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2044 Acetic / Official Monographs USP 38

40 mL of water, and 3 drops of phenolphthalein TS. Ti-

trate with 0.1 N sodium hydroxide VS to a faint pink
.

Acetic Acid Irrigation endpoint. Each mL of 0.1 N sodium hydroxide is equiv-

alent to 6.005 mg of acetic acid (C2H4O2).
DEFINITION Acceptance criteria: 85.0%–130.0%
Acetic Acid Irrigation is a sterile solution of Glacial Acetic
Acid in Water for Injection. It contains, in each 100 mL, SPECIFIC TESTS
NLT 237.5 mg and NMT 262.5 mg of C2H4O2. • PH 〈791〉
Sample solution: Acetic Acid Otic Solution and water
IDENTIFICATION (1:1)
• A. IDENTIFICATION TESTS—GENERAL, Acetate 〈191〉 Acceptance criteria: 2.0–4.0
Sample: 100 mL of Acetic Acid Irrigation
Analysis: Evaporate the Sample to about 10 mL. ADDITIONAL REQUIREMENTS
Acceptance criteria: The resulting solution meets the • PACKAGING AND STORAGE: Preserve in tight containers,
requirements. and store at controlled room temperature.
ASSAY
• PROCEDURE
Sample: 50 mL of Acetic Acid Irrigation
Analysis: Pipet the Sample into a 150-mL conical flask,
Acetohexamide
.

add 2 drops of phenolphthalein TS, and titrate with 0.1

N sodium hydroxide VS. Each mL of 0.1 N sodium hy-
droxide is equivalent to 6.005 mg of acetic acid
(C2H4O2).
Acceptance criteria: 237.5–262.5 mg of C2H4O2 in
each 100 mL of Acetic Acid Irrigation
SPECIFIC TESTS
• PH 〈791〉: 2.8–3.4 C15H20N2O4S 324.40
• BACTERIAL ENDOTOXINS TEST 〈85〉: It contains NMT 0.5 Benzenesulfonamide, 4-acetyl-N-[[cyclohexylamino]-
USP Endotoxin Unit/mL. carbonyl]-.
• OTHER REQUIREMENTS: It meets the requirements under 1-[(p-Acetylphenyl)sulfonyl]-3-cyclohexylurea [968-81-0].
Injections 〈1〉, except that the container in which it is
packaged may be designed to empty rapidly and may » Acetohexamide contains not less than 97.0 per-
exceed 1000 mL in capacity. cent and not more than 101.0 percent of
ADDITIONAL REQUIREMENTS C15H20N2O4S, calculated on the dried basis.
• PACKAGING AND STORAGE: Preserve in single-dose contain-
ers, preferably of Type I or Type II glass, and store at Packaging and storage—Preserve in well-closed contain-
USP Monographs

controlled room temperature. It may be packaged in suit- ers.

able plastic containers. USP Reference standards 〈11〉—
• USP REFERENCE STANDARDS 〈11〉 USP Acetohexamide RS
USP Endotoxin RS Identification—
A: Infrared Absorption 〈197K〉.
B: Ultraviolet Absorption 〈197U〉—
. Solution: 10 µg per mL.
Acetic Acid Otic Solution Medium: 0.01 N sodium hydroxide.
Absorptivities at 247 nm, calculated on the dried basis, do
DEFINITION not differ by more than 3.0%.
Acetic Acid Otic Solution is a solution of Glacial Acetic Acid Melting range 〈741〉: between 182.5° and 187°.
in a suitable nonaqueous solvent. It contains NLT 85.0% Loss on drying 〈731〉—Dry it at 105° for 3 hours: it loses
and NMT 130.0% of the labeled amount of C2H4O2. not more than 1.0% of its weight.
IDENTIFICATION Residue on ignition 〈281〉: not more than 0.1%.
• A. Selenium 〈291〉: 0.003%, a 200-mg specimen mixed
Sample solution: Dilute 5 mL of Acetic Acid Otic Solu- with 200 mg of magnesium oxide being used.
tion with 10 mL of water.
Analysis: Adjust the Sample solution with 1 N sodium
hydroxide to a pH of 7. Add ferric chloride TS. Delete the following:
Acceptance criteria: A deep red color is produced, and
it is destroyed by the addition of hydrochloric acid. •Heavy metals, Method II 〈231〉:
. 0.002%.• (Official 1-Dec-2015)
• B. Assay—Dissolve about 300 mg of Acetohexamide, accu-
Analysis: Warm it with sulfuric acid and alcohol. rately weighed, in 40 mL of dimethylformamide, add
Acceptance criteria: Ethyl acetate, recognizable by its 5 drops of thymol blue TS, and titrate, using a magnetic
characteristic odor, is evolved. stirrer, with 0.1 N sodium methoxide VS to a blue endpoint.
Perform a blank determination, and make any necessary
ASSAY correction. Each mL of 0.1 N sodium methoxide is equiva-
• PROCEDURE lent to 32.44 mg of C15H20N2O4S.
Sample: A quantity of Acetic Acid Otic Solution con-
taining 100 mg of glacial acetic acid
Analysis: Transfer the Sample to a 250-mL conical flask,
and add 5 mL of saturated sodium chloride solution,

Official from May 1, 2015

Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.
Accessed from 10.6.1.1 by merck1 on Mon May 11 20:56:46 EDT 2015

USP 38 Official Monographs / Acetohydroxamic 2045

Acetohexamide Tablets Acetohydroxamic Acid

.

