Accessed from 10.6.1.
1 by merck1 on Mon May 11 20:56:46 EDT 2015
2044 Acetic / Official Monographs
.
Acetic Acid Irrigation
DEFINITION
Acetic Acid Irrigation is a sterile solution of Glacial Acetic
Acid in Water for Injection. It contains, in each 100 mL,
NLT 237.5 mg and NMT 262.5 mg of C2H4O2.
IDENTIFICATION
• A. IDENTIFICATION TESTS—GENERAL, Acetate 〈191〉
Sample: 100 mL of Acetic Acid Irrigation
Analysis: Evaporate the Sample to about 10 mL.
Acceptance criteria: The resulting solution meets the
requirements.
ASSAY
• PROCEDURE
Sample: 50 mL of Acetic Acid Irrigation
Analysis: Pipet the Sample into a 150-mL conical flask,
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
• BACTERIAL ENDOTOXINS TEST 〈85〉: It contains NMT 0.5
USP Endotoxin Unit/mL.
• OTHER REQUIREMENTS: It meets the requirements under
Injections 〈1〉, except that the container in which it is
packaged may be designed to empty rapidly and may
exceed 1000 mL in capacity.
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in single-dose contain-
ers, preferably of Type I or Type II glass, and store at
USP Monographs
controlled room temperature. It may be packaged in suit-
able plastic containers.
• USP REFERENCE STANDARDS 〈11〉
USP Endotoxin RS
. Solution: 10 µg per mL.
Acetic Acid Otic Solution
DEFINITION
Acetic Acid Otic Solution is a solution of Glacial Acetic Acid
in a suitable nonaqueous solvent. It contains NLT 85.0%
and NMT 130.0% of the labeled amount of C2H4O2.
IDENTIFICATION
• A.
Sample solution: Dilute 5 mL of Acetic Acid Otic Solu-
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.
Acceptance criteria: A deep red color is produced, and
it is destroyed by the addition of hydrochloric acid.
• B.
Analysis: Warm it with sulfuric acid and alcohol.
Acceptance criteria: Ethyl acetate, recognizable by its
characteristic odor, is evolved.
ASSAY
• PROCEDURE
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.
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
endpoint. Each mL of 0.1 N sodium hydroxide is equiv-
alent to 6.005 mg of acetic acid (C2H4O2).
Acceptance criteria: 85.0%–130.0%
SPECIFIC TESTS
• PH 〈791〉
Sample solution: Acetic Acid Otic Solution and water
(1:1)
Acceptance criteria: 2.0–4.0
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers,
and store at controlled room temperature.
Acetohexamide
.
C15H20N2O4S 324.40
Benzenesulfonamide, 4-acetyl-N-[[cyclohexylamino]-
carbonyl]-.
1-[(p-Acetylphenyl)sulfonyl]-3-cyclohexylurea [968-81-0].
» Acetohexamide contains not less than 97.0 per-
cent and not more than 101.0 percent of
C15H20N2O4S, calculated on the dried basis.
Packaging and storage—Preserve in well-closed contain-
ers.
USP Reference standards 〈11〉—
USP Acetohexamide RS
Identification—
A: Infrared Absorption 〈197K〉.
B: Ultraviolet Absorption 〈197U〉—
Medium: 0.01 N sodium hydroxide.
Absorptivities at 247 nm, calculated on the dried basis, do
not differ by more than 3.0%.
Melting range 〈741〉: between 182.5° and 187°.
Loss on drying 〈731〉—Dry it at 105° for 3 hours: it loses
not more than 1.0% of its weight.
Residue on ignition 〈281〉: not more than 0.1%.
Selenium 〈291〉: 0.003%, a 200-mg specimen mixed
with 200 mg of magnesium oxide being used.
Delete the following:
•Heavy metals, Method II 〈231〉:
. 0.002%.• (Official 1-Dec-2015)
Assay—Dissolve about 300 mg of Acetohexamide, accu-
rately weighed, in 40 mL of dimethylformamide, add
5 drops of thymol blue TS, and titrate, using a magnetic
stirrer, with 0.1 N sodium methoxide VS to a blue endpoint.
Perform a blank determination, and make any necessary
correction. Each mL of 0.1 N sodium methoxide is equiva-
lent to 32.44 mg of C15H20N2O4S.
Accessed from 10.6.1.1 by merck1 on Mon May 11 20:56:46 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