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778 / 6-Methyl-5-hepten-2-one / Monographs FCC 9

Monographs

6-Methyl-5-hepten-2-one

Boiling Point: ∼300°

Methyl β-Naphthyl Ketone
.

Solubility in Alcohol, Appendix VI: One g dissolves in 5

First Published: Prior to FCC 6 mL of 95% alcohol.
Function: Flavoring agent
2-Acetonaphthone IDENTIFICATION
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Appendix IIIC
Sample preparation: Mineral oil mull
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
C12H10O Formula wt 170.21 those of the spectrum below.
FEMA: 2723
UNII: 21D49LOP2T [2-acetonaphthone] ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
DESCRIPTION XI.
Methyl β-Naphthyl Ketone occurs as a white or nearly white Acceptance criteria: NLT 99.0% of C12H10O
crystalline solid.
Odor: Orange blossom
Solubility: Soluble in most fixed oils; slightly soluble in
propylene glycol; insoluble or practically insoluble in
glycerin
 FCC 9 Monographs / Methyl 2-Octynoate / 779

OTHER REQUIREMENTS
• SOLIDIFICATION POINT, Appendix IIB
Acceptance criteria: NLT 53°

Monographs
Methyl β-Naphthyl Ketone (Mineral Oil Mull)

Acceptance criteria: NMT 2.0

Methyl 2-Methylbutyrate
.

• REFRACTIVE INDEX, Appendix II: At 20°

First Published: Prior to FCC 6 Acceptance criteria: Between 1.393 and 1.397
• SPECIFIC GRAVITY: Determine at 25° by any reliable
method (see General Provisions).
Methyl 2-Methylbutanoate
Acceptance criteria: Between 0.879 and 0.883

Methyl 2-Octynoate
.

C6H12O2 Formula wt 116.16 First Published: Prior to FCC 6

FEMA: 2719
UNII: OLG4D4939V [methyl 2-methylbutyrate] Methyl Heptine Carbonate

DESCRIPTION
Methyl 2-Methylbutyrate occurs as an almost colorless
liquid.
Odor: Sweet, fruity, apple
Solubility: Soluble in alcohol, most fixed oils; insoluble or C9H14O2 Formula wt 154.21
practically insoluble in water FEMA: 2729
Boiling Point: ∼115° UNII: 0TTP6YT2T3 [methyl heptine carbonate]
Function: Flavoring agent
DESCRIPTION
ASSAY Methyl 2-Octynoate occurs as a colorless to slightly yellow
• PROCEDURE: Proceed as directed under M-1b, Appendix
liquid.
XI.
Odor: Powerful, unpleasant, violet when diluted
Acceptance criteria: NLT 92.0% of C6H12O2
Solubility: Soluble in most fixed oils; slightly soluble in
SPECIFIC TESTS propylene glycol; insoluble or practically insoluble in
• ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL glycerin
OILS), M-15, Appendix XI Boiling Point: ∼217°
 780 / Methyl 2-Octynoate / Monographs FCC 9

Solubility in Alcohol, Appendix VI: One mL dissolves in 5 SPECIFIC TESTS

mL of 70% alcohol. • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
Function: Flavoring agent OILS), M-15, Appendix XI
Acceptance criteria: NMT 1.0
IDENTIFICATION • REFRACTIVE INDEX, Appendix II: At 20°
• INFRARED SPECTRA, Spectrophotometric Identification Tests, Acceptance criteria: Between 1.446 and 1.449
Appendix IIIC • SPECIFIC GRAVITY: Determine at 25° by any reliable
Acceptance criteria: The spectrum of the sample method (see General Provisions).
exhibits relative maxima at the same wavelengths as Acceptance criteria: Between 0.919 and 0.924
those of the spectrum below.
Monographs

OTHER REQUIREMENTS
ASSAY • CHLORINATED COMPOUNDS, Appendix VI
• PROCEDURE: Proceed as directed under M-1b, Appendix Acceptance criteria: Passes test
XI.
Acceptance criteria: NLT 96.0% of C9H14O2

Methyl 2-Octynoate

Function: Flavoring agent

Methyl Acetate
.

IDENTIFICATION
First Published: Prior to FCC 6
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Appendix IIIC
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

C3H6O2 Formula wt 74.08 ASSAY

FEMA: 2676 • PROCEDURE: Proceed as directed under M-1b, Appendix
UNII: W684QT396F [methyl acetate] XI.
Acceptance criteria: NLT 98.0% of C3H6O2
DESCRIPTION
Methyl Acetate occurs as a colorless liquid. SPECIFIC TESTS
Odor: Ethereal, fruity • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
Boiling Point: ∼57.5° OILS), M-15, Appendix XI
Solubility in Alcohol, Appendix VI: One mL dissolves in 1 Acceptance criteria: NMT 1.0
mL of 95% alcohol.
 FCC 9 Monographs / Methyl Alcohol / 781

• REFRACTIVE INDEX, Appendix II: At 20° • SPECIFIC GRAVITY: Determine at 25° by any reliable
Acceptance criteria: Between 1.358 and 1.363 method (see General Provisions).
Acceptance criteria: Between 0.927 and 0.932

Monographs
Methyl Acetate

Organic Impurities
Methyl Alcohol
.

• ACETONE AND ALDEHYDES

First Published: Prior to FCC 6 Sample: 1.25 mL
Control: 30 µg acetone
Analysis: To the Sample, add 3.75 mL of water and 5.0
Methanol
mL of alkaline mercuric-potassium iodide TS. Repeat
CH3OH Formula wt 32.04 the preceding using the Control.
CAS: [67-56-1] Acceptance criteria: Any turbidity produced by the
UNII: Y4S76JWI15 [methyl alcohol] Sample does not exceed that produced by the Control.
(NMT 0.003%)
DESCRIPTION
Methyl Alcohol occurs as a clear, colorless, flammable liquid. SPECIFIC TESTS
It is miscible with water, with ethyl alcohol, and with ether. • ACIDITY (AS FORMIC ACID)
Its refractive index at 20° is about 1.329. Sample: 19 mL (about 15 g)
Function: Extraction solvent Analysis: Add 0.5 mL phenolphthalein TS to a mixture
Packaging and Storage: Store in tight containers remote of 10 mL of alcohol and 25 mL of water, and titrate
from heat, sparks, and open flames. with 0.02 N sodium hydroxide to the first pink color
that persists for at least 30 s. Add the Sample, mix, and
ASSAY titrate with 0.02 N sodium hydroxide until the pink
• SPECIFIC GRAVITY: Determine by any reliable method (see
color is restored.
General Provisions).
Acceptance criteria: NMT 0.25 mL of 0.02 N sodium
Acceptance criteria: NMT 0.7893 at 25°/25°
hydroxide is required to restore the pink color (NMT
(equivalent to 0.7928 at 20°/ 20°), corresponding to
0.0015%).
NLT 99.85% of CH3OH, by weight
• ALKALINITY (AS NH3)
IMPURITIES Sample: 29 mL
Inorganic Impurities Analysis: Add 1 drop of methyl red TS to 25 mL of
• LEAD, Lead Limit Test, Atomic Absorption Spectrophotometric water, add 0.02 N sulfuric acid until a red color just
Graphite Furnace Method, Method I, Appendix IIIB appears, then add the Sample, and mix and titrate with
Acceptance criteria: NMT 1 mg/kg 0.02 N sulfuric acid until the red color is restored.
 782 / Methyl Alcohol / Monographs FCC 9

Acceptance criteria: NMT 0.2 mL of 0.02 N sulfuric DESCRIPTION

acid is required to restore the red color (NMT 3 mg/kg) Methyl Anthranilate occurs as a colorless to pale yellow
• DISTILLATION RANGE, Appendix IIB liquid with blue fluorescence.
Acceptance criteria: Within a range of 1°, including Odor: Grape
64.6° ± 0.1° Solubility: Soluble in most fixed oils, propylene glycol;
• NONVOLATILE RESIDUE insoluble or practically insoluble in glycerin
Sample: 125 mL (about 100 g) Boiling Point: ∼256°
Analysis: Evaporate the Sample to dryness in a tared Solubility in Alcohol, Appendix VI: One mL dissolves in 5
dish on a steam bath, dry the residue at 105° for 30 mL of 60% alcohol, and remains in solution upon dilution
min, cool, and weigh. to 10 mL.
Monographs

Acceptance criteria: NMT 10 mg/kg Function: Flavoring agent

• READILY CARBONIZABLE SUBSTANCES, Appendix IIB
Sample solution: 25 mL of sample in 25 mL of 95% IDENTIFICATION
sulfuric acid. [NOTE—The sulfuric acid should be cooled • INFRARED SPECTRA, Spectrophotometric Identification Tests,
to 10°.] Appendix IIIC
Control solution: 3.5 mL of platinum-cobalt CS diluted Acceptance criteria: The spectrum of the sample
to 50 mL exhibits relative maxima at the same wavelengths as
Acceptance criteria: The Sample solution has no more those of the spectrum below.
color than the Control solution. (Equivalent to NMT 35
APHA color units)
ASSAY
• PROCEDURE: Proceed as directed under Esters, Appendix
• SOLUBILITY IN WATER
VI.
Analysis: Mix 15 mL of sample and 45 mL of water.
Sample: 1.0 g
Acceptance criteria: After 1 h, the resulting solution is
Analysis: Use 75.59 as the equivalence factor (e).
as clear as an equal volume of water.
Acceptance criteria: NLT 98.0% of total esters as
• SUBSTANCES REDUCING PERMANGANATE
C8H9NO2
Sample: 20 mL, previously cooled to 15°
Analysis: Transfer the Sample, to a glass-stoppered SPECIFIC TESTS
cylinder, add 0.1 mL of 0.1 N potassium • REFRACTIVE INDEX, Appendix II [NOTE—Determine as a
permanganate, mix, and allow to stand for 5 min. supercooled liquid.]
Acceptance criteria: The pink color is not entirely Acceptance criteria: Between 1.581 and 1.585
discharged. • SPECIFIC GRAVITY: Determine at 25° by any reliable
• WATER, Water Determination, Appendix IIB method (see General Provisions).
Acceptance criteria: NMT 0.1% Acceptance criteria: Between 1.161 and 1.169

Methyl Anthranilate
.

First Published: Prior to FCC 6

C8H9NO2 Formula wt 151.16

FEMA: 2682
UNII: 981I0C1E5W [methyl anthranilate]
 FCC 9 Monographs / Methyl Benzoate / 783

OTHER REQUIREMENTS
• SOLIDIFICATION POINT, Appendix IIB
Acceptance criteria: NLT 23.8°

Monographs
Methyl Anthranilate

IDENTIFICATION
Methyl Benzoate
.

• INFRARED SPECTRA, Spectrophotometric Identification Tests,

First Published: Prior to FCC 6 Appendix IIIC
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
XI.
C8H8O2 Formula wt 136.15 Acceptance criteria: NLT 98.0% of C8H8O2
FEMA: 2683
UNII: 6618K1VJ9T [methyl benzoate] SPECIFIC TESTS
• ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
DESCRIPTION OILS), M-15, Appendix XI
Methyl Benzoate occurs as a colorless liquid. Acceptance criteria: NMT 1.0
Odor: Deep, pungent, floral • REFRACTIVE INDEX, Appendix II: At 20°
Solubility: Soluble in alcohol, most fixed oils, propylene Acceptance criteria: Between 1.514 and 1.518
glycol; insoluble or practically insoluble in glycerin • SPECIFIC GRAVITY: Determine at 25° by any reliable
Boiling Point: ∼198° method (see General Provisions).
Solubility in Alcohol, Appendix VI: One mL dissolves in 4 Acceptance criteria: Between 1.082 and 1.088
mL of 60% alcohol.
Function: Flavoring agent
 784 / Methyl Benzoate / Monographs FCC 9

OTHER REQUIREMENTS
• CHLORINATED COMPOUNDS, Appendix VI
Acceptance criteria: Passes test
Monographs

Methyl Benzoate

Methyl Butyrate Methyl Cinnamate

. .

