Accessed from 190.212.245.
6 by ebsc0sa on Sun Jun 09 09:09:05 EDT 2013
USP 36
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%.
ProcedureSeparately inject equal volumes (about 15 L)
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 g 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].
Allyl Isothiocyanate contains not less than
93.0 percent and not more than 105.0 percent of
C4H5NS.
CautionAllyl Isothiocyanate is a potent lachcry-
mator, with a pungent irritating odor. Care should
be taken to protect the eyes, to prevent inhalation
of fumes, and to avoid tasting.
Packaging and storagePreserve in tight containers.
Identification, Infrared Absorption 197FThe spectrum
exhibits pronounced peaks at about 700cm, 950cm, 980cm,
1300cm, 1340cm, 1350cm, 1410cm, 1420cm, 1650cm,
2100cm, and 2200cm.
Specific gravity 841: between 1.013 and 1.020.
Refractive index 831: between 1.527 and 1.531, de-
termined at 20.
Distilling range, Method I 721: between 148 and
154.
Limit of phenolsDilute 1 mL of it with 5 mL of alcohol,
and add 1 drop of ferric chloride TS: a blue color is not
produced immediately.
AssayTransfer about 4 mL of Allyl Isothiocyanate, accu-
rately weighed, to a 100-mL volumetric flask, add alcohol to
volume, and mix. Transfer 5.0 mL of this stock solution to a
100-mL conical flask, add 50.0 mL of 0.1 N silver nitrate VS
and 5 mL of ammonia TS. Connect the flask to a reflux con-
denser, heat on a water bath for 1 hour, and allow to cool
to room temperature. Disconnect the flask from the con-
denser, transfer the contents of the conical flask to a
100-mL volumetric flask with the aid of water, dilute with
water to volume, and mix. Pass through a dry filter, discard-
ing the first 10 mL of the filtrate. To 50.0 mL of the subse-
Official from May 1, 2013
Copyright (c) 2013 The United States Pharmacopeial Convention. All rights reserved.
Official Monographs / Aloe 2373
quent filtrate add 5 mL of nitric acid and 2 mL of ferric am-
monium sulfate TS, and titrate the excess silver nitrate with
0.1 N ammonium thiocyanate VS. Perform a blank determi-
nation, using 5 mL of alcohol in place of the stock solution,
and make any necessary correction. Each mL of 0.1 N silver
nitrate is equivalent to 4.958 mg of C4H5NS.
Aloe
.
DEFINITION
Aloe is the dried latex of the leaves of Aloe barbadensis Mill.
(Aloe vera L.), known in commerce as Curacao Aloe, or of
Aloe ferox Mill. and hybrids of this species with Aloe afri-
cana Mill. and Aloe spicata Baker, known in commerce as
Cape Aloe (Fam. Liliaceae). Aloe yields NLT 50.0% of
water-soluble extractive.
IDENTIFICATION
A. Powdered Aloe dissolves in nitric acid with efferves-
cence, forming a reddish-brown to brown or green
solution.
B. PROCEDURE
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 Curacao Aloe, and greenish yellow with Cape
Aloe. The filtrate darkens on standing. [NOTEReserve
the filtrate for Identification tests C and D.]
C. PROCEDURE
Sample: 5 mL of the filtrate obtained in Identification
test B
Analysis: Add 2 mL of nitric acid to the Sample.
Acceptance criteria: The mixture exhibits a reddish-or-
ange color with Curacao Aloe, and a reddish-brown
color that changes rapidly to green with Cape Aloe.
D. PROCEDURE
Sample: 10 mL of the filtrate obtained in Identification
test B
Analysis: Mix the Sample with 2 mL of ammonium
hydroxide.
Acceptance criteria: The mixture exhibits an amber
color with Cape Aloe, and a dark amber color with Cu-
racao Aloe.
ASSAY
WATER-SOLUBLE EXTRACTIVE
Sample: 2 g of powdered Aloe
Analysis: Macerate the Sample in 70 mL of water in a
suitable flask. Shake the mixture during 8 h at 30-min
intervals, and allow it to stand for 16 h without shak-
ing. Filter, and wash the flask and residue with small
portions of water, passing the washings through the fil-
ter, until the filtrate measures 100.0 mL. Evaporate a
50-mL aliquot of the filtrate in a tared dish on a steam
bath to dryness, and dry at 110 to constant weight.
Acceptance criteria: The weight of water-soluble extrac-
tive so obtained is NLT 50% of the weight of Aloe
taken.
SPECIFIC TESTS
WATER DETERMINATION, Method III 921
Sample: Use a powdered sample. If the Aloe is not pow-
dered, crush it in a mortar until it passes through a no.
40 sieve, and mix the ground material before weighing
the sample.
 Accessed from 190.212.245.6 by ebsc0sa on Sun Jun 09 09:09:05 EDT 2013
2374 Aloe / Official Monographs
Analysis: Dry at 105 for 5 h
Acceptance criteria: NMT 12.0%
ARTICLES OF BOTANICAL ORIGIN, Total Ash 561
Acceptance criteria: NMT 4.0%
ALCOHOL-INSOLUBLE SUBSTANCES
Sample: 1 g of powdered Aloe
Analysis: Add the Sample to 50 mL of alcohol in a flask.
