Stage 6 Harmonization

Official December 1, 2014 Sodium 1

. pletely extracted, as shown by a test with silver nitrate.

Dry the insoluble portion at 105° to constant weight,
Sodium Starch Glycolate and transfer an accurately weighed portion (700 mg)
of the dried 80% alcohol–insoluble portion to a suita-
Add the following: ble flask. Add 80 mL of glacial acetic acid, and heat the
mixture under reflux on a boiling water bath for 2 h.
Cool to room temperature, and titrate with 0.1 N per-
■Portions of this monograph that are national USP text, and
.

chloric acid VS, determining the endpoint

are not part of the harmonized text, are marked with potentiometrically.
symbols (◆◆) to specify this fact.■2S (NF32)
.

Calculate the percentage of sodium combined in the

Starch carboxymethyl ether, sodium salt. form of sodium starch glycolate:
DEFINITION Result = 100 × (22.99) × V × N/W
Sodium Starch Glycolate is the sodium salt of a carboxy-
methyl ether of starch or of a cross-linked carboxymethyl V = volume of perchloric acid consumed (mL)
ether of starch. It may contain NMT 7.0% of Sodium N = normality of the perchloric acid
Chloride. The pH and assay requirements for Type A and W = weight of the dried alcohol–insoluble residue
Type B are set forth in the accompanying table. taken for the Assay (mg)
Acceptance criteria: 2.8%–4.2% for Type A;
% Sodium, Combined 2.0%–3.4% for Type B
as Sodium Starch
OTHER COMPONENTS
pH Glycolate
• LIMIT OF SODIUM CHLORIDE
Type Min. Max. Min. Max. Sample: 500 mg of Sodium Starch Glycolate
A 5.5 7.5 2.8 4.2 Titrimetric system
B 3.0 5.0 2.0 3.4 (See Titrimetry 〈541〉.)
Mode: Direct titration
Titrant: 0.1 N silver nitrate VS
IDENTIFICATION Endpoint detection: Potentiometric
Electrodes
Change to read: Indicator: Suitable silver-based
Reference: Double junction electrode containing a
• ■◆
■2S (NF32) A. INFRARED ABSORPTION 〈197K〉■◆■2S (NF32) 10% potassium nitrate filling solution in the outer
jacket, and a standard filling solution in the inner
. . .

jacket
Change to read: Analysis: Transfer the Sample to a beaker, and suspend
in 100 mL of water. Add 1 mL of nitric acid. Titrate
• B. ■An■2S (NF32) acidified solution ■of it■2S (NF32) is colored
. . with the Titrant. Each mL of 0.1 N silver nitrate is
blue to violet by the addition of iodine and potassium equivalent to 5.844 mg of sodium chloride.
iodide TS 1. Acceptance criteria: NMT 7.0%

Change to read: Change to read:

• C. PROCEDURE • LIMIT OF SODIUM GLYCOLATE

Potassium pyroantimonate solution: ■Dissolve■2S (NF32) . [NOTE—Conduct this test without exposure to daylight.
2 g of potassium pyroantimonate ■in 85■2S (NF32) mL of . Use low-actinic glassware.]
■hot
■2S (NF32) water. Cool■2S (NF32) quickly, and add
.
■ . Solution A: 0.1 mg/mL of 2,7-dihydroxynaphthalene in
10 mL of a solution of potassium hydroxide (3 in 20). sulfuric acid; allow to stand until decolorized, and use
Allow to stand for 24 h, ■■2S (NF32) filter, ■and dilute
. . within 2 days.
with water to 100 mL.■2S (NF32) Standard solution: Transfer 310 mg of glycolic acid,
Analysis: To a 2-mL portion of the Sample solution pre- previously dried over phosphorus pentoxide in a desic-
pared for the test for Limit of Iron, ■add 2mL of 15% . cator at room temperature overnight, to a 500-mL vol-
potassium carbonate, and heat to boiling. No precipi- umetric flask. ■■2S (NF32) Dissolve in and dilute with
.

tate is formed. Add■2S (NF32) 4 mL of Potassium pyroan- water to volume. Transfer 5.0 mL of this solution to a
timonate solution, ■and heat to boiling. Allow to cool in
. 100-mL beaker, add 4 mL of 6 N acetic acid, and allow
ice water and, if■2S (NF32) necessary, rub the inside of the to stand for about 30 min. Add 50 mL of acetone and
test tube with a glass rod. 1 g of sodium chloride, mix, and pass through fast fil-
Acceptance criteria: A ■dense■2S (NF32) precipitate is
. ter paper moistened with acetone into a 100-mL volu-
formed. metric flask. Rinse the beaker and the filter paper with
acetone. Combine the filtrate and washings, dilute
with acetone to volume, and mix. Allow to stand for
Change to read: 24 h without shaking. Use the clear supernatant as the
Standard solution.
• ■◆
.

■2S (NF32)D. Sodium Starch Glycolate imparts an intense

.

