F SPECIFIC GRAVITY 841: 0.9210.924
B. Add 1 mL of phosphoric acid to 1 mL of Eucalyptol CONGEALING TEMPERATURE 651: NLT 0
contained in a test tube maintained in an ice bath. A OPTICAL ROTATION, Angular Rotation 781A: 0.5 to
solid white crystalline mass is formed, from which euca- +0.5
lyptol separates upon addition of warm water. DISTILLING RANGE, Method I 721: 174177
REFRACTIVE INDEX 831: 1.4551.460 at 20
ASSAY
PROCEDURE ADDITIONAL REQUIREMENTS
PACKAGING AND STORAGE: Preserve in tight containers.

USP Monographs
System suitability solution: 0.2 mg/mL of limonene
and 0.9 mg/mL of USP Eucalyptol RS in methanol USP REFERENCE STANDARDS 11
Sample solution: 0.9 mg/mL of Eucalyptol in methanol USP Eucalyptol RS
Blank: Methanol
Chromatographic system
(See Chromatography 621, System Suitability.)
Mode: GC .

Detector: Flame ionization Eugenol

Column: 0.32-mm 60-m fused-silica capillary col-
umn coated with phase G16
Temperature
Injector port: 250
Detector: 250
Column: See Table 1.
C10H12O2 164.20
Table 1 Phenol, 2-methoxy-4-(2-propenyl)-;
4-Allyl-2-methoxyphenol [97-53-0].
Hold Time
Initial Temperature Final at Final DEFINITION
Temperature Ramp Temperature Temperature Eugenol is obtained from clove oil and from other sources.
() (/min) () (min)
60 6 200 IDENTIFICATION
A. INFRARED ABSORPTION 197F
Split flow rate: 50 mL/min
Carrier gas: Helium IMPURITIES
Column head pressure: 30 psi
Injection size: 1 L Delete the following:
System suitability
Sample: System suitability solution HEAVY METALS, Method II 231: NMT 40 ppm (Official 1-
Suitability requirements
.

Jan-2018)
Resolution: NLT 2.0 between limonene and HYDROCARBONS
eucalyptol Analysis: Dissolve 1 mL in 20 mL of 0.5 N sodium hy-
Column efficiency: NLT 150,000 theoretical plates, droxide in a 50-mL stoppered tube, add 18 mL of
eucalyptol water, and mix.
Acceptance criteria: A clear mixture results immedi-
ately, but it may become turbid when exposed to air.

Official from May 1, 2017

Copyright (c) 2017 The United States Pharmacopeial Convention. All rights reserved.
 Accessed from 10.6.1.1 by clar1 on Fri Apr 28 14:43:24 EDT 2017

4126 Eugenol / Official Monographs USP 40

LIMIT OF PHENOL Sample solution: 0.1 mg/mL of Exemestane in Diluent

Analysis: Shake 1 mL with 20 mL of water. Filter, and Chromatographic system
add 1 drop of ferric chloride TS to 5 mL of the clear (See Chromatography 621, System Suitability.)
filtrate. Mode: LC
Acceptance criteria: The mixture exhibits a transient Detector: UV 247 nm
grayish-green color but not a blue or violet color. Column: 4.6-mm 15-cm; 3-m packing L1
Column temperature: 45
SPECIFIC TESTS Flow rate: 1.0 mL/min
SPECIFIC GRAVITY 841: 1.0641.070 Injection volume: 10 L
DISTILLING RANGE, Method II 721: NLT 95% distills from System suitability
250255 Sample: Standard solution
REFRACTIVE INDEX 831: 1.5401.542 at 20 Suitability requirements
SOLUBILITY IN 70% ALCOHOL: One volume dissolves in 2 Relative standard deviation: NMT 0.73%
volumes of 70% alcohol. Analysis
Samples: Standard solution and Sample solution
ADDITIONAL REQUIREMENTS Calculate the percentage of exemestane (C20H24O2) in
PACKAGING AND STORAGE: Preserve in tight, light-resistant the portion of Exemestane taken:
containers.
USP REFERENCE STANDARDS 11 Result = (rU/rS) (CS/CU) 100
USP Eugenol RS
rU = peak response of exemestane from the Sample
solution
rS = peak response of exemestane from the
.

Standard solution
Exemestane CS = concentration of USP Exemestane RS in the
Standard solution (mg/mL)
CU = concentration of Exemestane in the Sample
solution (mg/mL)
Acceptance criteria: 97.0%102.0% on the anhydrous
and solvent-free basis
IMPURITIES
RESIDUE ON IGNITION 281: NMT 0.2%
ORGANIC IMPURITIES
C20H24O2 296.40 Solution A: Water
Androsta-1,4-diene-3,17-dione, 6-methylene-; Solution B: Acetonitrile
6-Methyleneandrosta-1,4-diene-3,17-dione [107868-30-4]. Mobile phase: See Table 2. Return to original condi-
tions and re-equilibrate the system.
USP Monographs

DEFINITION
Exemestane contains NLT 97.0% and NMT 102.0% of ex-
emestane (C20H24O2), calculated on the anhydrous and Table 2
solvent-free basis. Time Solution A Solution B
(min) (%) (%)
IDENTIFICATION
0 75 25
A. INFRARED ABSORPTION 197K
B. The retention time of the major peak of the Sample 30 55 45
solution corresponds to that of the Standard solution, as 40 5 95
obtained in the Assay. 45 5 95

ASSAY Diluent: Acetonitrile and water (3:1)

PROCEDURE System suitability solution: 1 mg/mL of USP Exemes-
Solution A: Water tane RS, 0.01 mg/mL of USP Exemestane Related Com-
Solution B: Acetonitrile pound B RS, and 0.01 mg/mL of USP Exemestane Re-
Mobile phase: See Table 1. lated Compound C RS in Diluent
Sensitivity solution: 0.5 g/mL each of USP Exemes-
Table 1 tane RS, USP Exemestane Related Compound B RS, and
USP Exemestane Related Compound C RS in Diluent
Time Solution A Solution B Standard solution: 5 g/mL of USP Exemestane RS in
(min) (%) (%) Diluent
0 60 40 Sample solution: 1 mg/mL of Exemestane in Diluent.
15 60 40 The concentration is calculated on the anhydrous and
18 10 90 solvent-free basis.
28 10 90 Chromatographic system
(See Chromatography 621, System Suitability.)
30 60 40
Mode: LC
35 60 40 Detector: UV 247 nm
Column: 4.6-mm 25-cm; 3.5-m packing L1
Diluent: Acetonitrile and water (1:1) Column temperature: 40
Standard solution: 0.1 mg/mL of USP Exemestane RS Flow rate: 1.2 mL/min
in Diluent Injection volume: 10 L
System suitability
Samples: System suitability solution, Sensitivity solution,
and Standard solution
Suitability requirements
Resolution: NLT 2.0 between exemestane related
compound B and exemestane related compound C;

Official from May 1, 2017

Copyright (c) 2017 The United States Pharmacopeial Convention. All rights reserved.