1. No category

Accessed from 10.6.1.1 by correct6 on Tue May 26 10:49:24 EDT 2015
USP 38
Official Monographs / Edetate 3263
Analysis
Samples: Standard solution and Sample solution
Measure the responses for the major peaks.
Acceptance criteria: The peak response of nitrilotriacetic acid from the Sample solution does not exceed
the difference between the nitrilotriacetic acid peak responses obtained from the Standard solution and the
Sample solution (0.1%).
SPECIFIC TESTS
• PH 〈791〉
Sample solution: A solution (1 in 5)
Acceptance criteria: 6.5–8.0
• WATER DETERMINATION, Method I 〈921〉
Sample: 0.2 g
Acceptance criteria: 5.0%–13.0%
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers. No
storage requirements specified.
• USP REFERENCE STANDARDS 〈11〉
USP Edetate Calcium Disodium RS
Edetate Calcium Disodium Injection
.
» Edetate Calcium Disodium Injection is a sterile
solution of Edetate Calcium Disodium in Water
for Injection. It contains, in each mL, not less
than 180 mg and not more than 220 mg of
C10H12CaN2Na2O8.
.
Edetate Disodium
C10H14N2Na2O8 · 2H2O
C10H14N2Na2O8
372.24
336.21
DEFINITION
Edetate Disodium contains NLT 99.0% and NMT 101.0% of
edetate disodium (C10H14N2Na2O8), calculated on the
dried basis.
IDENTIFICATION
• A. INFRARED ABSORPTION 〈197K〉
Sample: Undried
Acceptance criteria: Meets the requirements
• B.
Sample: 50 mg
Analysis: To 5 mL of water in a test tube add 2 drops of
ammonium thiocyanate TS and 2 drops of ferric chloride TS. To the deep red solution add the Sample.
Acceptance criteria: The red color is discharged, leaving a yellowish solution.
• C. IDENTIFICATION TESTS—GENERAL, Sodium 〈191〉: It meets
the requirements of the flame test.
ASSAY
• PROCEDURE
Sample solution: Dissolve 5 g of Edetate Disodium in
about 100 mL of water contained in a 250-mL volumetric flask. Add water to volume.
Analysis: Place 200 mg of chelometric standard calcium
carbonate, previously dried at 110° for 2 h and cooled
in a desiccator, into a 400-mL beaker. Add 10 mL of
water, and swirl to form a slurry. Cover the beaker with
a watch glass, and without removing the latter, add
2 mL of 3 N hydrochloric acid from a pipet. Swirl the
contents of the beaker, and dissolve the calcium carbonate. With water, wash down the sides of the beaker,
the outer surface of the pipet, and the watch glass, and
dilute with water to 100 mL. While stirring the solution,
preferably with a magnetic stirrer, add 30 mL of the
Sample solution from a 50-mL buret. Add 15 mL of 1 N
sodium hydroxide and 0.30 g of hydroxy naphthol
blue, and continue the titration with the Sample solution
to a blue endpoint.
Calculate the weight of edetate disodium
(C10H14N2Na2O8) in the portion of Edetate Disodium
taken:
Result = (VT/VU) × W × (Mr1/Mr2)
VT
VU
= total volume of the Sample solution (mL)
= volume of the Sample solution consumed in
the titration (mL)
W
= weight of calcium carbonate (mg)
Mr1
= molecular weight of edetate disodium, 336.21
Mr2
= molecular weight of calcium carbonate,
100.09
Acceptance criteria: 99.0%–101.0% on the dried basis
IMPURITIES
Delete the following:
•• HEAVY METALS, Method II 〈231〉: NMT 50 ppm• (Official 1.
Dec-2015)
• CALCIUM
Sample solution: 1 g of Edetate Disodium in 20 mL of
water
Analysis: To the Sample solution add 2 drops of methyl
red TS, and neutralize with 6 N ammonium hydroxide.
Add 3 N hydrochloric acid dropwise until the solution is
just acidic, and then add 1 mL of ammonium oxalate
TS.
Official from May 1, 2015
Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.
USP Monographs
Packaging and storage—Preserve in single-dose containers, preferably of Type I glass.
USP Reference standards 〈11〉—
USP Edetate Calcium Disodium RS
USP Endotoxin RS
Identification—
A: Transfer a volume of Injection, equivalent to about 1 g
of edetate calcium disodium, to an evaporating dish, and
evaporate on a steam bath to dryness: the residue responds
to Identification test A under Edetate Calcium Disodium.
B: It responds to Identification test B under Edetate Calcium Disodium.
Bacterial endotoxins 〈85〉—It contains not more than
0.01 USP Endotoxin Unit per mg of edetate calcium disodium.
pH 〈791〉: between 6.5 and 8.0.
Particulate matter 〈788〉: meets the requirements for
small-volume injections.
Other requirements—It meets the requirements under Injections 〈1〉.
Assay—Dilute an accurately measured volume of Injection,
equivalent to about 1 g of edetate calcium disodium with
water to about 75 mL. Add 25 mL of 1 N acetic acid and
1 mL of diphenylcarbazone TS, mix, and titrate slowly with
0.1 M mercuric nitrate VS to the appearance of the first
purplish color. Perform a blank determination, and make
any necessary correction. Each mL of 0.1 M mercuric nitrate
is equivalent to 37.43 mg of C10H12CaN2Na2O8.
Glycine, N,N′-1,2-ethanediylbis[N-(carboxymethyl)-, disodium salt, dihydrate;
Disodium (ethylenedinitrilo)tetraacetate dihydrate
[6381-92-6].
