2348 Adenosine / Official Monographs USP 36

ASSAY rU = peak response for each impurity

rT = sum of the responses of all of the peaks
Acceptance criteria
Change to read:
Any individual impurity: NMT 1.0%
Total impurities: NMT 1.5%
PROCEDURE
Mobile phase: Dissolve 2.0 g of monobasic potassium SPECIFIC TESTS
phosphate in 800 mL of water. Add 5 mL of 1.0 M tet- PH 791: 4.57.5
rabutylammonium dihydrogen phosphate, dilute with PARTICULATE MATTER IN INJECTIONS 788: It meets the re-
water to 980 mL, and mix. Add 20 mL of acetonitrile. quirements for small-volume injections.
System suitability solution: 0.03 mg/mL each of USP BACTERIAL ENDOTOXINS TEST 85: When the product is
Adenosine RS and inosine dissolved in warm water (50 used for rapid intravenous injection, it contains NMT
to 55), and diluted with water 11.62 USP Endotoxin Units/mg of adenosine. When the
Standard solution: 0.03 mg/mL of USP Adenosine RS product is used for continuous peripheral intravenous in-
dissolved in warm water (50 to 55), and diluted with fusion, it contains NMT 5.95 USP Endotoxin Units/mg of
water to volume. Before addition of the warm water, if adenosine.
sodium chloride is present in the Injection, add 0.01 mL OTHER REQUIREMENTS: It meets the requirements under
of a solution of sodium chloride (0.9 in 100) per mL of Injections 1.
the anticipated final volume of the Standard solution.
ADDITIONAL REQUIREMENTS
L
LUSP36
PACKAGING AND STORAGE: Preserve in tight, single-dose Sample solution: Nominally 0.03 mg/mL of adenosine,
containers, preferably of Type I glass, and store at con- from a suitable volume of Injection in water
trolled room temperature. Chromatographic system
USP REFERENCE STANDARDS 11 (See Chromatography 621, System Suitability.)
USP Adenosine RS Mode: LC
USP Endotoxin RS Detector: UV 254 nm
Column: 3.9-mm 30-cm; packing L1
Flow rate: 2.5 mL/min
Injection volume: 10 L
Run time: 2.5 times the retention time of adenosine
.
System suitability
Medical Air
Samples: System suitability solution and Standard
solution
Medical Air is a natural or synthetic mixture of L
[NOTEThe relative retention times of inosine and
adenosine are 0.43 and 1.0, respectively.]LUSP36 gases consisting largely of nitrogen and oxygen.
Suitability requirements
It contains not less than 19.5 percent and not
Resolution: NLT 6.0 between adenosine and inosine,
more than 23.5 percent, by volume, of O
2
.
System suitability solution
Tailing factor: NMT 2.0 for the adenosine peak, Sys-
Packaging and storagePreserve in cylinders or in a low
tem suitability solution
pressure collecting tank. Containers used for Medical Air are
Relative standard deviation: NMT 1.5%, Standard
not to be treated with any toxic, sleep-inducing, or narcosis-
solution
producing compounds, and are not to be treated with any
Analysis
compound that would be irritating to the respiratory tract
Samples: Standard solution and Sample solution
when the Medical Air is used.
Calculate the percentage of the labeled amount of aden-
[NOTEReduce the container pressure by means of a
osine (C10H13N5O4) in the portion of Injection taken:
regulator. Measure the gases with a gas volume meter
downstream from the detector tube in order to minimize
Result = (rU/rS) (CS/CU) 100
contamination or change of the specimens. The various de-
tector tubes called for in the respective tests are listed under
rU = peak response from the Sample solution
Reagent Specifications in the section Reagents, Indicators, and
rS = peak response from the Standard solution
Solutions.]
CS = concentration of USP Adenosine RS in the
LabelingWhere it is piped directly from the collecting
Standard solution (mg/mL)
tank to the point of use, label each outlet Medical Air.
CU = nominal concentration of adenosine in the
Water and oilSupport 1 container in an inverted posi- Sample solution (mg/mL)
tion (with the valve at the bottom) for 5 minutes. Cautiously Acceptance criteria: 90.0%110.0%
open the valve slightly, maintaining the container in an in-
IMPURITIES verted position. Vent the gas with a barely audible flow
against a stainless steel mirror for a few seconds: no liquid is
discernible on the mirror.
Change to read:
OdorCarefully open the container valve to produce a
moderate flow of gas. Do not direct the gas stream toward
ORGANIC IMPURITIES
the face, but deflect a portion of the stream toward the
Mobile phase, System suitability solution, Standard
nose: no appreciable odor is discernible.
solution,
L
LUSP36 Chromatographic system, and Sys-
Carbon dioxidePass 1000 50 mL through a carbon di- tem suitability: Proceed as directed in the Assay.
oxide detector tube at the rate specified for the tube: the Sample solution: Nominally 0.3 mg/mL of adenosine
indicator change corresponds to not more than 0.05%. from a volume of Injection, in water
Analysis Carbon monoxidePass 1000 50 mL through a carbon
Sample: Sample solution monoxide detector tube at the rate specified for the tube:
Calculate the percentage of each impurity in the volume the indicator change corresponds to not more than 0.001%.
of Injection taken:
Limit of nitric oxide and nitrogen dioxidePass
550 50 mL through a nitric oxidenitrogen dioxide detec-
Result = (rU/rT) 100
tor tube at the rate specified for the tube: the indicator
change corresponds to not more than 2.5 ppm.
Official from December 1, 2013
Copyright (c) 2014 The United States Pharmacopeial Convention. All rights reserved.
Accessed from 200.31.14.243 by jamundi6 on Mon Apr 21 09:31:19 EDT 2014
USP 36 Official Monographs / Albendazole 2349
Sulfur dioxidePass 1050 50 mL through a sulfur diox- System suitability solution: 0.4 mg/mL each of USP
ide detector tube at the rate specified for the tube: the indi- L-Alanine RS and USP Glycine RS
cator change corresponds to not more than 5 ppm. Sample solution: 10 mg/mL of Alanine
Spray reagent: 2 mg/mL of ninhydrin in a mixture of
AssayDetermine the oxygen concentration of Medical Air
butyl alcohol and 2 N acetic acid (95:5)
using an electrochemical cell analyzer readable to 0.1% of
Developing solvent system: Butyl alcohol, glacial acetic
oxygen and calibrated with ambient air to an accuracy of
acid, and water (60:20:20)
0.2% of oxygen. [NOTEThe instrument utilizes the varia-
Application volume: 5 L
tions of electric current produced by the interaction of oxy-
Analysis
gen with an electrochemical cell to display the oxygen
Samples: Standard solution, System suitability solution,
strength of a confined sample or an in-line flow of the gas.
and Sample solution
This current generates a signal proportional to the oxygen
Proceed as directed for Chromatography 621, Thin-
concentration, which is displayed on a meter.]
Layer Chromatography. After air-drying the plate, re-
peat the development process. After air-drying a sec-
ond time, spray with Spray reagent, and heat to
. 100105 for 15 min. Examine the plate under
white light. The chromatogram obtained from the Alanine
System suitability solution exhibits two clearly sepa-
rated spots.
Acceptance criteria
Individual impurities: Any secondary spot of the Sam-
ple solution is not larger or more intense than the