Heat the mixture to boiling, and maintain at incipient
boiling for 15 min, replacing any loss due to evapora-
tion. Remove from the heat, and shake the mixture at
intervals during 1 h. Pass through a small dried and
tared filter paper or a dried and tared filtering crucible,
and wash the residue on the filter with alcohol until the
last washing is colorless. Dry the residue at 105 to con-
stant weight.
Acceptance criteria: The weight of the residue does not
exceed 10.0% of the weight of Aloe taken.
BOTANIC CHARACTERISTICS
Curacao aloe: Brownish black, opaque masses. Its frac-
tured surface is uneven, waxy, and somewhat resinous.
Cape aloe: Dusky to dark brown irregular masses, the
surfaces of which are often covered with a yellowish
powder. Its fracture is smooth and glassy.
Powdered aloe: Yellow, yellowish brown to olive-brown
in color. When mounted in a bland expressed oil, it
appears as greenish-yellow to reddish-brown angular or
irregular fragments, the hues of which depend to some
extent upon the thickness of the fragments.
IMPURITIES
Alprazolam
.
C17H13ClN4 308.76
4H-[1,2,4]Triazolo[4,3-][1,4]benzodiazepine, 8-chloro-
1-methyl-6-phenyl-;
8-Chloro-1-methyl-6-phenyl-4H-s-triazolo[4,3-][1,4]
benzodiazepine [28981-97-7].
DEFINITION
Alprazolam contains NLT 98.0% and NMT 102.0% of
C17H13ClN4.
[CAUTIONCare should be taken to prevent inhaling parti-
cles of Alprazolam and exposing the skin to it.]
IDENTIFICATION
A. INFRARED ABSORPTION 197M
B. The retention time of the major peak from the Sample
solution corresponds to that from the Standard solution,
as obtained in the Assay.
ASSAY
PROCEDURE
Diluent: Acetonitrile and water (1:1)
Buffer: 1.4 g/L of monobasic potassium phosphate in
water
Mobile phase: Acetonitrile and Buffer (1:1)
Standard solution: 25 g/mL of USP Alprazolam RS in
Diluent. [NOTEThe solution is stable for 48 h at room
temperature when stored in closed containers.]
Sample solution: 25 g/mL of Alprazolam in Diluent.
Sonicate for about 1 min. [NOTEThe solution is stable
for 48 h at room temperature when stored in closed
containers.]
Official from May 1, 2013
Copyright (c) 2013 The United States Pharmacopeial Convention. All rights reserved.
USP 36
Chromatographic system
(See Chromatography 621, System Suitability.)
Mode: LC
Detector: UV 231 nm
Column: 4.6-mm 25-cm; packing L1
Column temperature: 40
Flow rate: 1 mL/min
Injection size: 20 L
System suitability
Sample: Standard solution
Suitability requirements
Tailing factor: NMT 2.0
Relative standard deviation: NMT 2.0%
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of alprazolam (C17H13ClN4) in
the portion of Alprazolam taken:
Result = (rU/rS) (CS/CU) 100
rU = peak area from the Sample solution
rS = peak area from the Standard solution
CS = concentration of USP Alprazolam RS in the
Standard solution (mg/mL)
CU = concentration of Alprazolam in the Sample
solution (mg/mL)
Acceptance criteria: 98.0%102.0%
RESIDUE ON IGNITION 281: NMT 0.5%
HEAVY METALS, Method II 231: 20 ppm
ORGANIC IMPURITIES
Diluent, Buffer, Mobile phase, and Chromatographic
system: Proceed as directed in the Assay.
System suitability solution: 20 g/mL each of USP Al-
prazolam RS, USP Alprazolam Related Compound A RS,
and USP 2-Amino-5-chlorobenzophenone RS in Diluent
Standard solution: 0.25 g/mL of USP Alprazolam RS in
Diluent. [NOTEWhen stored in closed containers, the
solution is stable for 48 h at room temperature.]
Sample solution: 250 g/mL of Alprazolam in Diluent.
Sonicate for about 1 min. [NOTEWhen stored in
closed containers, the Sample solution is stable for 24 h
at room temperature.]
System suitability
Samples: Standard solution and System suitability
solution
[NOTEFor relative retention times, see Table 1.]
Suitability requirements
Resolution: NLT 2.0 between alprazolam related com-
pound A and alprazolam, System suitability solution
Relative standard deviation: NMT 5.0%, Standard
solution
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of each impurity in the portion
of Alprazolam taken:
Result = (rU/rS) (CS/CU) (1/F) 100
rU = peak response for each impurity in the Sample
solution
rS = peak response for alprazolam from the
Standard solution
CS = concentration of USP Alprazolam RS in the
Standard solution (g/mL)
CU = concentration of Alprazolam in the Sample
solution (g/mL)
F = relative response factor (see Table 1)