Sample solution: Transfer 200 mg to a 100-mL beaker.

yellow color to a nonluminous flame.■◆■2S (NF32) .

Add 4 mL of 6 N acetic acid and 5 mL of water. Stir

ASSAY until dissolution is complete (about 10 min). Add
• PROCEDURE 50 mL of acetone and 1 g of sodium chloride, ■mix,
.

■2S (NF32) and pass through fast filter paper moistened

Sample: 1 g
Analysis: Transfer the Sample to a conical flask, add with acetone into a 100-mL volumetric flask. Rinse the
20 mL of 80% alcohol, stir for 10 min, and filter. Re- beaker and filter paper with acetone. Combine the fil-
peat the extraction until the chloride has been com- trate and washings, ■■2S (NF32) dilute with acetone to
.

2014 The United States Pharmacopeial Convention All Rights Reserved.

 Stage 6 Harmonization
2 Sodium Official December 1, 2014

volume, ■and mix.■2S (NF32) Allow to stand for 24 h

. suitable beaker, add 2 mL of citric acid solution (1 in 5)
without shaking. Use the clear supernatant as the Sam- and 0.1 mL of thioglycolic acid, and mix. Render the
ple solution. solution alkaline, using litmus paper as an external indi-
Analysis: Treat the Sample solution and the Standard cator, by the addition of ammonium hydroxide. Dilute
solution as follows. Heat 2.0 mL of the solution on a with water to 20 mL, and mix. Allow the solutions to
water bath for 20 min to remove the acetone. Cool to stand for 5 min.
room temperature. Add 20.0 mL of Solution A to the Acceptance criteria: The color of the solution from the
solution under test, mix, and heat on a water bath for Sample solution is a shade of pink no deeper than that
20 min. Cool under running water, and quantitatively of the solution from the Standard solution (0.002%).
transfer to a 25-mL volumetric flask. Maintain the flask
under running water, and dilute with sulfuric acid to SPECIFIC TESTS
volume. Within 10 min, determine the absorbance of • MICROBIAL ENUMERATION TESTS 〈61〉 and TESTS FOR SPECI-
the solution at 540 nm with a suitable spectrophotom- FIED MICROORGANISMS 〈62〉: It meets the requirements of
eter, using water as the blank. the tests for absence of Salmonella species and Escher-
Acceptance criteria: The absorbance of the Sample so- ichia coli.
lution is NMT that of the Standard solution (2.0%). • PH 〈791〉: Disperse 1 g in 30 mL of water. The pH of the
resulting suspension is either 5.5–7.5 for Type A or
IMPURITIES 3.0–5.0 for Type B.
• LOSS ON DRYING 〈731〉:
Analysis: Dry at 130° for 90 min.
Change to read: Acceptance criteria: NMT 10.0%
• ■◆
. .

■2S (NF32) HEAVY METALS, Method II 〈231〉: 20 ppm■ .

ADDITIONAL REQUIREMENTS
◆■2S (NF32)
• LIMIT OF IRON
Standard solution: Dissolve 863.4 mg of ferric ammo- Change to read:
nium sulfate [FeNH4(SO4)2 · 12H2O] in water, add
25 mL of 2 N sulfuric acid, dilute with water to • ■◆
.

■2S (NF32)PACKAGING AND STORAGE: Preserve in well-

.

500.0 mL, and mix. Pipet 10 mL of this solution into a closed containers, preferably protected from wide varia-
100-mL volumetric flask, dilute with water to volume, tions in temperature and humidity, which may cause cak-
and mix. Pipet 5 mL of this solution into a 100-mL ing.■◆■2S (NF32)
.

volumetric flask, dilute with water to volume, and mix.

This solution contains the equivalent of 1.0 µg/mL of Change to read:
iron.
Sample solution: Place 2.5 g in a silica or platinum • ■2S (NF32)LABELING: Label it to indicate the botanical
■◆
crucible, and add 2 mL of 10 N sulfuric acid. Heat on a
. .

source of the starch from which it was derived, the cross-

water bath, then cautiously raise the temperature pro- linking agent (if used), the pH range, and whether it is
gressively over an open flame. Ignite, preferably in a Type A or Type B.■◆■2S (NF32)
muffle furnace, at 600 ± 25°. Continue heating until all
.

• USP REFERENCE STANDARDS 〈11〉

black particles have disappeared. Cool, add a few USP Sodium Starch Glycolate Type A RS
drops of 2 N sulfuric acid, and heat and ignite as USP Sodium Starch Glycolate Type B RS
above. Add a few drops of 2 M ammonium carbonate,
evaporate to dryness, and ignite as above. Cool, dis-
solve the residue in 50 mL of water, and mix.
[NOTE—Reserve a portion of this solution for Identifica-
tion test C.]
Analysis: Treat the Sample solution and the Standard
solution as follows. Transfer 10 mL of the solution to a

2014 The United States Pharmacopeial Convention All Rights Reserved.