principal spot of the Standard solution, NMT 0.5%
Total impurities: NMT 2.0%
C3H7NO2 89.09
L-Alanine [56-41-7].
SPECIFIC TESTS
OPTICAL ROTATION, Specific Rotation 781S: +13.7 to
DEFINITION
+15.1
Alanine contains NLT 98.5% and NMT 101.5% of C3H7NO2,
Sample solution: 100 mg/mL in 6 N hydrochloric acid
as L-alanine, calculated on the dried basis.
PH 791: 5.57.0, in a solution (1 in 20)
LOSS ON DRYING 731: Dry a sample at 105 for 3 h: it
IDENTIFICATION
loses NMT 0.2% of its weight.
INFRARED ABSORPTION 197K
ADDITIONAL REQUIREMENTS
ASSAY
PACKAGING AND STORAGE: Preserve in tight containers,
PROCEDURE
and store at controlled room temperature.
Sample: 80 mg of Alanine
USP REFERENCE STANDARDS 11
Titrimetric system
USP L-Alanine RS
(See Titrimetry 541.)
USP Glycine RS
Mode: Direct titration
Titrant: 0.1 N perchloric acid VS
Endpoint detection: Potentiometric
Blank: 3 mL of formic acid in 50 mL of glacial acetic
.
acid
Albendazole
Analysis: Dissolve the Sample in a mixture of 3 mL of
formic acid and 50 mL of glacial acetic acid, and titrate
with 0.1 N perchloric acid VS. Calculate the percentage
of C3H7NO2 in the portion taken:

Result = [(V B) N F 100]/W
V = Sample titrant volume (mL) C12H15N3O2S 265.33
B = Blank titrant volume (mL) Carbamic acid, [5-(propylthio)-1H-benzimidazol-2-yl]-,
N = titrant normality (mEq/mL) methyl ester;
F = equivalency factor: 89.09 mg/mEq Methyl 5-(propylthio)-2-benzimidazolecarbamate
W = weight of the Sample (mg) [54965-21-8].
Acceptance criteria: 98.5%101.5% on the dried basis
DEFINITION
IMPURITIES Albendazole contains NLT 98.0% and NMT 102.0% of al-
Inorganic Impurities bendazole (C12H15N3O2S), calculated on the dried basis.
RESIDUE ON IGNITION 281: NMT 0.15%
IDENTIFICATION
CHLORIDE AND SULFATE, Chloride 221: A 1.0-g portion
A. INFRARED ABSORPTION 197M
shows no more chloride than corresponds to 0.70 mL of
B. The RF value of the principal spot of the Sample solu-
0.020 N hydrochloric acid (0.05%).
tion corresponds to that of the principal spot of the Stan-
CHLORIDE AND SULFATE, Sulfate 221: A 1.0-g portion
dard solution, as obtained in the test for Organic
shows no more sulfate than corresponds to 0.30 mL of
Impurities.
0.020 N sulfuric acid (0.03%).
IRON 241: NMT 30 ppm
ASSAY
HEAVY METALS, Method I 231: NMT 15 ppm
PROCEDURE
Organic Impurities
Sample: 250 mg of Albendazole
PROCEDURE
Analysis: Transfer the Sample to a suitable flask, and dis-
Adsorbent: 0.25-mm layer of chromatographic silica
solve in 100 mL of glacial acetic acid, warming gently if
gel mixture
necessary. Cool, and titrate with 0.1 N perchloric acid
Standard solution: 0.05 mg/mL of USP L-Alanine RS.
VS to a potentiometric endpoint (see Titrimetry 541).
[NOTEThis solution has a concentration equivalent to
0.5% of that of the Sample solution.]
Official from December 1, 2013
Copyright (c) 2014 The United States Pharmacopeial Convention. All rights reserved.
Accessed from 200.31.14.243 by jamundi6 on Mon Apr 21 09:31:19 EDT 2014