Accessed from 218.202.219.

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FCC 7 Monographs / Monoammonium Glycyrrhizinate / 695

Monographs
Monoammonium L-Glutamate (Mineral Oil Mull)

Packaging and Storage: Store in a cool, dry place in a

Monoammonium Glycyrrhizinate
.

tight container.
First Published: Prior to FCC 6
IDENTIFICATION
• AMMONIUM, Appendix IIIA
Ammonium Glycyrrhizinate, Pentahydrate Acceptance criteria: Passes test
Ammonium Glycyrrhizinate
ASSAY
• PROCEDURE
[NOTE—This procedure is based on AOAC method
982.19.]
Mobile phase: Acetonitrile, acetic acid and water
(38:1:61), degassed. [NOTE—The water used should be
glass-distilled and filtered through a 0.45-µm filter
(Millipore, or equivalent).]
Standard solution: Dissolve 10 mg (on the dried basis)
of monoammonium glycyrrhizinate standard for
analytical use (available from Sigma) in 20 mL of a 1:1
solution of acetonitrile:water, and filter through a 0.45-
µm Millipore filter, or equivalent. [NOTE—Prepare fresh
C42H65NO16·5H2O Formula wt anhydrous 839.98 daily.]
INS: 958 Sample solution: Dissolve 10 mg of sample in 20 mL of
a 1:1 solution of acetonitrile:water, and filter through a
DESCRIPTION
0.45-µm Millipore filter, or equivalent.
Monoammonium Glycyrrhizinate occurs as a white powder
Chromatographic system, Appendix IIA
with an intensely sweet taste. It is obtained by extraction
Mode: High-performance liquid chromatography
from ammoniated glycyrrhizin. It is soluble in ammonia
Detector: UV-254 nm (0.2 to 0.1 AUFS range)
water and is insoluble in glacial acetic acid.
Column: 30-cm × 4-mm (id), 10 µm particle size C18
Function: Flavoring agent
reverse-phase column (µBondapak C18, Waters Corp.,
or equivalent)

Copyright (c) 2011 The United States Pharmacopeial Convention. All rights reserved.
 Accessed from 218.202.219.1 by usand3 on Tue Dec 20 10:08:52 EST 2011
696 / Monographs / Monoammonium Glycyrrhizinate
Temperature: Room temperature
Flow rate: 2.0 mL/min. [NOTE—Maintain the Mobile
phase at a pressure and flow rate capable of giving the
required elution time (see System Suitability in High-
Performance Liquid Chromatography).]
Injection volume: About 10 µL
System suitability
Sample: Standard solution
Suitability requirement: The relative standard
deviation for duplicate injections is NMT 2.0%.
Monographs
Analysis: Separately inject, in duplicate, volumes of the
Standard solution and the Sample solution into the
chromatograph and determine the mean peak area for
each solution. [NOTE—The approximate retention time
for monoammonium glycyrrhizinate is 6 min.]
Calculate the percent monoammonium glycyrrhizinate,
equivalent to C42H65NO16, in the sample taken by the
formula:
Result = 100 × (20CS/WU) × (AU/AS)
CS = concentration (mg/mL) of the Standard
solution
WU = weight of sample (mg) taken to prepare the
Sample solution
AU = peak area of the Sample solution
AS = peak area of the Standard solution
Acceptance criteria: NLT 85.0% and NMT 102.0% of
C42H65NO16, calculated on the dried basis
SPECIFIC TESTS
• ASH (TOTAL), Appendix IIC
Acceptance criteria: NMT 0.5%
• LOSS ON DRYING, Appendix IIC: 78° for 4 h at 1-mm Hg
Sample: 1 g
Acceptance criteria: NMT 6.0%
• OPTICAL (SPECIFIC) ROTATION, Appendix IIB
Sample solution: 15 mg/mL in 40% ethanol. [NOTE—
Prepare using undried sample.]
Acceptance criteria: [α]D20 between +45° and +53°, on
the as-is basis
Monoglyceride Citrate
.
First Published: Prior to FCC 6
CAS: [36291-32-4]
DESCRIPTION
Monoglyceride Citrate occurs as a viscous, amber liquid. It is
a mixture of glyceryl monooleate and its citric acid
monoester, manufactured by the reaction of glyceryl
monooleate with citric acid under controlled conditions. It
is dispersible in most common fat solvents and in alcohol,
and it is insoluble in water.
Function: Solubilizer for antioxidants
Packaging and Storage: Store in well-closed containers.
Copyright (c) 2011 The United States Pharmacopeial Convention. All rights reserved.
FCC 7
IMPURITIES
Inorganic Impurities
• LEAD, Lead Limit Test, Flame Atomic Absorption
Spectrophotometric Method, Appendix IIIB
Sample: 10 g
Acceptance criteria: NMT 2 mg/kg
SPECIFIC TESTS
• ACID VALUE, Method II, Appendix VII
Acceptance criteria: Between 70 and 100
• RESIDUE ON IGNITION (SULFATED ASH), Appendix IIC
Sample: 1 g
Acceptance criteria: NMT 0.3%
• SAPONIFICATION VALUE, Appendix VII
Acceptance criteria: Between 260 and 265
• TOTAL CITRIC ACID
Standard solution: Transfer 35 mg of sodium citrate
dihydrate into a 100-mL volumetric flask, dissolve in
and dilute to volume with water and mix. Calculate the
concentration (µg/mL) of citric acid in the Standard
solution by the formula:
Result = 1000 × F × W/100
F = factor converting sodium citrate dihydrate
to citric acid, 0.6533
W = weight of the sodium citrate dihydrate
taken to prepare the Standard solution (mg)
Sample preparation: Transfer 150 mg into a
saponification flask, add 50 mL of 4% alcoholic
potassium hydroxide solution, and reflux for 1 h. Acidify
the reaction mixture with hydrochloric acid to a pH of
2.8 to 3.2, transfer into a 400-mL beaker, and
evaporate to dryness on a steam bath. Quantitatively
transfer the contents of the beaker into a separatory
funnel, using NMT 50 mL of water to rinse the beaker,
and then extract with three 50-mL portions of
petroleum ether (b.p. 30° to 60°), discarding the
extracts. Transfer the water layer to a 100-mL
volumetric flask, dilute to volume with water, and mix.
This dilution of the water layer is the Sample
preparation.
Analysis: Pipet 2.0 mL each the Standard solution and of
the Sample preparation into separate, 40-mL graduated
centrifuge tubes, and add 2 mL of 1:2 sulfuric acid and
11 mL of water to each tube. Boil for 3 min, cool, and
add 5 mL of bromine TS to each tube. Dilute to 20 mL,
allow to stand for 10 min, and centrifuge. Transfer 4.0
mL of each solution into separate 19- × 110-mm test
tubes, add 1 mL of water, 0.5 mL of 1:2 sulfuric acid,
and 0.3 mL of 1 M potassium bromide, and shake. Add
0.3 mL of 1.5 N potassium permanganate, shake, and
allow to stand for 2 min. Add 1 mL of a saturated
solution of ferrous sulfate, shake, allow to stand for 2
min, and then dilute to 10 mL with water. Add 10.0
mL of n-hexane (previously washed with sulfuric acid,
followed by a water wash, and then dried over
anhydrous sodium sulfate), shake vigorously for 2 min,
and then centrifuge at a low speed for 1 min. Transfer
5.0 mL of the hexane extract into a 20- × 145-mm
tube containing 10.0 mL of 40 mg/mL sodium sulfide