Accessed from 10.6.1.
1 by JNJconsumer on Thu May 11 14:38:36 EDT 2017
2602 Adenosine / Official Monographs
ASSAY
• PROCEDURE
Mobile phase: Dissolve 2.0 g of monobasic potassium
phosphate in 800 mL of water. Add 5 mL of 1.0 M tet-
rabutylammonium dihydrogen phosphate, dilute with
water to 980 mL, and mix. Add 20 mL of acetonitrile.
System suitability solution: 0.03 mg/mL each of USP
Adenosine RS and inosine dissolved in warm water (50°
to 55°), and diluted with water
Standard solution: 0.03 mg/mL of USP Adenosine RS
dissolved in warm water (50° to 55°), and diluted with
water to volume. Before addition of the warm water, if
sodium chloride is present in the Injection, add 0.01 mL
of a solution of sodium chloride (0.9 in 100) per mL of
the anticipated final volume of the Standard solution.
Sample solution: Nominally 0.03 mg/mL of adenosine,
from a suitable volume of Injection in water
Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: LC
Detector: UV 254 nm
Column: 3.9-mm × 30-cm; packing L1
Flow rate: 2.5 mL/min
Injection volume: 10 µL
Run time: 2.5 times the retention time of adenosine
System suitability
Samples: System suitability solution and Standard
solution
[NOTE—The relative retention times of inosine and
adenosine are 0.43 and 1.0, respectively.]
Suitability requirements
Resolution: NLT 6.0 between adenosine and inosine,
System suitability solution
Tailing factor: NMT 2.0 for the adenosine peak, Sys-
tem suitability solution
Relative standard deviation: NMT 1.5%, Standard
solution
Analysis
USP Monographs
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of
adenosine (C10H13N5O4) in the portion of Injection
taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response from the Sample solution
rS = peak response from the Standard solution
CS = concentration of USP Adenosine RS in the
Standard solution (mg/mL)
CU = nominal concentration of adenosine in the
Sample solution (mg/mL)
Acceptance criteria: 90.0%–110.0%
IMPURITIES
• ORGANIC IMPURITIES
Mobile phase, System suitability solution, Standard
solution, Chromatographic system, and System suit-
ability: Proceed as directed in the Assay.
Sample solution: Nominally 0.3 mg/mL of adenosine
from a volume of Injection, in water
Analysis
Sample: Sample solution
Calculate the percentage of each impurity in the vol-
ume of Injection taken:
Result = (rU/rT) × 100
rU = peak response for each impurity
rT = sum of the responses of all of the peaks
Official from May 1, 2017
Copyright (c) 2017 The United States Pharmacopeial Convention. All rights reserved.
USP 40
Acceptance criteria
Any individual impurity: NMT 1.0%
Total impurities: NMT 1.5%
SPECIFIC TESTS
• PH 〈791〉: 4.5–7.5
• PARTICULATE MATTER IN INJECTIONS 〈788〉: It meets the re-
quirements for small-volume injections.
• BACTERIAL ENDOTOXINS TEST 〈85〉: When the product is
used for rapid intravenous injection, it contains NMT
11.62 USP Endotoxin Units/mg of adenosine. When the
product is used for continuous peripheral intravenous in-
fusion, it contains NMT 5.95 USP Endotoxin Units/mg of
adenosine.
• OTHER REQUIREMENTS: It meets the requirements under
Injections and Implanted Drug Products 〈1〉.
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight, single-dose
containers, preferably of Type I glass, and store at con-
trolled room temperature.
• USP REFERENCE STANDARDS 〈11〉
USP Adenosine RS
USP Endotoxin RS
.
Medical Air
DEFINITION
Medical Air is a natural or synthetic mixture of gases consist-
ing largely of nitrogen and oxygen. It contains NLT
19.5% and NMT 23.5%, by volume, of oxygen (O2).
IDENTIFICATION
• A. The paramagnetic signal exhibited by the Sample gas
in the Assay confirms the presence of oxygen.
• B. The Sample gas in the Assay meets the assay Accep-
tance criteria.
ASSAY
• PROCEDURE
The certified standards called for in the following test are
listed in Reagents, Indicators, and Solutions.
Zero gas: Nitrogen certified standard
Span gas: 21% Oxygen certified standard. [NOTE—See
Reagents, Indicators, and Solutions.]
Sample gas: Medical Air
Mode: Paramagnetic oxygen measurement (see Medical
Gases Assay 〈415〉)
Analysis: Determine the concentration of oxygen in
percentage by volume of Medical Air using a suitable
paramagnetic analyzer.
Acceptance criteria: 19.5%–23.5% of oxygen by
volume
IMPURITIES
See Impurities Testing in Medical Gases Assay 〈413〉. The de-
tector tubes called for in the following tests are listed in
Reagents, Indicators, and Solutions.
If the label indicates that Medical Air is a synthetic mixture
of oxygen and nitrogen, and where oxygen complies to
Oxygen USP and Nitrogen complies to Nitrogen NF, then
the Impurities tests are not required.
• LIMIT OF CARBON DIOXIDE
Sample: Detector tube manufacturer’s recommended
volume ±5% of Medical Air
Analysis: Pass the Sample through a carbon dioxide de-
tector tube at the rate specified for the tube by the
detector tube manufacturer.