First Published: Prior to FCC 6 First Published: Prior to FCC 6

C5H10O2 Formula wt 102.13

FEMA: 2693 C10H10O2 Formula wt 162.19
UNII: CGX598508O [methyl butyrate] FEMA: 2698
UNII: 533CV2ZCQL [methyl cinnamate]
DESCRIPTION
Methyl Butyrate occurs as a colorless liquid. DESCRIPTION
Odor: Fruity Methyl Cinnamate occurs as a white to slightly yellow
Boiling Point: ∼102° crystalline mass.
Solubility in Alcohol, Appendix VI: One mL dissolves in 1 Odor: Fruity, balsamic
mL of 95% ethanol. Solubility: Soluble in alcohol, most fixed oils, glycerin,
Function: Flavoring agent propylene glycol; insoluble or practically insoluble in water
Boiling Point: ∼260°
ASSAY Solubility in Alcohol, Appendix VI: One g dissolves in 4
• PROCEDURE: Proceed as directed under M-1b, Appendix mL of 80% alcohol.
XI. Function: Flavoring agent
Acceptance criteria: NLT 98.0% of C5H10O2
IDENTIFICATION
SPECIFIC TESTS • INFRARED SPECTRA, Spectrophotometric Identification Tests,
• ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL Appendix IIIC
OILS), M-15, Appendix XI Acceptance criteria: The spectrum of the sample
Acceptance criteria: NMT 1.0 exhibits relative maxima at the same wavelengths as
• REFRACTIVE INDEX, Appendix II: At 20° those of the spectrum below.
Acceptance criteria: Between 1.386 and 1.390
• SPECIFIC GRAVITY: Determine at 25° by any reliable ASSAY
method (see General Provisions). • PROCEDURE: Proceed as directed under M-1b, Appendix
Acceptance criteria: Between 0.892 and 0.897 XI.
 FCC 9 Monographs / Methyl Cyclopentenolone / 785

Acceptance criteria: NLT 98.0% of C10H10O2 OTHER REQUIREMENTS

• CHLORINATED COMPOUNDS, Appendix VI
SPECIFIC TESTS Acceptance criteria: Passes test
• ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL • LEAD, M-9, Appendix XI
OILS), M-15, Appendix XI Acceptance criteria: NMT 10 mg/kg
Acceptance criteria: NMT 2.0

Monographs
Methyl Cinnamate

Solubility: Soluble in alcohol, propylene glycol; slightly

Methyl Cyclopentenolone
.

soluble in most fixed oils; 1 g dissolves in 72 mL water

First Published: Prior to FCC 6 Solubility in Alcohol, Appendix VI: One g dissolves in 5
mL of 90% alcohol.
Function: Flavoring agent
3-Methylcyclopentane-1,2-dione
IDENTIFICATION
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Appendix IIIC
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
C6H8O2 Formula wt 112.13
those of the spectrum below.
FEMA: 2700
UNII: 627E92X64B [methylcyclopentenolone] OTHER REQUIREMENTS
• MELTING RANGE OR TEMPERATURE DETERMINATION,
DESCRIPTION Appendix IIB
Methyl Cyclopentenolone occurs as a white, crystalline Acceptance criteria: Between 104° and 108°
powder.
Odor: Nutty, maple-licorice aroma in dilute solution
 786 / Methyl Cyclopentenolone / Monographs FCC 9
Monographs

Methyl Cyclopentenolone

Acceptance criteria: The spectrum of the sample

Methyl Ester of Rosin, Partially
.

exhibits relative maxima at the same wavelengths as

Hydrogenated those of the spectrum below.
First Published: Prior to FCC 6
IMPURITIES
Inorganic Impurities
• LEAD, Sample Solution for Lead Limit Test, Appendix IV
DESCRIPTION
Control: 5 µg Pb (5 mL of Diluted Standard Lead
Methyl Ester of Rosin, Partially Hydrogenated, occurs as a
Solution)
light amber-colored liquid resin. It is soluble in acetone but
Acceptance criteria: NMT 1 mg/kg
insoluble in water.
Function: Masticatory substance in chewing gum base SPECIFIC TESTS
Packaging and Storage: Store in well-closed containers. • ACID NUMBER, Appendix IX
Acceptance criteria: Between 4 and 8
IDENTIFICATION
• REFRACTIVE INDEX, Appendix IIB
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
[NOTE—Use an Abbé or other refractometer of equal or
Appendix IIIC
greater accuracy.]
Sample preparation: Neat dispersion of sample on a
Acceptance criteria: Between 1.517 and 1.520 at 20°
potassium bromide plate
 FCC 9 Monographs / Methyl Ethyl Cellulose / 787

• VISCOSITY (ROSINS AND RELATED SUBSTANCES), Appendix IX

Acceptance criteria: Between 23 and 76 poises

Monographs
Methyl Ester of Rosin, Partially Hydrogenated

Analysis: Whip the Sample with a kitchen-type mixer (as

Methyl Ethyl Cellulose
.

if whipping egg whites).

First Published: Prior to FCC 6 Acceptance criteria: A stable air/liquid foam is
produced.
Modified Cellulose ASSAY
INS: 465 CAS: [9004-69-7] • ASSAY FOR ETHOXYL GROUPS, Hydroxypropoxyl
DESCRIPTION Determination, Appendix IIIC
Methyl Ethyl Cellulose occurs as a white or pale cream, Analysis: Each mL of 0.02 N sodium hydroxide is
fibrous solid or powder. It is the methyl ether of ethyl equivalent to 0.9 mg of ethoxyl groups (-OC2H5)
cellulose in which both the methyl and the ethyl groups Acceptance criteria: NLT 14.5% and NMT 19.0% of
are attached to the anhydroglucose units by ether linkages. ethoxyl groups (-OC2H5).
It disperses in cold water to form aqueous sols that • ASSAY FOR METHOXYL GROUPS, Methoxyl Determination,
undergo a reversible transformation to gel upon heating Appendix IIIC
and cooling, respectively. Sample: 50 mg, previously dried, placed in a tared
Function: Emulsifier; stabilizer; foaming agent gelatin capsule
Packaging and Storage: Store in well-closed containers. Analysis: Determine as directed, but calculate the total
alkoxyl content as ethoxyl groups (-OC2H5). Each mL of
IDENTIFICATION 0.1 N sodium thiosulfate is equivalent to 0.7510 mg of
• A. PROCEDURE ethoxyl groups (-OC2H5). Calculate the methoxyl
Sample: 1 g groups (-OCH3) by the formula:
Analysis: Add the Sample to 100 mL of water. [NOTE—
Save this solution for use in Identification tests B and C.] Result = (A − B) × 31/45
Acceptance criteria: The sample disperses to form an
opalescent, fibrous solution. A = total alkoxyl content, calculated as -OC2H5
• B. PROCEDURE B = -OC2H5 determined in the Assay for Ethoxyl
Sample: A few mL of the solution prepared in Groups (above)
Identification test A (above) 31 = molecular weight of -OCH3
Analysis: Heat the Sample to about 60°. 45 = molecular weight of -OC2H5
Acceptance criteria: The solution becomes cloudy, and Acceptance criteria: NLT 3.5% and NMT 6.5% of
a gelatinous precipitate forms that redissolves upon methoxyl groups (-OCH3)
cooling.
• C. PROCEDURE IMPURITIES
Sample: The remaining solution from Identification test A Inorganic Impurities
(above) • LEAD, Lead Limit Test, Appendix IIIB
 788 / Methyl Ethyl Cellulose / Monographs FCC 9

Sample: Prepare as directed for organic compounds C11H14O2 Formula wt 178.23

using 2 g of sample. FEMA: 2475
Control: 6 µg Pb (6 mL of Diluted Standard Lead UNII: 29T9VA6R7M [methyl eugenol]
Solution)
Acceptance criteria: NMT 3 mg/kg DESCRIPTION
Methyl Eugenol occurs as a colorless to pale yellow liquid.
SPECIFIC TESTS Odor: Delicate, clove-carnation
• LOSS ON DRYING, Appendix IIC: 105° for 4 h Solubility: Soluble in most fixed oils; insoluble or
Sample: 3 g practically insoluble in glycerin, propylene glycol
Acceptance criteria Boiling Point: ∼249°
Monographs

Fibrous form: NMT 15.0% Solubility in Alcohol, Appendix VI: One mL dissolves in 2
Powdered form: NMT 10.0% mL of 70% alcohol, and remains in solution on dilution to
• RESIDUE ON IGNITION (SULFATED ASH), Appendix IIC 10 mL.
Sample: 1 g Function: Flavoring agent
Acceptance criteria: NMT 0.6%
• VISCOSITY DETERMINATION, Viscosity of Methylcellulose, IDENTIFICATION
Appendix IIB • INFRARED SPECTRA, Spectrophotometric Identification Tests,
Sample solution: Transfer an amount of sample Appendix IIIC
equivalent to 5.0 g on the dried basis into a 250-mL Acceptance criteria: The spectrum of the sample
beaker. Adjust the rotor of a variable-speed stirrer about exhibits relative maxima at the same wavelengths as
1 in above the sample, add 195 mL of recently boiled those of the spectrum below.
and cooled water, and stir at a speed that will avoid
undue aeration. Continue stirring for about 1.5 h, then ASSAY
either set aside for 3 h to overnight, or centrifuge to • PROCEDURE: Proceed as directed under M-1b, Appendix
expel any entrapped air. Adjust the temperature to 20° XI.
± 0.1°. Acceptance criteria: NLT 98.0% of C11H14O2 (one major
Analysis: Determine as directed using a Viscometer for isomer)
High Viscosity. SPECIFIC TESTS
Acceptance criteria: NLT 80% and NMT 120% of that • REFRACTIVE INDEX, Appendix II: At 20°
stated on the label or otherwise represented by the Acceptance criteria: Between 1.532 and 1.536
vendor. [NOTE—The usual range of viscosity types is • SPECIFIC GRAVITY: Determine at 25° by any reliable
between 20 and 60 cP.] method (see General Provisions).
Acceptance criteria: Between 1.032 and 1.036

Methyl Eugenol
.

First Published: Prior to FCC 6

Eugenyl Methyl Ether

1,2-Dimethoxy-4-allylbenzene
 FCC 9 Monographs / Methyl Furoate / 789

OTHER REQUIREMENTS
• EUGENOL, M-1b, Appendix XI
Acceptance criteria: NMT 1.0%

Monographs
Methyl Eugenol

IDENTIFICATION
Methyl Furoate
.