Anhydrous [139-33-3].
Accessed from 10.6.1.1 by correct6 on Tue May 26 10:49:24 EDT 2015
USP Monographs
3264 Edetate / Official Monographs
Acceptance criteria: No precipitate is formed.
• LIMIT OF NITRILOTRIACETIC ACID
Mobile phase: Add 10 mL of 1.0 M tetrabutylammonium hydroxide in methanol to 200 mL of water, and
adjust with 1 M phosphoric acid to a pH of 7.5 ± 0.1.
Transfer the solution so obtained to a 1000-mL volumetric flask. Add 90 mL of methanol, and dilute with
water to volume. Pass through a filter of 0.5-µm or
finer pore size, and degas.
Cupric nitrate solution: 10 mg/mL of cupric nitrate
[Cu(NO3)2]
Standard stock solution: Transfer 100 mg of nitrilotriacetic acid to a 10-mL volumetric flask. Add 0.5 mL of
ammonium hydroxide, mix, and dilute with water to
volume.
Standard solution: Transfer 1.0 g of Edetate Disodium
to a 100-mL volumetric flask. Add 100 µL of Standard
stock solution, and dilute with Cupric nitrate solution to
volume. If necessary, sonicate to dissolve.
System suitability solution: Transfer 10 mg of Edetate
Disodium to a 100-mL volumetric flask. Add 100 µL of
Standard stock solution, and dilute with Cupric nitrate
solution to volume. If necessary, sonicate to dissolve.
Sample solution: 10 mg/mL of Edetate Disodium in Cupric nitrate solution. If necessary, sonicate to dissolve.
Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: LC
Detector: UV 254 nm
Column: 4.6-mm × 15-cm; packing L7
Flow rate: 2 mL/min
Injection volume: 50 µL
System suitability
Samples: Standard solution and System suitability
solution
[NOTE—The relative retention times for nitrilotriacetic
acid, copper, and edetate are about 0.35, 0.65, and
1.0, respectively.]
Suitability requirements
Resolution: NLT 3 between nitrilotriacetic acid and
copper, System suitability solution
Relative standard deviation: NMT 2.0%, Standard
solution
Analysis
Samples: Standard solution and Sample solution
Acceptance criteria: NMT 0.1%; the response of the
nitrilotriacetic acid peak of the Sample solution does not
exceed the difference between the nitrilotriacetic acid
peak responses from the Standard solution and the Sample solution.
SPECIFIC TESTS
• PH 〈791〉
Sample solution: 50 mg/mL
Acceptance criteria: 4.0–6.0
• LOSS ON DRYING 〈731〉
Analysis: Dry at 150° for 6 h.
Acceptance criteria: 8.7%–11.4%
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in well-closed
containers.
• USP REFERENCE STANDARDS 〈11〉
USP Edetate Disodium RS
Edetate Disodium Injection
.
» Edetate Disodium Injection is a sterile solution
of Edetate Disodium in Water for Injection,
which, as a result of pH adjustment, contains varying amounts of the disodium and trisodium
USP 38
salts. It contains the equivalent of not less than
90.0 percent and not more than 110.0 percent of
the labeled amount of C10H14N2Na2O8.
Packaging and storage—Preserve in single-dose containers, preferably of Type I glass.
USP Reference standards 〈11〉—
USP Edetate Disodium RS
USP Endotoxin RS
Identification—Transfer a volume of Injection, equivalent
to about 1 g of edetate disodium, to an evaporating dish,
adjust with 3 N hydrochloric acid to a pH of 5.0, and evaporate on a steam bath to dryness: the residue responds to
Identification tests A and C under Edetate Disodium.
Bacterial endotoxins 〈85〉—It contains not more than 0.2
USP Endotoxin Unit per mg of edetate disodium.
pH 〈791〉: between 6.5 and 7.5.
Other requirements—It meets the requirements under Injections 〈1〉.
Assay—
Assay preparation—Dilute an accurately measured volume
of Injection, equivalent to about 2 g of edetate disodium,
with water to volume in a 100-mL volumetric flask, and
mix.
Procedure—Proceed as directed for Procedure in the Assay
under Edetate Disodium. Calculate the weight, in mg, of
C10H14N2Na2O8 in the volume of Injection taken by the
formula:
(336.21/100.09)W(VT /V)
in which 336.21 and 100.09 are the molecular weights of
edetate disodium and calcium carbonate, respectively; W is
the weight, in mg, of calcium carbonate; VT is the volume,
in mL, of the Assay preparation; and V is the volume, in mL,
of the Assay preparation consumed in the titration.
Edrophonium Chloride
.
C10H16ClNO 201.69
Benzenaminium, N-ethyl-3-hydroxy-N,N-dimethyl-, chloride.
Ethyl(m-hydroxyphenyl)dimethylammonium chloride
[116-38-1].
» Edrophonium Chloride contains not less than
98.0 percent and not more than 100.5 percent of
C10H16ClNO, calculated on the dried basis.
Packaging and storage—Preserve in well-closed containers.
USP Reference standards 〈11〉—
USP Edrophonium Chloride RS
Identification—
A: Infrared Absorption 〈197K〉.
B: Ultraviolet Absorption 〈197U〉—
Solution: 50 µg per mL.
Medium: 0.1 N hydrochloric acid.
Absorptivities at 273 nm, calculated on the dried basis, do
not differ by more than 2.0%.
C: To 10 mL of a solution (1 in 10) add 1 drop of ferric
chloride TS: a violet-blue color is produced.
Official from May 1, 2015
Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.