Accessed from 10.6.1.
1 by merck1 on Mon May 11 21:22:17 EDT 2015
USP 38
nol related compound B and allopurinol related compound
C is not less than 1.1, and that between allopurinol related
compound C and allopurinol is not less than 6.0. [NOTE—For
the purpose of identification, the relative retention times are
about 0.7 for allopurinol related compound B, 0.8 for al-
lopurinol related compound C, and 1.0 for allopurinol.]
Chromatograph the Standard preparation, and record the
peak responses as directed for Procedure: the relative stan-
dard deviation for replicate injections is not more than
2.0%.
Procedure—Separately inject equal volumes (about 20 µL)
of the Standard preparation and the Assay preparation into
the chromatograph, record the chromatograms, and meas-
ure the responses for the major peaks. Calculate the per-
centage of C5H4N4O in the portion of Allopurinol taken by
the formula:
100(CS / CU)(rU / rS)
in which CU and CS are the concentrations, in mg per mL, of
allopurinol in the Assay preparation and the Standard prepa-
ration, respectively; and rU and rS are the peak responses
obtained from the Assay preparation and the Standard prepa-
ration, respectively.
.
Allopurinol Oral Suspension
DEFINITION
Allopurinol Oral Suspension contains NLT 90.0% and NMT
110.0% of the labeled amount of allopurinol (C5H4N4O).
Prepare Allopurinol Oral Suspension 20 mg/mL as follows
(see Pharmaceutical Compounding—Nonsterile Preparations
〈795〉).
Allopurinol 2g
Glycerin 5 mL
Vehicle for Oral Suspension, NF 45 mL
Vehicle for Oral Solution, NF, a sufficient
quantity to make 100 mL
Select the number of tablets that contain the specified
amount of allopurinol, and calculate the quantity of each
ingredient required for the total amount to be prepared.
Count, weigh, or measure each ingredient. Thoroughly
pulverize the tablets. Mix the powdered Allopurinol tablets
and Glycerin to form a smooth paste. Incorporate the Ve-
hicle for Oral Suspension. Add sufficient Vehicle for Oral So-
lution to volume, and mix well. Adjust the pH, if neces-
sary. Package and label.
SPECIFIC TESTS
• PH 〈791〉: 6.5–7.5
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Package in a tight container,
and store at controlled room temperature.
• LABELING: Label it to state that it is to be shaken well
before use, and that it is to be discarded after 60 days.
Label it to state that it is to be kept out of the reach of
children. Label it to indicate the nominal content of al-
lopurinol in the Oral Suspension.
• BEYOND-USE DATE: NMT 60 days after the date on which
it was compounded
Official from May 1, 2015
Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.
Official Monographs / Allopurinol 2095
Allopurinol Tablets
.
» Allopurinol Tablets contain not less than
93.0 percent and not more than 107.0 percent of
the labeled amount of allopurinol (C5H4N4O).
Packaging and storage—Preserve in well-closed contain-
ers.
USP Reference standards 〈11〉—
USP Allopurinol RS
Identification—Extract a quantity of finely powdered Tab-
lets, equivalent to about 50 mg of allopurinol, by trituration
with 10 mL of 0.1 N sodium hydroxide. Filter, acidify the
filtrate with 1 N acetic acid, collect the precipitated allopuri-
nol (allow 10 to 15 minutes for sufficient precipitation to
occur), wash the precipitate with 3 mL of dehydrated alco-
hol, in portions, and finally wash with 4 mL of anhydrous
ethyl ether. Allow to dry in air for 15 minutes, then dry at
105° for 3 hours: the residue so obtained meets the require-
ments for the Identification test under Allopurinol.
Dissolution 〈711〉—
Medium: 0.01 N hydrochloric acid; 900 mL.
Apparatus 2: 75 rpm.
Time: 45 minutes.
Standard stock solution—Prepare a stock solution by trans-
ferring about 40 mg of USP Allopurinol RS, accurately
weighed, to a 200-mL volumetric flask. Add 10 mL of 0.1 N
sodium hydroxide, sonicate for about 2 minutes, shake by
mechanical means for about 10 minutes, dilute with Dissolu-
tion Medium to volume, and mix.