• INFRARED SPECTRA, Spectrophotometric Identification Tests,

First Published: Prior to FCC 6 Appendix IIIC
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
C6H6O3 Formula wt 126.11 XI.
FEMA: 2703 Acceptance criteria: NLT 98.0% of C6H6O3
UNII: O9A8D29YDE [methyl 2-furoate]
SPECIFIC TESTS
DESCRIPTION • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
Methyl Furoate occurs as a pale yellow to brown liquid. OILS), M-15, Appendix XI
Odor: Fruity Acceptance criteria: NMT 5.0
Solubility: Soluble in propylene glycol, vegetable oils; • REFRACTIVE INDEX, Appendix II: At 20°
insoluble or practically insoluble in water Acceptance criteria: Between 1.483 and 1.500
Boiling Point: ∼181° • SPECIFIC GRAVITY: Determine at 25° by any reliable
Solubility in Alcohol, Appendix VI: One mL dissolves in 1 method (see General Provisions).
mL of 95% ethanol. Acceptance criteria: Between 1.174 and 1.180
Function: Flavoring agent
 790 / Methyl Furoate / Monographs FCC 9
Monographs

Methyl Furoate

IDENTIFICATION
Methyl Hexanoate
.

• INFRARED SPECTRA, Spectrophotometric Identification Tests,

First Published: Prior to FCC 6 Appendix IIIC
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
C7H14O2 Formula wt 130.19 XI.
FEMA: 2708 Acceptance criteria: NLT 98.0% of C7H14O2
UNII: 246364VPJS [methyl caproate]
SPECIFIC TESTS
DESCRIPTION • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
Methyl Hexanoate occurs as a colorless to pale yellow liquid. OILS), M-15, Appendix XI
Odor: Fruity Acceptance criteria: NMT 2.0
Solubility: Soluble in propylene glycol, vegetable oils; • REFRACTIVE INDEX, Appendix II: At 20°
insoluble or practically insoluble in water Acceptance criteria: Between 1.402 and 1.408
Boiling Point: ∼151° • SPECIFIC GRAVITY: Determine at 25° by any reliable
Solubility in Alcohol, Appendix VI: One mL dissolves in 1 method (see General Provisions).
mL of 95% ethanol. Acceptance criteria: Between 0.880 and 0.886
Function: Flavoring agent
 FCC 9 Monographs / Methyl Hexyl Ketone / 791

Monographs
Methyl Hexanoate

Function: Flavoring agent

Methyl Hexyl Ketone
.

IDENTIFICATION
First Published: Prior to FCC 6
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Appendix IIIC
2-Octanone Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
C8H16O Formula wt 128.21 • PROCEDURE: Proceed as directed under M-1a, Appendix
FEMA: 2802 XI.
UNII: J2G84H29AF [2-octanone] Acceptance criteria: NLT 95.0% of C8H16O

DESCRIPTION SPECIFIC TESTS

Methyl Hexyl Ketone occurs as a colorless to pale yellow • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
liquid. OILS), M-15, Appendix XI
Odor: Apple Acceptance criteria: NMT 1.0
Solubility: Soluble in propylene glycol, vegetable oils; • REFRACTIVE INDEX, Appendix II: At 20°
insoluble or practically insoluble in water Acceptance criteria: Between 1.414 and 1.418
Boiling Point: ∼175° • SPECIFIC GRAVITY: Determine at 25° by any reliable
Solubility in Alcohol, Appendix VI: One mL dissolves in 1 method (see General Provisions).
mL of 95% alcohol. Acceptance criteria: Between 0.813 and 0.818
 792 / Methyl Hexyl Ketone / Monographs FCC 9
Monographs

Methyl Hexyl Ketone

Methyl Ionones Methyl Isobutyrate

. .

First Published: Prior to FCC 6 First Published: Prior to FCC 6

Mixture of α-, β-, γ- or α-iso, and δ-isomers

C5H10O2 Formula wt 102.13

C14H22O Formula wt 206.3 FEMA: 2694
UNII: EL78BGX1LO [methyl ionones] UNII: EM286QL922 [methyl isobutyrate]

DESCRIPTION DESCRIPTION
Methyl Ionones occur as clear to pale yellow to yellow Methyl Isobutyrate occurs as a colorless liquid.
liquids. Odor: Fruity
Odor: Woody, orris Boiling Point: ∼90°
Boiling Point: ∼232° to 270° Solubility in Alcohol, Appendix VI: One mL dissolves in 1
Solubility in Alcohol, Appendix VI: One mL dissolves in 1 mL of 95% alcohol.
mL of 95% ethanol. Function: Flavoring agent
Function: Flavoring agent
IDENTIFICATION
ASSAY • INFRARED SPECTRA, Spectrophotometric Identification Tests,
• PROCEDURE: Proceed as directed under M-1b, Appendix Appendix IIIC
XI. Acceptance criteria: The spectrum of the sample
Acceptance criteria: NLT 88.0% of C14H22O (sum of exhibits relative maxima at the same wavelengths as
four isomers) those of the spectrum below.

SPECIFIC TESTS ASSAY

• ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL • PROCEDURE: Proceed as directed under M-1b, Appendix
OILS), M-15, Appendix XI XI.
Acceptance criteria: NMT 5.0 Acceptance criteria: NLT 97.0% of C5H10O2
• REFRACTIVE INDEX, Appendix II: At 20°
Acceptance criteria: Between 1.497 and 1.507
SPECIFIC TESTS
• ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
• SPECIFIC GRAVITY: Determine at 25° by any reliable
OILS), M-15, Appendix XI
method (see General Provisions).
Acceptance criteria: NMT 1.0
Acceptance criteria: Between 0.925 and 0.934
 FCC 9 Monographs / Methyl Isoeugenol / 793

• REFRACTIVE INDEX, Appendix II: At 20° • SPECIFIC GRAVITY: Determine at 25° by any reliable
Acceptance criteria: Between 1.382 and 1.386 method (see General Provisions).
Acceptance criteria: Between 0.884 and 0.888

Monographs
Methyl Isobutyrate

Function: Flavoring agent

Methyl Isoeugenol
.

IDENTIFICATION
First Published: Prior to FCC 6
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Appendix IIIC
4-Allyl-1,2-dimethoxy Benzene Acceptance criteria: The spectrum of the sample
Isoeugenyl Methyl Ether exhibits relative maxima at the same wavelengths as
4-Propenyl Veratrole those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1a, Appendix
XI.
Acceptance criteria: NLT 85.0% of C11H14O2 (one
C11H14O2 Formula wt 178.23
isomer)
FEMA: 2476
UNII: 46RN7Q97DE [methyl isoeugenol] SPECIFIC TESTS
• REFRACTIVE INDEX, Appendix II: At 20°
DESCRIPTION Acceptance criteria: Between 1.566 and 1.569
Methyl Isoeugenol occurs as a colorless to pale yellow • SPECIFIC GRAVITY: Determine at 25° by any reliable
liquid. method (see General Provisions).
Odor: Delicate, clove-carnation Acceptance criteria: Between 1.047 and 1.053
Solubility: Soluble in most fixed oils; insoluble or
practically insoluble in glycerin, propylene glycol
Boiling Point: ∼270°
Solubility in Alcohol, Appendix VI: One mL dissolves in 2
mL of 70% alcohol, and remains in solution upon dilution
to 10 mL.
 794 / Methyl Isoeugenol / Monographs FCC 9

OTHER REQUIREMENTS
• ISOEUGENOL, M-1b, Appendix XI
Acceptance criteria: NMT 1.0%
Monographs

Methyl Isoeugenol

IDENTIFICATION
Methyl Isovalerate
.

• INFRARED SPECTRA, Spectrophotometric Identification Tests,

First Published: Prior to FCC 6 Appendix IIIC
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
C6H1202 Formula wt 116.16 XI.
FEMA: 2753 Acceptance criteria: NLT 95.0% of C10H12O2
UNII: QPS4788198 [methyl isovalerate]
SPECIFIC TESTS
DESCRIPTION • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
Methyl Isovalerate occurs as a colorless to pale yellow liquid. OILS), M-15, Appendix XI
Odor: Apple Acceptance criteria: NMT 1.0
Solubility: Soluble in propylene glycol, vegetable oils; • REFRACTIVE INDEX, Appendix II: At 20°
insoluble or practically insoluble in water Acceptance criteria: Between 1.390 and 1.396
Boiling Point: ∼114° • SPECIFIC GRAVITY: Determine at 25° by any reliable
Solubility in Alcohol, Appendix VI: One mL dissolves in 1 method (see General Provisions).
mL of 95% ethanol. Acceptance criteria: Between 0.878 and 0.884
Function: Flavoring agent
 FCC 9 Monographs / Methyl Phenylacetate / 795

Monographs
Methyl Isovalerate

IDENTIFICATION
Methyl Phenylacetate
.

• INFRARED SPECTRA, Spectrophotometric Identification Tests,

First Published: Prior to FCC 6 Appendix IIIC
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
C9H10O2 Formula wt 150.18 XI.
FEMA: 2733 Acceptance criteria: NLT 98.0% of C9H10O2
UNII: D4PDC41X96 [methyl phenylacetate]
SPECIFIC TESTS
DESCRIPTION • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
Methyl Phenylacetate occurs as a colorless or nearly colorless OILS), M-15, Appendix XI
liquid. Acceptance criteria: NMT 1.0
Odor: Honey, jasmine • REFRACTIVE INDEX, Appendix II: At 20°
Solubility: Soluble in alcohol, most fixed oils; insoluble or Acceptance criteria: Between 1.503 and 1.509
practically insoluble in glycerin, propylene glycol, water • SPECIFIC GRAVITY: Determine at 25° by any reliable
Boiling Point: ∼215° method (see General Provisions).
Solubility in Alcohol, Appendix VI: One mL dissolves in 6 Acceptance criteria: Between 1.061 and 1.067
mL of 60% alcohol.
Function: Flavoring agent
 796 / Methyl Phenylacetate / Monographs FCC 9

OTHER REQUIREMENTS
• CHLORINATED COMPOUNDS, Appendix VI
Acceptance criteria: Passes test
Monographs

Methyl Phenylacetate

Function: Flavoring agent

Methyl Phenylcarbinyl Acetate
.

IDENTIFICATION
First Published: Prior to FCC 6
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Appendix IIIC
α-Phenyl Ethyl Acetate Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
C10H12O2 Formula wt 164.20 XI.
FEMA: 2684 Acceptance criteria: NLT 97.0% of C10H12O2
UNII: FYS3E9NBA3 [α-methylbenzyl acetate]
SPECIFIC TESTS
DESCRIPTION • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
Methyl Phenylcarbinyl Acetate occurs as a colorless liquid. OILS), M-15, Appendix XI
Odor: Gardenia Acceptance criteria: NMT 2.0
Solubility: Soluble in most fixed oils, glycerin; insoluble or • REFRACTIVE INDEX, Appendix II: At 20°
practically insoluble in water Acceptance criteria: Between 1.493 and 1.497
Boiling Point: ∼214° • SPECIFIC GRAVITY: Determine at 25° by any reliable
Solubility in Alcohol, Appendix VI: One mL dissolves in 7 method (see General Provisions).
mL of 60% alcohol. Acceptance criteria: Between 1.023 and 1.026
 FCC 9 Monographs / Methyl Salicylate / 797

OTHER REQUIREMENTS
• CHLORINATED COMPOUNDS, Appendix VI
Acceptance criteria: Passes test

Monographs
Methyl Phenylcarbinyl Acetate

Reference standard: USP Methyl Salicylate RS

Methyl Salicylate
.

Sample and standard preparation: F

First Published: Prior to FCC 6 Acceptance criteria: The spectrum of the sample
Last Revision: First Supplement, FCC 8 exhibits maxima at the same wavelengths as those in
the spectrum of the Reference standard.

ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
XI.
Reference standard: USP Methyl Salicylate RS
Acceptance criteria: NLT 98.0% of methyl salicylate
C8H8O3 Formula wt 152.15
FEMA: 2745 SPECIFIC TESTS
UNII: LAV5U5022Y [methyl salicylate] • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
OILS), M-15, Appendix XI
DESCRIPTION [NOTE—Use phenol red TS as the indicator.]
Methyl Salicylate occurs as a colorless to yellow liquid. Acceptance criteria: NMT 1.0
Odor: Wintergreen • REFRACTIVE INDEX, Appendix II: At 20°
Solubility: Soluble in alcohol, glacial acetic acid; slightly Acceptance criteria: 1.535–1.538
soluble in water • SPECIFIC GRAVITY: Determine at 25° by any reliable
Boiling Point: ∼222° (decomp) method (see General Provisions).
Solubility in Alcohol, Appendix VI: One mL dissolves in 7 Acceptance criteria: 1.180–1.185
mL of 70% alcohol, and may be slightly cloudy.
Function: Flavoring agent

IDENTIFICATION
• INFRARED ABSORPTION, Spectrophotometric Identification
Tests, Appendix IIIC
 798 / Methyl Thiobutyrate / Monographs FCC 9

IDENTIFICATION
Methyl Thiobutyrate
.

• INFRARED SPECTRA, Spectrophotometric Identification Tests,

First Published: Prior to FCC 6 Appendix IIIC
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
C5H10OS Formula wt 118.20 XI.
Monographs

FEMA: 3310 Acceptance criteria: NLT 97.0% of C5H10OS

UNII: 2P1E432MYZ [methyl thiobutyrate]
SPECIFIC TESTS
DESCRIPTION • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
Methyl Thiobutyrate occurs as a colorless to pale yellow OILS), M-15, Appendix XI
liquid. Acceptance criteria: NMT 3.0
Odor: Pungent • REFRACTIVE INDEX, Appendix II: At 20°
Solubility: Soluble in propylene glycol, vegetable oils; Acceptance criteria: Between 1.461 and 1.467
insoluble or practically insoluble in water • SPECIFIC GRAVITY: Determine at 25° by any reliable
Boiling Point: ∼143° method (see General Provisions).
Solubility in Alcohol, Appendix VI: One mL dissolves in 1 Acceptance criteria: Between 0.964 and 0.970
mL of 95% ethanol.
Function: Flavoring agent

Methyl Thiobutyrate
 FCC 9 Monographs / Methyl-3-methylthiopropionate / 799

IDENTIFICATION
Methyl Valerate
.

• INFRARED SPECTRA, Spectrophotometric Identification Tests,

First Published: Prior to FCC 6 Appendix IIIC
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
C6H12O2 Formula wt 116.16 XI.

Monographs
FEMA: 2752 Acceptance criteria: NLT 98.0% of C6H12O2
UNII: ZW21JJJ9VN [methyl valerate]
SPECIFIC TESTS
DESCRIPTION • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
Methyl Valerate occurs as a colorless to pale yellow liquid. OILS), M-15, Appendix XI
Odor: Fruity Acceptance criteria: NMT 1.0
Solubility: Soluble in propylene glycol, vegetable oils; • REFRACTIVE INDEX, Appendix II: At 20°
insoluble or practically insoluble in water Acceptance criteria: Between 1.395 and 1.401
Boiling Point: ∼128° • SPECIFIC GRAVITY: Determine at 25° by any reliable
Solubility in Alcohol, Appendix VI: One mL dissolves in 1 method (see General Provisions).
mL of 95% ethanol. Acceptance criteria: Between 0.885 and 0.891
Function: Flavoring agent

Methyl Valerate

UNII: 28913SS9T9 [methyl 3-methylthiopropionate]

Methyl-3-methylthiopropionate
.

First Published: Prior to FCC 6

DESCRIPTION
Methyl-3-methylthiopropionate occurs as a colorless to pale
yellow liquid.
Odor: Onion
Solubility: Soluble in propylene glycol, vegetable oils;
insoluble or practically insoluble in water
Boiling Point: ∼74° to 75° (18 mm Hg)
C5H10O2S Formula wt 134.19 Solubility in Alcohol, Appendix VI: One mL dissolves in 1
FEMA: 2720 mL of 95% ethanol.
 800 / Methyl-3-methylthiopropionate / Monographs FCC 9

Function: Flavoring agent Acceptance criteria: NLT 97.0% of C5H10O2S

IDENTIFICATION SPECIFIC TESTS

• INFRARED SPECTRA, Spectrophotometric Identification Tests, • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
Appendix IIIC OILS), M-15, Appendix XI
Acceptance criteria: The spectrum of the sample Acceptance criteria: NMT 1.0
exhibits relative maxima at the same wavelengths as • REFRACTIVE INDEX, Appendix II: At 20°
those of the spectrum below. Acceptance criteria: Between 1.462 and 1.468
• SPECIFIC GRAVITY: Determine at 25° by any reliable
ASSAY method (see General Provisions).
• PROCEDURE: Proceed as directed under M-1a, Appendix
Monographs

Acceptance criteria: Between 1.069 and 1.078

XI.

Methyl-3-methylthiopropionate

Odor: Sweet, nutty

Methylbenzyl Acetate
.

Solubility: Soluble in most fixed oils; slightly soluble in

First Published: Prior to FCC 6 propylene glycol; insoluble or practically insoluble in
Last Revision: First Supplement, FCC 8 glycerin
Solubility in Alcohol, Appendix VI: One mL dissolves in 2
mL of 70% alcohol, and remains clear on dilution.
Mixed isomers of ortho-, meta-, and para-methylbenzyl
Function: Flavoring agent
acetate
IDENTIFICATION
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Appendix IIIC
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
C10H12O2 Formula wt 164.20 those of the spectrum below.
FEMA: 3702
UNII: 606K99GR0L [o-cresol acetate] ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
DESCRIPTION XI.
Methylbenzyl Acetate occurs as a colorless liquid. Acceptance criteria: NLT 98.0% of C10H12O2
 FCC 9 Monographs / α-Methylbenzyl Alcohol / 801

SPECIFIC TESTS Acceptance criteria: 1.030–1.035

• ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
OILS), M-15, Appendix XI OTHER REQUIREMENTS
Acceptance criteria: NMT 1.0 • CHLORINATED COMPOUNDS, Appendix VI
• REFRACTIVE INDEX, Appendix II: At 20° Acceptance criteria: Passes test
Acceptance criteria: 1.501–1.504
• SPECIFIC GRAVITY: Determine at 25° by any reliable
method (see General Provisions).

Monographs
Methylbenzyl Acetate

IDENTIFICATION
α-Methylbenzyl Alcohol
.

• INFRARED SPECTRA, Spectrophotometric Identification Tests,

First Published: Prior to FCC 6 Appendix IIIC
Acceptance criteria: The spectrum of the sample
Methyl Phenylcarbinol exhibits relative maxima at the same wavelengths as
α-Phenethyl Alcohol those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
XI.
Acceptance criteria: NLT 99.0% of C8H10O

C8H10O Formula wt 122.17 SPECIFIC TESTS

FEMA: 2685 • REFRACTIVE INDEX, Appendix II: At 20°
UNII: E6O895DQ52 [1-phenylethanol, (+/-)-] Acceptance criteria: Between 1.525 and 1.529
• SPECIFIC GRAVITY: Determine at 25° by any reliable
DESCRIPTION method (see General Provisions).
α-Methylbenzyl alcohol occurs as a colorless liquid above Acceptance criteria: Between 1.009 and 1.014
room temperature.
Odor: Mild, hyacinth OTHER REQUIREMENTS
Solubility: Very soluble in glycerin; soluble in most fixed • KETONES, M-2d, Appendix XI
oils, propylene glycol Sample: 10.0 g
Boiling Point: ∼204° Analysis: Use 60.07 as the equivalence factor (e).
Solubility in Alcohol, Appendix VI: One mL dissolves in 3 Acceptance criteria: NMT 1.0% as acetophenone
mL of 50% alcohol.
Function: Flavoring agent
 802 / α-Methylbenzyl Alcohol / Monographs FCC 9

• SOLIDIFICATION POINT, Appendix IIB

Acceptance criteria: NLT 19°
Monographs

α-Methylbenzyl Alcohol

Function: Flavoring agent

2-Methylbutyric Acid
.

IDENTIFICATION
First Published: Prior to FCC 6
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Appendix IIIC
Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
C5H10O2 Formula wt 102.13 • PROCEDURE: Proceed as directed under M-3a, Appendix
FEMA: 2695 XI.
UNII: PX7ZNN5GXK [2-methylbutyric acid] Acceptance criteria: NLT 98.0% of C5H10O2

DESCRIPTION SPECIFIC TESTS

2-Methylbutyric Acid occurs as a colorless to pale yellow • REFRACTIVE INDEX, Appendix II: At 20°
liquid. Acceptance criteria: Between 1.404 and 1.408
Odor: Fruity • SPECIFIC GRAVITY: Determine at 25° by any reliable
Solubility: Soluble in propylene glycol, vegetable oils; method (see General Provisions).
insoluble or practically insoluble in water Acceptance criteria: Between 0.932 and 0.936
Boiling Point: ∼176°
Solubility in Alcohol, Appendix VI: One mL dissolves in 1
mL of 95% alcohol.
 FCC 9 Monographs / 2-Methylbutyl Isovalerate / 803

Monographs
2-Methylbutyric Acid

Acceptance criteria: Between 0.872 and 0.877

2-Methylbutyl Acetate
.

First Published: Prior to FCC 6

2-Methylbutyl Isovalerate
.

First Published: Prior to FCC 6

2-Methylbutyl-3-methylbutanoate

C7H14O2 Formula wt 130.18

FEMA: 3644
UNII: IY8732E0YC [2-methylbutyl acetate]

DESCRIPTION C10H20O2 Formula wt 172.27

2-Methylbutyl Acetate occurs as a colorless to pale yellow FEMA: 3506
liquid. UNII: 7G5TZ5034W [2-methylbutyl isovalerate]
Odor: Banana
Boiling Point: ∼138° DESCRIPTION
Function: Flavoring agent 2-Methylbutyl Isovalerate occurs as a colorless liquid.
Odor: Herbaceous, fruity
ASSAY Solubility: Soluble in alcohol, most fixed oils; insoluble or
• PROCEDURE: Proceed as directed under M-1b, Appendix
practically insoluble in water
XI.
Boiling Point: ∼191° to 195°
Acceptance criteria: NLT 97.0% of C7H14O2
Function: Flavoring agent
SPECIFIC TESTS ASSAY
• ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
• PROCEDURE: Proceed as directed under M-1a, Appendix
OILS), M-15, Appendix XI
XI.
Acceptance criteria: NMT 1.0
Acceptance criteria: NLT 98.0% of C10H20O2
• REFRACTIVE INDEX, Appendix II: At 20°
Acceptance criteria: Between 1.399 and 1.404
• SPECIFIC GRAVITY: Determine at 25° by any reliable
method (see General Provisions).
 804 / 2-Methylbutyl Isovalerate / Monographs FCC 9

SPECIFIC TESTS ASSAY

• ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL • PROCEDURE
OILS), M-15, Appendix XI [CAUTION—Perform all steps involving hydriodic acid
Acceptance criteria: NMT 2.0 carefully in a well-ventilated hood. Use goggles, acid-
• REFRACTIVE INDEX, Appendix II: At 20° resistant gloves, and other appropriate safety
Acceptance criteria: Between 1.413 and 1.416 equipment. Be extremely careful when handling the hot
• SPECIFIC GRAVITY: Determine at 25° by any reliable vials because they are under pressure. In the event of
method (see General Provisions). hydriodic acid exposure, wash with copious amounts of
Acceptance criteria: Between 0.852 and 0.857 water and seek medical attention at once.]
Internal standard solution: 25 mg/mL toluene in o-
Monographs

xylene
Standard solution: Transfer 135 mg of adipic acid into
Methylcellulose
.