» Acetohexamide Tablets contain not less than

93.0 percent and not more than 107.0 percent of
the labeled amount of C15H20N2O4S.
Packaging and storage—Preserve in well-closed contain- C2H5NO2 75.07
ers. N-Acetyl hydroxyacetamide;
USP Reference standards 〈11〉— Acetohydroxamic acid [546-88-3].
USP Acetohexamide RS DEFINITION
Identification—Evaporate on a steam bath to dryness a Acetohydroxamic Acid, dried over phosphorus pentoxide for
20-mL portion of the diluted chloroform solution prepared 16 h, contains NLT 98.0% and NMT 101.0% of acetohy-
as directed in the Assay: the residue meets the requirements droxamic acid (C2H5NO2).
of Identification test A under Acetohexamide.
Dissolution 〈711〉— IDENTIFICATION
Medium: pH 7.6 phosphate buffer (see pH 〈791〉); • A. INFRARED ABSORPTION 〈197K〉
900 mL. • B.
Sample solution: 20 mg/mL in water
Apparatus 1: 100 rpm. Analysis: To 10 mL of the Sample solution add 2 drops
Time: 60 minutes. of potassium permanganate TS.
Procedure—Determine the amount of C15H20N2O4S dis- Acceptance criteria: The pink color of the permanga-
solved from UV absorbances at the wavelength of maximum nate disappears.
absorbance at about 245 nm of filtered portions of the solu-
tion under test, suitably diluted with Medium, if necessary, ASSAY
using Medium as the blank, in comparison with a Standard • PROCEDURE
solution having a known concentration of USP Acetohex- Ferric chloride solution: 20 mg/mL of ferric chloride in
amide RS in the same Medium. 0.1 N hydrochloric acid
Standard solution: 500 µg/mL of USP Acetohydroxa-
Tolerances—Not less than 75% (Q) of the labeled amount mic Acid RS in 0.1 N hydrochloric acid
of C15H20N2O4S is dissolved in 60 minutes. Sample solution: 500 µg/mL of Acetohydroxamic Acid,
Uniformity of dosage units 〈905〉: meet the require- previously dried, in 0.1 N hydrochloric acid
ments. Blank: 0.1 N hydrochloric acid
Assay—Weigh and finely powder not fewer than 20 Tablets. Analysis
Transfer an accurately weighed portion of the powder, Samples: Standard solutions, Sample solution, and Blank
equivalent to about 500 mg of acetohexamide, to a 100-mL Transfer 10.0 mL each of the Standard solution, Sample

USP Monographs
volumetric flask, add 60 mL of 0.1 N sodium hydroxide, and solution, and Blank to separate 100-mL volumetric
shake for 30 minutes. Dilute with water to volume, mix, and flasks. To each flask add 50 mL of 0.1 N hydrochloric
filter, discarding the first 20 mL of the filtrate. Transfer acid and 10.0 mL of Ferric chloride solution, and dilute
20.0 mL of the subsequent filtrate to a 125-mL separator, with 0.1 N hydrochloric acid to volume. Without de-
add 2 mL of 3 N hydrochloric acid, and extract with four lay, concomitantly determine the absorbances of the
40-mL portions of chloroform, filtering each portion solutions at the wavelength of maximum absorbance
through chloroform-washed paper into a 200-mL volumetric at about 502 nm using the Blank to set the
flask. Dilute with chloroform to volume, and mix. Transfer instrument.
20.0 mL of this solution to a suitable beaker, and evaporate Calculate the percentage of acetohydroxamic acid
on a steam bath to dryness. Transfer the residue, with the (C2H5NO2) in the portion of Acetohydroxamic Acid
aid of 0.1 N sodium hydroxide, to a 100-mL volumetric taken:
flask, add 0.1 N sodium hydroxide to volume, and mix.
Transfer 10.0 mL of this solution to a third 100-mL volumet- Result = (AU/AS) × (CS/CU) × 100
ric flask, dilute with water to volume, and mix. Concomi-
tantly determine the absorbances of the solution from the AU = absorbance of the Sample solution
Tablets and a Standard solution prepared from USP AS = absorbance of the Standard solution
Acetohexamide RS, in the same medium, at a concentration CS = concentration of USP Acetohydroxamic Acid
of about 10 µg per mL, in 1-cm cells, at the wavelength of RS in the Standard solution (µg/mL)
maximum absorbance at about 247 nm, with a suitable CU = concentration of Acetohydroxamic Acid in the
spectrophotometer, using 0.01 N sodium hydroxide as the Sample solution (µg/mL)
blank. Calculate the quantity, in mg, of C15H20N2O4S in the Acceptance criteria: 98.0%–101.0% on the previously
portion of Tablets taken by the formula: dried basis

50C(AU / AS) IMPURITIES

• RESIDUE ON IGNITION 〈281〉: NMT 0.1%
in which C is the concentration, in µg per mL, of USP
Acetohexamide RS in the Standard solution; and AU and AS Delete the following:
are the absorbances of the solution from the Tablets and the
Standard solution, respectively. •• HEAVY METALS, Method I 〈231〉
.

Sample solution: Dissolve 1 g in 23 mL of water, and

add 2 mL of 1 N acetic acid.
Acceptance criteria: NMT 20 ppm• (Official 1-Dec-2015)
• LIMIT OF HYDROXYLAMINE
Buffer: 1.36 g/L of monobasic potassium phosphate in
water, adjusted with 1 M potassium hydroxide to a pH
of 7.4

Official from May 1, 2015

Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.