Standard solution—Dilute the Standard stock solution with
Dissolution Medium to obtain a solution having a concentra-
tion similar to that expected in the solution under test.
USP Monographs
Procedure—Determine the amount of C5H4N4O dissolved
by employing UV absorption at the wavelength of maxi-
mum absorbance at about 250 nm on filtered portions of
the solution under test, suitably diluted with Dissolution Me-
dium, in comparison with the Standard solution.
Tolerances—Not less than 75% (Q) of the labeled amount
of C5H4N4O is dissolved in 45 minutes.
Uniformity of dosage units 〈905〉: meet the require-
ments.
Assay—[NOTE—Do not allow the Mobile phase to remain in
the column overnight. After performing the procedure, flush
the system with water for not less than 20 minutes, and
then flush with methanol for 20 minutes.]
Mobile phase—Prepare a filtered and degassed 0.05 M
solution of monobasic ammonium phosphate.
Internal standard solution—On the day of use, dissolve
about 50 mg of hypoxanthine in 10 mL of 0.1 N sodium
hydroxide, shake by mechanical means until dissolved
(about 10 minutes), dilute with water to 50 mL, and mix.
Standard preparation—On the day of use, transfer about
50 mg of USP Allopurinol RS, accurately weighed, to a
50-mL volumetric flask, add 10 mL of 0.1 N sodium hydrox-
ide, shake by mechanical means for 10 minutes, dilute with
water to volume, and mix. Transfer 4.0 mL of this solution
and 2.0 mL of Internal standard solution to a 200-mL volu-
metric flask, dilute with Mobile phase to volume, and mix.
Assay preparation—Weigh and finely powder not fewer
than 20 Tablets. Transfer an accurately weighed portion of
the powder, equivalent to about 50 mg of allopurinol, to a
50-mL volumetric flask, add 10 mL of 0.1 N sodium hydrox-
ide, shake by mechanical means for 10 minutes, add water
to volume, and mix. [NOTE—From this point, conduct the
remainder of the Assay without delay.] Filter, rejecting the
first 10 mL of the filtrate. Transfer 4.0 mL of the filtrate and
2.0 mL of Internal standard solution to a 200-mL volumetric
flask, dilute with Mobile phase to volume, and mix.
 Accessed from 10.6.1.1 by merck1 on Mon May 11 21:22:17 EDT 2015
2096 Allopurinol / Official Monographs
Chromatographic system (see Chromatography 〈621〉)—The
liquid chromatograph is equipped with a 254-nm detector
and a 4-mm × 30-cm column that contains packing L1. The
flow rate is about 1.5 mL per minute. Chromatograph the
Standard preparation, and record the peak responses as di-
rected for Procedure: the relative retention times are about
0.6 for hypoxanthine and 1.0 for allopurinol; the resolution,
R, between the analyte and internal standard is not less than
5; and the relative standard deviation for replicate injections
is not more than 3.0%.
Procedure—Separately inject equal volumes (about 15 µL)
of the Standard preparation and the Assay preparation into
the chromatograph, record the chromatograms, and meas-
ure the responses for the major peaks. Calculate the quan-
tity, in mg, of allopurinol (C5H4N4O) in the portion of Tab-
lets taken by the formula:
2.5C(RU / RS)
in which C is the concentration, in µg per mL, of USP Al-
lopurinol RS in the Standard preparation; and RU and RS are
the peak response ratios of allopurinol to hypoxanthine ob-
tained from the Assay preparation and the Standard prepara-
tion, respectively.
.
Allyl Isothiocyanate
C4H5NS 99.15
3-Isothiocyanato-1-propene;
Isothiocyanic acid allyl ester [57-06-7].
USP Monographs
DEFINITION
Allyl Isothiocyanate contains NLT 93.0% and NMT 105.0%
of allyl isothiocyanate (C4H5NS).
[CAUTION—Allyl Isothiocyanate is a potent lachrymator, with
a pungent, irritating odor. Care should be taken to pro-
tect the eyes, to prevent inhalation of fumes, and to avoid
tasting.]
IDENTIFICATION
• A. INFRARED ABSORPTION 〈197F〉: The spectrum exhibits
pronounced peaks at about 700, 950, 980, 1300, 1340,
1350, 1410, 1420, 1650, 2100, and 2200 cm−1. .