a suitable serum vial, add 4.0 mL of hydriodic acid

followed by 4.0 mL of the Internal standard solution,
First Published: Prior to FCC 6
and close the vial securely with a septum stopper.
Weigh the vial and its contents, add 90 µL of methyl
Modified Cellulose iodide with a syringe through the septum, reweigh, and
MC calculate the weight of methyl iodide added. Shake
well, and allow the layers to separate.
Sample solution: Transfer 65 mg of sample into a 5-mL
vial equipped with a pressure-tight septum closure, add
an amount of adipic acid equal to the weight of the
sample, and pipet 2 mL of the Internal standard solution
into the vial. Cautiously pipet 2 mL of hydriodic acid
INS: 461 CAS: [9004-67-5] into the mixture, immediately secure the closure, and
accurately weigh. Shake the vial for 30 s, heat at 150°
DESCRIPTION for 20 min, remove from the heat, shake again, using
Methylcellulose occurs as a white, fibrous powder or extreme caution, and heat at 150° for 40 min. Allow
granules. It is the methyl ether of cellulose. It is soluble in the vial to cool for about 45 min, and weigh. If the
water and in a limited number of organic solvent systems. weight loss is greater than 10 mg, discard the mixture
Aqueous solutions of Methylcellulose are surface active, and prepare another Sample solution.
form films upon drying, and undergo a reversible Chromatographic system, Appendix IIA
transformation from sol to gel upon heating and cooling, Mode: Gas chromatography
respectively. Detector: Thermal conductivity detector
Function: Thickener; stabilizer; emulsifier; bodying agent; Column: 1.8-m × 4-mm (id) glass column, or
bulking agent; binder; film former equivalent, packed with 10% methylsilicone oil (UCW
Packaging and Storage: Store in well-closed containers. 982 or equivalent) on 100- to 120-mesh flux-calcined
chromatographic siliceous earth (Chromosorb WHP, or
IDENTIFICATION equivalent)
• A. PROCEDURE Temperature
Sample: 1 g Column: 100°
Analysis: Add the Sample to 100 mL of water. [NOTE— Injector port: 200°
Save this solution for use in Identification tests B and C.] Detector: 200°
Acceptance criteria: The sample swells and disperses to Carrier gas: Helium
form a clear to opalescent, mucilaginous solution, Flow rate: 20 mL/min
depending upon the intrinsic viscosity, which is stable Injection size: About 2 µL
in the presence of most electrolytes and alcohol in Calibration: Inject an aliquot from the upper layer of
concentrations up to 40%. the Standard solution into the chromatograph, and
• B. PROCEDURE record the chromatogram. [NOTE—The retention times
Sample: A few mL of the solution prepared in for methyl iodide, toluene, and o-xylene are
Identification test A (above) approximately 3, 7, and 13 min, respectively.]
Analysis: Heat the Sample. Calculate the relative response factor, F, of equal weights
Acceptance criteria: The solution becomes cloudy, and of toluene and methyl iodide by the formula:
a flaky precipitate forms that redissolves as the solution
cools. Result = Q/A
• C. PROCEDURE
Sample: A few mL of the solution prepared in
Identification test A (above) Q = quantity ratio of methyl iodide to toluene in
Analysis: Pour the Sample onto a glass plate, and allow the Standard solution
the water to evaporate.
Acceptance criteria: A thin, self-sustaining film results.
FCC 9 Monographs / α-Methylcinnamaldehyde / 805

A = peak area ratio of methyl iodide to toluene

α-Methylcinnamaldehyde
.

obtained from the chromatogram of the

Standard solution First Published: Prior to FCC 6
Analysis: Inject an aliquot from the upper layer of the Last Revision: First Supplement, FCC 6
Sample solution into the chromatograph, and record the
chromatogram.
Calculate the percentage of methoxyl groups (–OCH3) in
the sample by the formula:

Result = a × (W/w) × (Mr1/Mr2) × F × 2

Monographs
C10H10O Formula wt 146.19
a = ratio of the area of the methyl iodide peak FEMA: 2697
to that of the toluene peak in the UNII: 1C647N9853 [α-methylcinnamaldehyde]
chromatogram of the Sample solution
W = weight of toluene in the Internal standard DESCRIPTION
solution (g) α-Methylcinnamaldehyde occurs as a yellow liquid. It may
w = weight of the sample taken (g) contain a suitable antioxidant.
Mr1 = molecular weight of methoxyl group, 31 Odor: Cinnamon
Mr2 = molecular weight of methyl iodide, 142 Solubility: Soluble in most fixed oils, propylene glycol;
F = relative response factor of toluene and insoluble or practically insoluble in glycerin
methyl iodide (determined above) Boiling Point: ∼148° (27 mm Hg)
Acceptance criteria: NLT 27.5% and NMT 31.5% of Solubility in Alcohol, Appendix VI: One mL dissolves in 3
methoxyl groups (–OCH3), calculated on the dried basis mL of 70% alcohol, and remains clear on dilution.
Function: Flavoring agent
IMPURITIES
Inorganic Impurities IDENTIFICATION
• LEAD, Lead Limit Test, Appendix IIIB • INFRARED SPECTRA, Spectrophotometric Identification Tests,
Sample solution: Prepare as directed for organic Appendix IIIC
compounds using 2 g of sample. Acceptance criteria: The spectrum of the sample
Control: 6 µg Pb (6 mL of Diluted Standard Lead exhibits relative maxima at the same wavelengths as
Solution) those of the spectrum below.
Acceptance criteria: NMT 3 mg/kg
ASSAY
SPECIFIC TESTS • PROCEDURE: Proceed as directed under M-1b, Appendix XI
• LOSS ON DRYING, Appendix IIC: 105° for 2 h Acceptance criteria: NLT 97.0% of C10H10O (one major
Sample: 3 g isomer)
Acceptance criteria: NMT 5.0%
• RESIDUE ON IGNITION (SULFATED ASH), Appendix IIC SPECIFIC TESTS
Sample: 1 g • ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
Acceptance criteria: NMT 1.5% OILS), M-15, Appendix XI
• VISCOSITY DETERMINATION, Viscosity of Methylcellulose, Acceptance criteria: NMT 5.0
Appendix IIB • REFRACTIVE INDEX, Appendix II: At 20°
Sample solution: Transfer an amount of sample Acceptance criteria: Between 1.602 and 1.607
equivalent to 2 g of solids on the dried basis to a wide- • SPECIFIC GRAVITY: Determine at 25° by any reliable
mouth 250-mL centrifuge bottle and add 98 g of water, method (see General Provisions).
previously heated to between 80° and 90°. Stir with a Acceptance criteria: Between 1.035 and 1.039
mechanical stirrer for 10 min, then place the bottle in
an ice bath until dissolution is complete, adjust the
weight of the solution with water to 100 g if necessary,
and centrifuge it to expel any entrapped air. Adjust the
temperature of the Sample solution to 20° ± 0.1°.
Acceptance criteria
Viscosity types of 100 cP or less: NLT 80% and NMT
120% of that stated on the label
Viscosity types of higher than 100 cP: NLT 75% and
NMT 140% of that stated on the label
 806 / α-Methylcinnamaldehyde / Monographs FCC 9
Monographs

α-Methylcinnamaldehyde

Concentration
Methylene Chloride
.

Analyte (% w/w)
methyl chloride 0.014
First Published: Prior to FCC 6
vinyl chloride 0.007

Dichloromethane ethyl chloride 0.0084

Methylene Dichloride propylene oxide 2.4

CH2Cl2 Formula wt 84.93 vinylidene chloride 0.0098

CAS: [75-09-2] trans-1,2-dichloroethylene 0.017
UNII: 588X2YUY0A [methylene chloride] chloroform 0.012
cyclohexane 0.047
DESCRIPTION
Methylene Chloride occurs as a clear, colorless, 2-methyl-2-butene 0.009
nonflammable liquid. It is soluble in about 50 parts of
water, and is miscible with alcohol, with acetone, with Dilute the standard stepwise with high-purity DCM to
chloroform, and with ether. Its refractive index at 20° is create a series of standards in the range of approximately
about 1.424. 10 to 300 mg/kg, except for propylene oxide, which
Function: Extraction solvent should be in the range of 0.06 to 2.4 (w/w%).
Packaging and Storage: Store in tight containers. [NOTE—Assay the DCM used to prepare the Standard
solution without the analytes to determine the possible
ASSAY presence of the analytes, and make any necessary
• PROCEDURE corrections.]
Standard solution: Prepare a standard solution Chromatographic system, Appendix IIA
containing appropriate concentrations of methyl Mode: Gas chromatography
chloride, chloroform, methylene chloride, vinyl chloride, Detector: Flame ionization
ethyl chloride, vinylidene chloride, 2-methyl-2-butene, Column 1: 30-m × 0.32-mm (id) fused-silica capillary
trans-1,2-dichloroethylene, cyclohexane, and propylene column, or equivalent, coated with 1.8-µm film of (6%
oxide in high-purity dichloromethane (DCM) by adding cyanopropylphenyl) methylpolysiloxane liquid phase,
each reagent to DCM in a glass bottle fitted with a or equivalent
silicone rubber septum. Inject the listed analytes into Column 2: 25-m × 0.53-mm (id) fused-silica capillary
the bottle by accurately weighing a syringe containing column coated with a 2.0-µm film of 5% phenyl/95%
the analyte, injecting the analyte through the septum, methylsilicone liquid phase, or equivalent
and reweighing the syringe to determine the amount of [NOTE—Connect the two columns in series with Column
analyte added. Add sufficient amounts of each analyte 2 being behind Column 1.]
to obtain these approximate concentrations: Temperature
Column oven: 40° (isothermal)
Injector: 150°
Detector: 250°
FCC 9 Monographs / Methylparaben / 807

Carrier gas: Helium and a few drops of starch TS to the aqueous phase, and
Flow rate: 4.4 mL/min allow it to stand for 5 min.
Injection volume: 1 to 5 µL Acceptance criteria: A blue color does not appear.
Injection type: Split injection mode • NONVOLATILE RESIDUE
Split flow rate: 98 mL/min Sample: 38 mL (about 50 g)
Analysis: Separately inject the Standard solution and the Analysis: In a fume hood, evaporate the Sample to
sample into the chromatograph. Determine the peak dryness in a tared dish on a steam bath, dry the residue
areas by electronic integration. Plot peak area against at 105° for 30 min, cool, and weigh.
concentration for each analyte corrected for the blank Acceptance criteria: NMT 0.015%
to construct a standard curve. Determine the • SPECIFIC GRAVITY: Determine by any reliable method (see

Monographs
concentration of additives and byproducts in the General Provisions).
sample by comparison to the standard curve. Acceptance criteria: Between 1.318 and 1.323
Approximate retention times for the components of the • WATER, Water Determination, Appendix IIB
Standard solution are as follows: Acceptance criteria: NMT 0.02%

Approximate retention time

Chemical name (RT)

Methylparaben
.

