Accessed from 10.6.1.
1 by merck1 on Mon May 11 20:57:04 EDT 2015
USP 38
Acetohexamide Tablets
.
» 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-
ers.
USP Reference standards 〈11〉—
USP Acetohexamide RS
Identification—Evaporate on a steam bath to dryness a
20-mL portion of the diluted chloroform solution prepared
as directed in the Assay: the residue meets the requirements
of Identification test A under Acetohexamide.
Dissolution 〈711〉—
Medium: pH 7.6 phosphate buffer (see pH 〈791〉);
900 mL.
Apparatus 1: 100 rpm.
Time: 60 minutes.
Procedure—Determine the amount of C15H20N2O4S dis-
solved from UV absorbances at the wavelength of maximum
absorbance at about 245 nm of filtered portions of the solu-
tion under test, suitably diluted with Medium, if necessary,
using Medium as the blank, in comparison with a Standard
solution having a known concentration of USP Acetohex-
amide RS in the same Medium.
Tolerances—Not less than 75% (Q) of the labeled amount
of C15H20N2O4S is dissolved in 60 minutes.
Uniformity of dosage units 〈905〉: meet the require-
ments.
Assay—Weigh and finely powder not fewer than 20 Tablets.
Transfer an accurately weighed portion of the powder,
equivalent to about 500 mg of acetohexamide, to a 100-mL
volumetric flask, add 60 mL of 0.1 N sodium hydroxide, and
shake for 30 minutes. Dilute with water to volume, mix, and
filter, discarding the first 20 mL of the filtrate. Transfer
20.0 mL of the subsequent filtrate to a 125-mL separator,
add 2 mL of 3 N hydrochloric acid, and extract with four
40-mL portions of chloroform, filtering each portion
through chloroform-washed paper into a 200-mL volumetric
flask. Dilute with chloroform to volume, and mix. Transfer
20.0 mL of this solution to a suitable beaker, and evaporate
on a steam bath to dryness. Transfer the residue, with the
aid of 0.1 N sodium hydroxide, to a 100-mL volumetric
flask, add 0.1 N sodium hydroxide to volume, and mix.
Transfer 10.0 mL of this solution to a third 100-mL volumet-
ric flask, dilute with water to volume, and mix. Concomi-
tantly determine the absorbances of the solution from the
Tablets and a Standard solution prepared from USP
Acetohexamide RS, in the same medium, at a concentration
of about 10 µg per mL, in 1-cm cells, at the wavelength of
maximum absorbance at about 247 nm, with a suitable
spectrophotometer, using 0.01 N sodium hydroxide as the
blank. Calculate the quantity, in mg, of C15H20N2O4S in the
portion of Tablets taken by the formula:
50C(AU / AS)
in which C is the concentration, in µg per mL, of USP
Acetohexamide RS in the Standard solution; and AU and AS
are the absorbances of the solution from the Tablets and the
Standard solution, respectively.
Official from May 1, 2015
Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.
Official Monographs / Acetohydroxamic 2045
Acetohydroxamic Acid
C2H5NO2 75.07
N-Acetyl hydroxyacetamide;
Acetohydroxamic acid [546-88-3].
DEFINITION
Acetohydroxamic Acid, dried over phosphorus pentoxide for
16 h, contains NLT 98.0% and NMT 101.0% of acetohy-
droxamic acid (C2H5NO2).
IDENTIFICATION
• A. INFRARED ABSORPTION 〈197K〉
• B.
Sample solution: 20 mg/mL in water
Analysis: To 10 mL of the Sample solution add 2 drops
of potassium permanganate TS.
Acceptance criteria: The pink color of the permanga-
nate disappears.
ASSAY
• PROCEDURE
Ferric chloride solution: 20 mg/mL of ferric chloride in
0.1 N hydrochloric acid
Standard solution: 500 µg/mL of USP Acetohydroxa-
mic Acid RS in 0.1 N hydrochloric acid
Sample solution: 500 µg/mL of Acetohydroxamic Acid,
previously dried, in 0.1 N hydrochloric acid
Blank: 0.1 N hydrochloric acid
Analysis
Samples: Standard solutions, Sample solution, and Blank
Transfer 10.0 mL each of the Standard solution, Sample
USP Monographs
solution, and Blank to separate 100-mL volumetric
flasks. To each flask add 50 mL of 0.1 N hydrochloric
acid and 10.0 mL of Ferric chloride solution, and dilute
with 0.1 N hydrochloric acid to volume. Without de-
lay, concomitantly determine the absorbances of the
solutions at the wavelength of maximum absorbance
at about 502 nm using the Blank to set the
instrument.
Calculate the percentage of acetohydroxamic acid
(C2H5NO2) in the portion of Acetohydroxamic Acid
taken:
Result = (AU/AS) × (CS/CU) × 100
AU = absorbance of the Sample solution
AS = absorbance of the Standard solution
CS = concentration of USP Acetohydroxamic Acid
RS in the Standard solution (µg/mL)
CU = concentration of Acetohydroxamic Acid in the
Sample solution (µg/mL)
Acceptance criteria: 98.0%–101.0% on the previously
dried basis
IMPURITIES
• RESIDUE ON IGNITION 〈281〉: NMT 0.1%
Delete the following:
•• 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