ASSAY
• PROCEDURE
Sample solution: Transfer 4 mL into a 100-mL volumet-
ric flask, and dilute with alcohol to volume.
Analysis: Transfer 5.0 mL of the Sample solution to a
100-mL conical flask, and add 50.0 mL of 0.1 N silver
nitrate VS and 5 mL of ammonia TS. Connect the flask
to a reflux condenser, heat on a water bath for 1 h,
and allow to cool to room temperature. Disconnect the
flask from the condenser, transfer the contents of the
conical flask to a 100-mL volumetric flask with the aid
of water, and dilute with water to volume. Pass through
a dry filter, discarding the first 10 mL of the filtrate. To
50.0 mL of the subsequent filtrate add 5 mL of nitric
acid and 2 mL of ferric ammonium sulfate TS, and ti-
trate the excess silver nitrate with 0.1 N ammonium
thiocyanate VS. Perform a blank determination, using
5 mL of alcohol in place of the Sample solution, and
make any necessary correction. Each mL of 0.1 N silver
nitrate is equivalent to 4.958 mg of allyl isothiocyanate
(C4H5NS).
Official from May 1, 2015
Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.
USP 38
Acceptance criteria: 93.0%–105.0%
IMPURITIES
• LIMIT OF PHENOLS
Sample solution: Dilute a 1-mL sample with 5 mL of
alcohol.
Analysis: Add 1 drop of ferric chloride TS to the Sample
solution.
Acceptance criteria: A blue color is not produced
immediately.
SPECIFIC TESTS
• SPECIFIC GRAVITY 〈841〉: 1.013–1.020
• REFRACTIVE INDEX 〈831〉: 1.527–1.531, determined at 20°
• DISTILLING RANGE, Method I 〈721〉: 148°–154°
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers.
.
Aloe
DEFINITION
Aloe is the dried latex of the leaves of Aloe vera (L.) Burm. f.
(syn. Aloe barbadensis Mill.), known in commerce as aloe
vera, Curaçao aloe, or Barbados aloe; or of Aloe ferox
Mill., or of hybrids of Aloe ferox Mill. with Aloe africana
Mill. and Aloe spicata L.f., known in commerce as cape
aloe (Fam. Liliaceae). Aloe vera contains NLT 16.0% of
aloin, and cape aloe and its hybrids contain NLT 6.0% of
aloin, both calculated on the dried basis.
IDENTIFICATION
• A.
Sample: 1 g finely powdered
Analysis: Mix the Sample with 25 mL of cold water.
Shake the mixture occasionally during 2 h, filter, and
wash the filter and residue with sufficient cold water to
make the filtrate measure 100 mL.
Acceptance criteria: The color of the filtrate, viewed in
the bulb of a 100-mL volumetric flask, is dark orange
with curaçao aloe and greenish yellow with cape aloe.
The filtrate darkens on standing. [NOTE—Reserve the fil-
trate for Identification test B.]
• B.
Sample: 5 mL of the filtrate obtained in Identification
test A
Analysis: Add 2 mL of nitric acid to the Sample, and
mix.
Acceptance criteria: The mixture exhibits a reddish-or-
ange color with aloe vera and a reddish-brown color
that changes rapidly to green with cape aloe.
• C. THIN-LAYER CHROMATOGRAPHY
Standard solution: 1.0 mg/mL of USP Aloin RS in
methanol
Sample solution: 0.5 g of finely powdered Aloe in
10 mL of methanol, sonicate for 15 min, centrifuge or
filter, and use the supernatant or the filtrate.
Chromatographic system
(See Chromatography 〈621〉, Thin-Layer Chromato-
graphy.)
Adsorbent: Chromatographic silica gel mixture with
an average particle size of 5 µm (HPTLC plates)
Application volume: 2 µL of the Standard solution and
5 µL of the Sample solution as 8-mm bands
Relative humidity: Condition the plate to a relative
humidity of about 33% using a suitable device.
Developing solvent system: Ethyl acetate, methanol,
and water (100:17:13)
Developing distance: 6 cm
Derivatization reagent: 10% solution of potassium
hydroxide in methanol (prepare in an ice bath)