methyl chloride 2.8

vinyl chloride 3.0
First Published: Prior to FCC 6
ethyl chloride 3.5 Last Revision: Third Supplement, FCC 7
propylene oxide 4.1
2-methyl-2-butene 4.5 Methyl p-Hydroxybenzoate
vinylidene chloride 4.6
dichloromethane 5.3
trans-1,2- 5.9
dichloroethylene
chloroform 8.7
C8H8O3 Formula wt 152.15
cyclohexane 10.5
INS: 218 CAS: [99-76-3]
carbon tetrachloride 12.0
UNII: A2I8C7HI9T [methylparaben]
Acceptance criteria: The sum of the concentrations of DESCRIPTION
the impurities and stabilizers is less than 1.0%. (NLT Methylparaben occurs as small, colorless crystals or as a
99.0% CH2Cl2) white, crystalline powder. One g dissolves in about 400 mL
of water at 25°, in about 50 mL of water at 80°, in about
IMPURITIES
2.5 mL of alcohol, in about 7 mL of ether, and in about 4
Inorganic Impurities
mL of propylene glycol. It is slightly soluble in glycerin and
• LEAD, Lead Limit Test, Atomic Absorption Spectrophotometric
in fixed oils.
Graphite Furnace Method, Method I, Appendix IIIB
Function: Preservative; antimicrobial agent
Acceptance criteria: NMT 1 mg/kg
Packaging and Storage: Store in well-closed containers.
SPECIFIC TESTS
• ACIDITY (AS HCL)
IDENTIFICATION
• INFRARED ABSORPTION, Spectrophotometric Identification
Sample: 100 mL
Tests, Appendix IIIC
Analysis: Transfer the Sample into a separatory funnel,
Reference standard: USP Methylparaben RS
add 100 mL of neutralized water, and shake vigorously
Sample and standard preparation: M
for 2 min. Allow the layers to separate, transfer the
Acceptance criteria: The spectrum of the sample
aqueous phase into an Erlenmeyer flask, add 4 drops of
exhibits maxima at the same wavelengths as those in
bromothymol blue TS, and titrate with 0.01 N sodium
the spectrum of the Reference standard.
hydroxide.
• MELTING RANGE OR TEMPERATURE DETERMINATION, Appendix
Acceptance criteria: Not more than 3.6 mL 0.01 N
IIB
sodium hydroxide is required for the titration of the
Sample preparation: Dissolve 500 mg of sample in 10
Sample. (NMT 10 mg/kg)
mL of 1 N sodium hydroxide, boil for 30 min, allow the
• DISTILLATION RANGE, Appendix IIB
solution to evaporate to a volume of about 5 mL, and
Acceptance criteria: Between 39.0° and 41.0°
cool. Acidify the solution with 2 N sulfuric acid, collect
• FREE HALOGENS
the resulting p-hydroxybenzoic acid crystals on a filter,
Sample: 10 mL
wash several times with small portions of water, and
Analysis: Transfer the Sample to a separatory funnel, add
dry in a desiccator over silica gel.
25 mL of water, and shake vigorously for 1 min. Allow
Acceptance criteria: The Sample preparation so obtained
the layers to separate, and then remove and discard the
melts between 212° and 217°.
lower sample layer. Add 1 mL of potassium iodide TS
 808 / Methylparaben / Monographs FCC 9

ASSAY neutral to litmus. Add 0.2 mL of 0.1 N sodium

• PROCEDURE hydroxide and 2 drops of methyl red TS to 10 mL of
Mobile phase: Methanol and a 6.8-g/L solution of the filtrate.
potassium dihydrogen phosphate (65:35 v/v) Acceptance criteria: The solution is yellow, without
Sample solution: Dissolve 50.0 mg in 2.5 mL of even a light cast of pink.
methanol, and dilute with Mobile phase to 50 mL. • LOSS ON DRYING, Appendix IIC: Over silica gel for 5 h
Dilute 10.0 mL of this solution with Mobile phase to Acceptance criteria: NMT 0.5%
100 mL. • MELTING RANGE OR TEMPERATURE DETERMINATION, Appendix
Standard solution: Dissolve 50.0 mg of USP IIB
Methylparaben RS in 2.5 mL of methanol, and dilute Acceptance criteria: 125°–128°
Monographs

with Mobile phase to 50 mL. Dilute 10.0 mL of this • RESIDUE ON IGNITION (SULFATED ASH), Appendix IIC
solution with Mobile phase to 100 mL. Sample: 4 g
Chromatographic system, Appendix IIA Acceptance criteria: NMT 0.05%
Mode: High-performance liquid chromatography
Detector: UV 272 nm
Column: 4.6-mm × 15-cm column packed with
2-Methylpentanoic Acid
.

octadecyl silane chemically bonded to porous silica or

ceramic microparticles 5 µm in diameter First Published: Prior to FCC 6
Flow rate: 1.3 mL/min
[NOTE—The run time is about 5 times the retention
time of methylparaben.]
Injection size: 10 µL
System suitability
Sample: Standard solution
Suitability requirement: The relative standard
C6H12O2 Formula wt 116.16
deviation for 6 injections is NMT 0.85%.
FEMA: 2754
Analysis: Separately inject the Sample solution and the
Standard solution into the chromatograph. Record the UNII: 26A19CG6J9 [2-methylpentanoic acid]
chromatograms and calculate the percentage of
DESCRIPTION
methylparaben in the sample taken:
2-Methylpentanoic Acid occurs as a colorless to pale yellow
Result = (rU/rS) × (CS/CU) × 100 liquid.
Odor: Caramel, pungent
rU = peak area of methylparaben from the Boiling Point: ∼196° to 197°
chromatogram of the Sample solution Solubility in Alcohol, Appendix VI: One mL dissolves in 1
rS = peak area of methylparaben from the mL of 95% alcohol.
chromatogram of the Standard solution Function: Flavoring agent
CS = concentration of USP Methylparaben RS in
the Standard solution, corrected for purity IDENTIFICATION
(mg/mL) • INFRARED SPECTRA, Spectrophotometric Identification Tests,
CU = concentration of the Sample solution (mg/ Appendix IIIC
mL) Acceptance criteria: The spectrum of the sample
Acceptance criteria: 99.0%–100.5%, calculated on the exhibits relative maxima at the same wavelengths as
dried basis those of the spectrum below.

IMPURITIES ASSAY
Inorganic Impurities • PROCEDURE: Proceed as directed under M-3a, Appendix
• LEAD, Lead Limit Test, Flame Atomic Absorption XI.
Spectrophotometric Method, Appendix IIIB Acceptance criteria: NLT 98.0% of C6H12O2
Sample: 10 g
SPECIFIC TESTS
Acceptance criteria: NMT 2 mg/kg
• REFRACTIVE INDEX, Appendix II: At 20°
SPECIFIC TESTS Acceptance criteria: Between 1.411 and 1.416
• ACIDITY • SPECIFIC GRAVITY: Determine at 25° by any reliable
Sample: 750 mg method (see General Provisions).
Analysis: Mix the Sample with 15 mL of water, heat at Acceptance criteria: Between 0.916 and 0.923
80° for 1 min, cool, and filter. The filtrate is acid or
 FCC 9 Monographs / 2-Methylpyrazine / 809

Monographs
2-Methylpentanoic Acid

Acceptance criteria: The spectrum of the sample

2-Methylpyrazine
.

exhibits relative maxima at the same wavelengths as

First Published: Prior to FCC 6 those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1a, Appendix
XI.
Acceptance criteria: NLT 99.0% of C5H6N2

C5H6N2 Formula wt 94.12

SPECIFIC TESTS
• REFRACTIVE INDEX, Appendix II: At 20°
FEMA: 3309
Acceptance criteria: Between 1.504 and 1.506
UNII: RVC6500U9C [2-methylpyrazine]
• SPECIFIC GRAVITY: Determine at 25° by any reliable
DESCRIPTION method (see General Provisions).
2-Methylpyrazine occurs as a colorless to slightly yellow Acceptance criteria: Between 1.010 and 1.030
liquid. OTHER REQUIREMENTS
Odor: Nutty, cocoa • WATER, Water Determination, Method I, Appendix IIB
Solubility: Miscible in water, alcohol, acetone, most fixed [NOTE—Use freshly distilled pyridine as solvent.]
oils Acceptance criteria: NMT 0.5%
Boiling Point: ∼137°
Function: Flavoring agent

IDENTIFICATION
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Appendix IIIC
 810 / 2-Methylpyrazine / Monographs FCC 9
Monographs

2-Methylpyrazine

Function: Flavoring agent

3-Methylthiopropionaldehyde
.

IDENTIFICATION
First Published: Prior to FCC 6
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Last Revision: First Supplement, FCC 6
Appendix IIIC
Acceptance criteria: The spectrum of the sample
Methional exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1a, Appendix
C4H8OS Formula wt 104.17 XI.
FEMA: 2747 Acceptance criteria: NLT 98.0% of C4H8OS
UNII: 0AAO8V0F1R [3-methylthiopropionaldehyde]
SPECIFIC TESTS
DESCRIPTION • REFRACTIVE INDEX, Appendix II: At 20°
3-Methylthiopropionaldehyde occurs as a colorless to pale Acceptance criteria: Between 1.484 and 1.493
yellow liquid. It may contain a suitable antioxidant. • SPECIFIC GRAVITY: Determine at 25° by any reliable
Odor: Meaty potato method (see General Provisions).
Boiling Point: ∼165° to 166° Acceptance criteria: Between 1.038 and 1.048
Solubility in Alcohol, Appendix VI: One mL dissolves in 1
mL of 95% alcohol.
 FCC 9 Monographs / 2-Methylundecanal / 811

Monographs
3-Methylthiopropionaldehyde

Boiling Point: ∼171°

2-Methylundecanal
.

Function: Flavoring agent

First Published: Prior to FCC 6
IDENTIFICATION
Last Revision: First Supplement, FCC 6
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Appendix IIIC
Aldehyde C-12 MNA Acceptance criteria: The spectrum of the sample
Methyl n-Nonyl Acetaldehyde exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1b, Appendix
XI.
C12H24O Formula wt 184.32 Acceptance criteria: NLT 94.0% of C12H24O
FEMA: 2749
UNII: S94QNS2VY5 [2-methylundecanal] SPECIFIC TESTS
• ACID VALUE, FLAVOR CHEMICALS (OTHER THAN ESSENTIAL
DESCRIPTION OILS), M-15, Appendix XI
2-Methylundecanal occurs as a colorless to slightly yellow Acceptance criteria: NMT 10.0
liquid. It may contain a suitable antioxidant. • REFRACTIVE INDEX, Appendix II: At 20°
Odor: Fatty Acceptance criteria: Between 1.431 and 1.436
Solubility: Soluble in most fixed oils, alcohol, propylene • SPECIFIC GRAVITY: Determine at 25° by any reliable
glycol (may be turbid); insoluble or practically insoluble in method (see General Provisions).
glycerin Acceptance criteria: Between 0.822 and 0.830
 812 / 2-Methylundecanal / Monographs FCC 9
Monographs

2-Methylundecanal

Function: Flavoring agent

4-p-Methoxyphenyl-2-butanone
.

IDENTIFICATION
First Published: Prior to FCC 6
• INFRARED SPECTRA, Spectrophotometric Identification Tests,
Appendix IIIC
Anisyl Acetone Acceptance criteria: The spectrum of the sample
exhibits relative maxima at the same wavelengths as
those of the spectrum below.