Acceptance criteria: NMT 500 ppm
• LIMIT OF CARBON MONOXIDE
Sample: Detector tube manufacturer’s recommended
volume ±5% of Medical Air
Accessed from 10.6.1.1 by JNJconsumer on Thu May 11 14:38:36 EDT 2017
USP 40
Analysis: Pass the Sample through a carbon monoxide
detector tube at the rate specified for the tube by the
detector tube manufacturer.
Acceptance criteria: NMT 10 ppm
• LIMIT OF SULFUR DIOXIDE
Sample: Detector tube manufacturer’s recommended
volume ±5% of Medical Air
Analysis: Pass the Sample through a sulfur dioxide de-
tector tube at the rate specified for the tube by the
detector tube manufacturer.
Acceptance criteria: NMT 5 ppm
• LIMIT OF NITRIC OXIDE AND NITROGEN DIOXIDE
Sample: Detector tube manufacturer’s recommended
volume ±5% of Medical Air
Analysis: Pass the Sample through a nitric oxide–ni-
trogen dioxide detector tube at the rate specified for
the tube by the detector tube manufacturer.
Acceptance criteria: NMT 2.5 ppm
• LIMIT OF WATER AND OIL
Analysis: Support one container in an inverted position
(with the valve at the bottom) for 5 min. Cautiously
open the valve slightly, maintaining the container in an
inverted position. Vent the gas with a barely audible
flow against a stainless steel mirror for a few seconds.
Acceptance criteria: No liquid is discernible on the
mirror.
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in pressurized contain-
ers. Container connections shall be appropriate for air.
Adaptors shall not be used to connect containers to pa-
tient use supply system piping or equipment.
• LABELING: Label states if Medical Air is a synthetic mix-
ture of Oxygen USP and Nitrogen NF. Where it is piped
directly from the collecting tank to the patient point of
use, label each outlet “Medical Air”.
.
Alanine
C3H7NO2 89.09
L-Alanine [56-41-7].
DEFINITION
Alanine contains NLT 98.5% and NMT 101.5% of L-alanine
(C3H7NO2), calculated on the dried basis.
IDENTIFICATION
• A. INFRARED ABSORPTION 〈197K〉
ASSAY
• PROCEDURE
Sample: 80 mg of Alanine
Titrimetric system
(See Titrimetry 〈541〉.)
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
Analysis: Dissolve the Sample in a mixture of 3 mL of
formic acid and 50 mL of glacial acetic acid, and titrate
with Titrant.
Calculate the percentage of L-alanine (C3H7NO2) in the
portion of Alanine taken:
Result = [(VS − VB) × N × F × 100]/W
VS = Titrant volume consumed by the Sample (mL)
Official from May 1, 2017
Copyright (c) 2017 The United States Pharmacopeial Convention. All rights reserved.
Official Monographs / Alanine 2603
VB = Titrant volume consumed by the Blank (mL)
N = actual normality of the Titrant (mEq/mL)
F = equivalency factor, 89.09 mg/mEq
W = Sample weight (mg)
Acceptance criteria: 98.5%–101.5% on the dried basis
IMPURITIES
• RESIDUE ON IGNITION 〈281〉: NMT 0.15%
• CHLORIDE AND SULFATE, Chloride 〈221〉
Standard solution: 0.70 mL of 0.020 N hydrochloric
acid
Sample: 1.0 g of Alanine
Acceptance criteria: NMT 0.05%
• CHLORIDE AND SULFATE, Sulfate 〈221〉
Standard solution: 0.30 mL of 0.020 N sulfuric acid
Sample: 1.0 g of Alanine
Acceptance criteria: NMT 0.03%
• IRON 〈241〉: NMT 30 ppm
Delete the following:
•• HEAVY METALS, Method I 〈231〉: NMT 15 ppm• (Official 1-
.
Jan-2018)
• RELATED COMPOUNDS
Mobile phase: 0.008 N sulfuric acid solution
System suitability solution: A mixture of 0.05 mg/mL
of USP Fumaric Acid RS, 0.05 mg/mL of USP Maleic
Acid RS, and 3 mg/mL of USP Malic Acid RS in water
Maleic acid standard solution: 0.05 mg/mL of USP
Maleic Acid RS in water
Malic acid standard solution: 3 mg/mL of USP Malic
Acid RS in water
Fumaric acid standard solution: 0.05 mg/mL of USP
Fumaric Acid RS in water
Sample solution: 100 mg/mL of Alanine in water
Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
USP Monographs
Mode: LC
Detector: UV 214 nm
Column: 7.8-mm × 30-cm; 9-µm packing L17
Column temperature: 30°
Flow rate: 0.6 mL/min
Injection volume: 10 µL
System suitability
Sample: System suitability solution
[NOTE—See Table 1 for the relative retention times.]
Suitability requirements
Resolution: NLT 1.5 between maleic acid and malic
acid
Relative standard deviation: NMT 5.0% for each of
fumaric acid, maleic acid, and malic acid
Analysis
Samples: Standard solutions and Sample solution
Calculate the percentage of each specified acid in the
portion of Alanine taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response of maleic acid, malic acid, or
fumaric acid from the Sample solution
rS = peak response of maleic acid, malic acid, or
fumaric acid from the corresponding
Standard solution
CS = concentration of USP Maleic Acid RS, USP
Malic Acid RS, or USP Fumaric Acid RS in the
corresponding Standard solution (mg/mL)
CU = concentration of Alanine in the Sample solution
(mg/mL)
Calculate the percentage of any unspecified impurity in
the portion of Alanine taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response of any unspecified impurity
from the Sample solution