ASSAY
• PROCEDURE: Proceed as directed under M-1a, Appendix
C11H14O2 Formula wt 178.23 XI.
FEMA: 2672 Acceptance criteria: NLT 98.0% of C11H14O2
UNII: GVG47S4S5V [anisylacetone] SPECIFIC TESTS
• REFRACTIVE INDEX, Appendix II: At 20°
DESCRIPTION Acceptance criteria: Between 1.517 and 1.521
4-p-Methoxyphenyl-2-butanone occurs as a colorless to pale
• SPECIFIC GRAVITY: Determine at 25° by any reliable
yellow liquid.
method (see General Provisions).
Odor: Sweet, floral, fruity
Acceptance criteria: Between 1.042 and 1.048
Boiling Point: ∼277°
Solubility in Alcohol, Appendix VI: One mL dissolves in 1
mL of 95% alcohol.
 FCC 9 Monographs / Mineral Oil, High Viscosity / 813

Monographs
4-p-Methoxyphenyl-2-butanone

IDENTIFICATION
Mineral Oil, High Viscosity
.

• CARBON NUMBER AT 5% DISTILLATION POINT1

First Published: Second Supplement, FCC 7 [NOTE—“Carbon Number” is the number of carbon
atoms in a molecule.]
Liquid Petrolatum System suitability solution: 1% each of hexadecane
Liquid Paraffin and octadecane in n-octane
CAS: [8012-95-1] Calibration solution: Prepare a mixture of hydrocarbons
INS: 905a of known boiling points covering the range of the
UNII: N6K5787QVP [light mineral oil] sample. At least one compound must have a boiling
point lower than the initial boiling point of the sample.
DESCRIPTION Chromatographic system, Appendix IIA
Mineral Oil, High Viscosity occurs as a colorless, transparent, [NOTE—Use a suitable gas chromatograph. Typical
oily liquid, free or nearly free from fluorescence. It is a conditions that may be used in the system are
mixture of refined liquid hydrocarbons, essentially paraffinic identified below.]
and naphthenic in nature, obtained from petroleum by Mode: Gas chromatography
solvent extraction and/or crystallization with subsequent Detector: Flame ionization
purification by acid treatment and/or hydrogen treatment. Packed column: 5% SE-30 or equivalent
It has an initial boiling point above 350°. Its average Carrier gas: Helium
molecular weight is NLT 500. It is insoluble in water and Column temperature: 10°–350°, at a rate of 6.5°/min
sparingly soluble in alcohol, soluble in volatile oils, and Detector temperature: 370°
miscible with most fixed oils, but not with castor oil. It Injection block temperature: 370°
may contain any antioxidant permitted in food in an System suitability
amount not greater than that required to produce its Suitability requirement 1: The peak height for the
intended effect. dodecane peak is NLT 10% of full scale under the
Function: Lubricant; release agent; protective coating conditions used for the Calibration solution.
Packaging and Storage: Store in tight containers. Suitability requirement 2: The baseline drift, when
the chromatographic system is operated at the

1 As determined by ASTM D2887 Standard Test Method for Boiling Range

Distribution of Petroleum Fractions by Gas Chromatography. The original

ASTM method is available in its entirety from ASTM International, 100 Barr
Harbor Drive, West Conshohocken, PA 19428. Phone: 610-832-9555; email:
[email protected]; website: www.astm.org.
 814 / Mineral Oil, High Viscosity / Monographs FCC 9

required sensitivity level to meet Suitability SPECIFIC TESTS

requirement 1, is NMT 1% of full scale per hour for • READILY CARBONIZABLE SUBSTANCES
the Calibration solution. Chromic acid cleaning mixture: Dissolve 200 g of
Suitability requirement 3: Retention times have a sodium dichromate in 100 mL of water to which 1500
repeatability of NMT 6 s for each component of the mL of sulfuric acid has been added, slowly with stirring.
Calibration solution. Sample: 5 mL
Suitability requirement 4: The resolution, R, Control solution: Mix 3 mL of ferric chloride CS, 1.5
determined for the System suitability solution is mL of cobaltous chloride CS, and 0.5 mL of cupric
between 3 and 8 when calculated by: sulfate CS in a glass-stoppered test tube that previously
has been rinsed with Chromic acid cleaning mixture, then
Monographs

R = 2d/(W1 + W2) rinsed with water, and dried. Overlay this mixture with
d = distance between the peak maxima of 5 mL of mineral oil.
hexadecane and octadecane (mm) Analysis: Place the Sample in a glass-stoppered test tube
W1 = hexadecane peak width at baseline (mm) that previously has been rinsed with Chromic acid
W2 = octadecane peak width at baseline (mm) cleaning mixture, then rinsed with water, and dried. Add
Calibration curve: Cool the column to the selected 5 mL of 94.5% to 94.9% sulfuric acid; while
starting temperature (the retention time for the initial simultaneously starting a stopwatch, place the tube in a
boiling point must be NLT 1 min) and inject the boiling water bath. After the test tube has been in the
Calibration solution. For each component, record the bath for 30 s, use a 3-s time span to remove it, and
retention time of the peak maximum and the peak while holding the stopper in place, give three vigorous
areas. Plot the retention time of each peak versus the vertical shakes over an amplitude of about 5 in, then
corresponding normal boiling point of that component, return it to the bath. Repeat every 30 s until exactly 10
in C°, to obtain a calibration curve. min has passed, then remove the test tube.
Analysis: Using the conditions for the Calibration curve, Acceptance criteria: The Sample remains unchanged in
inject a sample. Record the area of each time segment color, and the acid does not become darker than the
at fixed time intervals NMT 1% of the retention time standard color of the Control solution.
equivalent to a boiling point of 538° obtained from the • SPECIFIC GRAVITY Determine by any reliable method (see
Calibration curve. General Provisions).
Sum the area segments to obtain the cumulative area at Acceptance criteria: NLT that stated, or within the
each time interval during the run. At the point of the range claimed by the vendor
chromatogram where the baseline at the end first • ULTRAVIOLET ABSORBANCE (POLYNUCLEAR HYDROCARBONS)
becomes steady, observe the cumulative area counts. Hexane: Use a pure grade of hexane (predominantly n-
Move back along the record until a cumulative area hexane and methylcyclopentane) having an ultraviolet
equal to 99.5% of the total at the steady point appears. absorbance not exceeding 0.10 down to 220 nm and
Mark this point as the final boiling point. Observe the not exceeding 0.02 down to 260 nm. The purity should
area counts at the start of the run until the point is be such that the Solvent control as defined below, has
reached where the cumulative area count is equal to an absorbance curve, compared to water, showing no
0.5% of the total area. Mark this point as the initial extraneous impurity peaks and no absorbance
boiling point of the sample. Divide the cumulative area exceeding that of dimethyl sulfoxide, compared to
at each interval between the initial and final boiling water, at any wavelength in the range 260–400 nm. If
points by the total cumulative area and multiply by necessary to obtain the prescribed purities, the hexane
100. This will give the cumulative percent of the sample may be passed through activated silica gel.
recovered at each time interval. Tabulate the cumulative Dimethyl sulfoxide: Use a pure grade of dimethyl
percent recovered at each interval and the retention sulfoxide (99.9%, melting point: 18°) that has a clear,
time at the end of the interval. Using linear water-white appearance; has an absorbance curve,
interpolation, if necessary, determine the retention time compared with water, not exceeding 1.0 at 264 nm;
associated with 5% and read the corresponding boiling and shows no extraneous impurity peaks in the
temperature from the Calibration curve. wavelength range up to 400 nm. Store in glass-
Acceptance criteria: The carbon number is NLT 28 at stoppered bottles.
5% distillation. The boiling point at 5% distillation is Apparatus: Use 125-mL glass-stoppered separatory
higher than 422°. funnels equipped with tetrafluoroethylene polymer
stopcocks or other suitable stopcocks that will not
IMPURITIES contaminate the solvents.
Inorganic Impurities Sample preparation: Transfer 25 mL of the sample and
• LEAD, Lead Limit Test, Atomic Absorption Spectrophotometric 25 mL of Hexane to a separatory funnel and mix. Add
Graphite Furnace Method, Method II, Appendix IIIB 5.0 mL of Dimethyl sulfoxide, shake the mixture
Acceptance criteria: NMT 1 mg/kg vigorously for at least 1 min, and allow it to stand until
the lower layer is clear. Completely transfer the lower
layer to a second separatory funnel, add 2 mL of
Hexane, and shake the mixture vigorously. Allow it to
 FCC 9 Monographs / Mineral Oil, Medium and Low Viscosity / 815

stand until the lower layer is clear, and then draw off IDENTIFICATION
the lower layer, designated as the Sample preparation. • CARBON NUMBER AT 5% DISTILLATION POINT1
Solvent control: In a separatory funnel, vigorously shake [NOTE—“Carbon Number” is number of carbon atoms in
5.0 mL of Dimethyl sulfoxide with 25 mL of Hexane for a molecule.]
at least 1 min, allow it to stand until the lower layer is System suitability solution: 1% each of hexadecane
clear, and draw off this layer, designated as Solvent and octadecane in n-octane
control. Calibration solution: Prepare a mixture of hydrocarbons
Standard solution: Use a standard reference solution of of known boiling points covering the range of the
naphthalene (National Institute of Standards and sample. At least one compound must have a boiling
Technology, Standard Material No. 577 or a solution of point lower than the initial boiling point of the sample.

Monographs
equivalent purity) containing a concentration of 7.0 Chromatographic system, Appendix IIA
mg/mL in purified isooctane. [NOTE—Use a suitable gas chromatograph. Typical
Analysis: Determine the absorbance of the Sample conditions that may be used in the system are
preparation and the Solvent control in a 1-cm cell in the identified below.]
range 260–400 nm. Mode: Gas chromatography
Determine the absorbance of the Standard solution at Detector: Flame ionization
275 nm measured against isooctane of the same Packed column: 5% SE-30 or equivalent
spectral purity in 1-cm cells. (The absorbance will be Carrier gas: Helium
approximately 0.30.) Temperature
[NOTE—Make suitable corrections of the absorbance Column: 10°–350°, at a rate of 6.5°/min
when testing samples containing added antioxidants.] Detector: 370°
Acceptance criteria: The absorbance of the Sample Injection block: 370°
preparation does not exceed that of the Solvent control System suitability
at any wavelength in the specified range by more than Suitability requirement 1: The peak height for the
one-third of the absorbance of the Standard solution. dodecane peak is NLT 10% of full scale under the
• VISCOSITY: Determine by any reliable method (see conditions used for the Calibration solution.
Viscosity Determination, Appendix IIB). Suitability requirement 2: The baseline drift, when
Acceptance criteria: NLT 11 centistokes at 100° the Chromatographic system is operated at the
required sensitivity level to meet Suitability
requirement 1, is NMT 1% of full scale per hour for
the Calibration solution.
Mineral Oil, Medium and Low Viscosity
.

Suitability requirement 3: Retention times have a

First Published: Prior to FCC 6 repeatability of NMT 6 s for each component of the
Last Revision: Second Supplement, FCC 7 Calibration solution.
Suitability requirement 4: The resolution, R,
determined for the System suitability solution is
Liquid Petrolatum
between 3 and 8 when calculated by:
Liquid Paraffin
White Mineral Oil R = 2d/(W1 + W2)
CAS: [8042-47-5]
UNII: T5L8T28FGP [mineral oil] d = distance between the peak maxima of
hexadecane and octadecane (mm)
DESCRIPTION W1 = hexadecane peak width at baseline (mm)
Mineral Oil, Medium and Low Viscosity occurs as a colorless, W2 = octadecane peak width at baseline (mm)
transparent, oily liquid, free or nearly free from Calibration curve: Cool the column to the selected
fluorescence. It is a mixture of refined liquid hydrocarbons, starting temperature (the retention time for the initial
essentially paraffinic and naphthenic in nature, obtained boiling point must be NLT 1 min) and inject the
from petroleum by solvent extraction and/or crystallization Calibration solution. Record for each component the
with subsequent purification by acid treatment and/or retention time of each peak maximum and the peak
hydrogen treatment. It has an initial boiling point above areas. Plot the retention time of each peak versus the
200°. Its average molecular weight is between 300 and corresponding normal boiling point of that component,
500. It is insoluble in water and in alcohol, is soluble in in °C, to obtain a calibration curve.
volatile oils, and is miscible with most fixed oils, but not Analysis: Using the conditions for the Calibration curve,
with castor oil. It may contain any antioxidant permitted in inject a sample. Record the area of each time segment
food in an amount not greater than that required to at fixed time intervals NMT 1% of the retention time
produce its intended effect. equivalent to a boiling point of 538° obtained from the
Function: Defoaming agent; release agent; glazing agent; Calibration curve.
sealing agent
Packaging and Storage: Store in tight containers. 1As determined by ASTM D2887 Standard Test Method for Boiling Range
Distribution of Petroleum Fractions by Gas Chromatography. The original
ASTM method is available in its entirety from ASTM International, 100 Barr
Harbor Drive, West Conshohocken, PA 19428. Phone: 610-832-9555; email:
[email protected]; website: www.astm.org.
 816 / Mineral Oil, Medium and Low Viscosity / Monographs FCC 9

Sum the area segments to obtain the cumulative area at • ULTRAVIOLET ABSORBANCE (POLYNUCLEAR HYDROCARBONS)
each time interval during the run. At the point of the Hexane: Use a pure grade of hexane (predominantly n-
chromatogram where the baseline at the end first hexane and methylcyclopentane) having an ultraviolet
becomes steady, observe the cumulative area counts. absorbance not exceeding 0.10 down to 220 nm and
Move back along the record until a cumulative area not exceeding 0.02 down to 260 nm. The purity should
equal to 99.5% of the total at the steady point appears. be such that the Solvent control as defined below, has
Mark this point as the final boiling point. Observe the an absorbance curve, compared to water, showing no
area counts at the start of the run until the point is extraneous impurity peaks and no absorbance
reached where the cumulative area count is equal to exceeding that of dimethyl sulfoxide, compared to
0.5% of the total area. Mark this point as the initial water, at any wavelength in the range 260 to 420 nm,
Monographs

boiling point of the sample. Divide the cumulative area inclusive. If necessary to obtain the prescribed purities,
at each interval between the initial and final boiling the hexane may be passed through activated silica gel.
points by the total cumulative area and multiply by Dimethyl sulfoxide: Use a pure grade of dimethyl
100. This will give the cumulative percent of the sample sulfoxide (99.9%, melting point: 18°) that has a clear,
recovered at each time interval. Tabulate the cumulative water-white appearance; has an absorbance curve,
percent recovered at each interval and the retention compared with water, not exceeding 1.0 at 264 nm;
time at the end of the interval. Using linear and shows no extraneous impurity peaks in the
interpolation, if necessary, determine the retention time wavelength range up to 420 nm. Store in glass-
associated with 5% and read the corresponding boiling stoppered bottles.
temperature from the Calibration curve. Apparatus: Use 125-mL glass-stoppered separatory
Acceptance criteria: Carbon number is between 17 and funnels equipped with tetrafluoroethylene polymer
25 at 5% distillation. The boiling point at the 5% stopcocks or other suitable stopcocks that will not
distillation is between 287° and 422°. contaminate the solvents.
Sample preparation: Transfer 25 mL of sample and 25
IMPURITIES mL of Hexane to a separatory funnel and mix. Add 5.0
Inorganic Impurities mL of Dimethyl sulfoxide, shake the mixture vigorously
• LEAD, Lead Limit Test, Atomic Absorption Spectrophotometric for at least 1 min, and allow it to stand until the lower
Graphite Furnace Method, Method II, Appendix IIIB layer is clear. Completely transfer the lower layer to a
Acceptance criteria: NMT 1 mg/kg second separatory funnel, add 2 mL of Hexane, and
shake the mixture vigorously. Allow it to stand until the
SPECIFIC TESTS
lower layer is clear, and then draw off the lower layer,
• READILY CARBONIZABLE SUBSTANCES
designated as the Sample preparation.
Chromic acid cleaning mixture: Dissolve 200 g of
Solvent control: In a separatory funnel, vigorously shake
sodium dichromate in 100 mL of water to which 1500
5.0 mL of Dimethyl sulfoxide with 25 mL of Hexane for
mL of sulfuric acid has been added, slowly with stirring.
at least 1 min, allow it to stand until the lower layer is
Sample: 5 mL
clear, and draw off this layer, designated as Solvent
Control solution: Mix 3 mL of ferric chloride CS, 1.5
control.
mL of cobaltous chloride CS, and 0.5 mL of cupric
Standard solution: Use a standard reference solution of
sulfate CS in a glass-stoppered test tube that previously
naphthalene (National Institute for Standards and
has been rinsed with Chromic acid cleaning mixture, then
Technology Standard Material No. 577, or a solution of
rinsed with water, and dried. Overlay this mixture with
equivalent purity) containing a concentration of
5 mL of mineral oil.
7.0 mg/1000 mL in purified isooctane.
Analysis: Place the Sample in a glass-stoppered test tube
Analysis: Determine the absorbance of the Sample
that previously has been rinsed with Chromic acid
preparation and the Solvent control in a 1-cm cell in the
cleaning mixture, then rinsed with water, and dried. Add
range 260 to 420 nm, inclusive.
5 mL of 94.5%–94.9% sulfuric acid; while
Determine the absorbance of the Standard solution at
simultaneously starting a stopwatch, place the tube in a
275 nm measured against isooctane of the same
boiling water bath. After the test tube has been in the
spectral purity in 1-cm cells. (The absorbance will be
bath for 30 seconds, use a 3-second time span to
approximately 0.30.)
remove it, and while holding the stopper in place, give
[NOTE—Make suitable corrections of the absorbance
three vigorous vertical shakes over an amplitude of
when testing samples containing added antioxidants.]
about 5 in, then return it to the bath. Repeat every 30
Acceptance criteria: The absorbance of the Sample
seconds until exactly 10 min has passed, then remove
preparation does not exceed that of the Solvent control
the test tube.
at any wavelength in the specified range by more than
Acceptance criteria: The Sample remains unchanged in
one-third of the absorbance of the Standard solution.
color, and the acid does not become darker than the
• VISCOSITY: Determine by any reliable method (see
standard color of the Control solution.
Viscosity Determincation, Appendix IIB).
• SPECIFIC GRAVITY: Determine by any reliable method (see
Acceptance criteria: Between 3 and 11 centistokes at
General Provisions).
100°
Acceptance criteria: NLT that stated, or within the
range claimed by the vendor
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FCC 9 Monographs / Monk Fruit Extract / 817

temperature, and dissolve the residue in 2 mL of

Monk Fruit Extract
.

methanol.
First Published: Third Supplement, FCC 7 Sample solution: Prepare a solution by dissolving 50
Last Revision: First Supplement, FCC 8 mg of the sample in 20 mL of water. Extract the
aqueous solution twice, using 10 mL of n-butanol each
time, and combine the n-butanol extracts. Evaporate
Luo Han Fruit Concentrate
the combined n-butanol extract at room temperature,
Luo Han Guo Concentrate
and dissolve the residue in 2 mL of methanol.
Luo Han Guo Extract
Adsorbent: 0.25-mm layer of chromatographic silica
Monk Fruit Concentrate
gel, prepared with a gypsum (calcium sulfate
Siraitia grosvenorii Extract

Monographs
hemihydrate) binder
Developing solvent system: n-Butanol, acetic acid, and
water (4:1:1)
Spray reagent: 10% sulfuric acid solution
Application volume: 2 µL
Analysis: After developing the plate in the Developing
solvent system, remove the plate from the developing
chamber, and allow the solvent to evaporate. Spray the
plate with the Spray reagent, and heat at 105° to allow
color development.
Acceptance criteria: The principal spot obtained from
the Sample solution corresponds in color and RF value to
that obtained from Standard solution A. The
chromatogram obtained from the Sample solution
C60H102O29 (Mogroside V) Formula wt, Mogroside V 1286
CAS: Mogroside V [88901-36-4] corresponds to that obtained from Standard solution B
in the placement and color of the spots.
DESCRIPTION
Monk Fruit Extract occurs as an off-white to light yellow ASSAY
powder. It is an extract of the fruit luo han guo (Siraitia • MOGROSIDE V CONTENT
grosvenorii Swingle, also known as monk fruit) that has Mobile phase: Acetonitrile and water (22:78)
been concentrated to optimize the concentration of Standard solution: 0.10 mg/mL of USP Mogroside V RS
mogroside V. It is obtained through water extraction of the in Mobile phase
mechanically crushed or shredded pulp of the fruit. The Sample solution: Dissolve 30 mg of the sample in
precipitate is removed by decanting, and the supernatant Mobile phase in a 50-mL volumetric flask. Sonicate the
is cooled and passed through a food-grade copolymer solution for 40 min, cool to room temperature, and
resin which binds the target compounds. The resin is dilute with Mobile phase to volume. Filter the solution
flushed with cold ethanol to release the extracted through a 0.45-µm membrane.
compounds, and the effluent is heated under vacuum to Chromatographic system, Appendix IIA
remove the ethanol, then spray dried. Monk Fruit Extract is Mode: High-performance liquid chromatography
composed primarily of cucurbitane glycosides, known as Detector: UV 203 nm
mogrosides, with mogroside V being the principal Column: 4.6-mm × 250-mm column that contains 5-
sweetening component. Other components are mogroside µm porous silica microparticles chemically bonded to
II, mogroside III, mogroside IV, mogroside VI, flavonoids, octadecylsilane1
melanoidins, and protein fragments. Monk Fruit Extract is Column temperature: 25°
freely soluble in water. Although not a requirement for this Flow rate: 1.0 mL/min
monograph, users interested in analyzing this ingredient Injection size: 20 µL
for potential pesticide residues may use the informational Analysis: Separately inject the Standard solution and the
method found under Pesticide Residues in Appendix XIII. Sample solution into the chromatograph, record the
Function: Non-nutritive sweetener chromatograms, and measure the areas for the major
Packaging and Storage: Store in tight, light-resistant peaks in the respective chromatograms. [NOTE—The
containers. Avoid exposure to excessive heat. approximate retention time for mogroside V is 15.7
min.] Using the peak area obtained from the
IDENTIFICATION chromatogram of the Standard solution, determine the
• THIN-LAYER CHROMATOGRAPHY, Appendix IIA percentage of mogroside V in the Sample solution:
Standard solution A: 7.5 mg/mL of USP Mogroside V
RS in methanol. Sonicate to aid dissolution. Result = (rU/rS) × (CS/CU) × 100
Standard solution B: Prepare a solution by dissolving rU = peak area of mogroside V obtained from the
50 mg of USP Monk Fruit Extract RS in 20 mL of water. chromatogram of the Sample solution
Extract the aqueous solution twice, using 10 mL of n-
butanol each time, and combine the n-butanol extracts. 1 ZORBAX SB-C18 (Agilent Technologies); Symmetry Shield RP 18 (Waters

Evaporate the combined n-butanol extract at room Corporation); or equivalent. Use a compatible guard column (C18, 5-µm,
4.6-mm × 7.5-mm).