# 交联聚维酮-USP35

Accessed from 128.83.63.20 by nEwp0rt1 on Tue Nov 29 21:22:37 EST 2011

NF 30
= factor converting glycolic acid to sodium glycolate, 12.9 W1 = weight of glycolic acid in the specimen (mg), determined from the standard curve and the absorbance of the Sample solution b = percentage of Loss on Drying, determined separately W2 = weight of the specimen taken (g) Acceptance criteria: The sum of the percentages of sodium chloride and sodium glycolate is NMT 0.5%. SPECIFIC TESTS ? CONTENT OF WATER-SOLUBLE MATERIAL Analysis: Disperse 10 g in 800 mL of water, and stir for 1 min every 10 min during the first 30 min. Allow to stand for an additional h, or centrifuge, if necessary. Decant 200 mL of the aqueous slurry onto a rapid-filtering filter paper in a vacuum filtration funnel, apply vacuum, and collect about 150 mL of the filtrate. Pour the filtrate into a tared 250-mL beaker, weigh, and calculate the weight, in g, of the filtrate, W3, by difference. Concentrate on a hot plate to a small volume, but not to dryness; dry at 105° for 4 h; again weigh; and calculate the weight, in g, of residue W1, by difference. Calculate the percentage of water-soluble material in the specimen, on the dried basis, taken: Result = [100 × W1 × (800 + W2)]/{W2 × W3 × [1 ? (0.01 × b)]} W1 = weight of residue by difference (g) W2 = weight of the specimen taken (g) W3 = weight of the filtrate by difference (g) b = percentage Loss on Drying of the specimen taken Acceptance criteria: NMT 10.0% ? DEGREE OF SUBSTITUTION Sample: 1 g Analysis: Transfer the Sample to a glass-stoppered, 500-mL conical flask. Add 300 mL of sodium chloride solution (1 in 10), then add 25.0 mL of 0.1 N sodium hydroxide VS. Insert the stopper, and allow to stand for 5 min with intermittent shaking. Add 5 drops of m-cresol purple TS, and from a buret add 15 mL of 0.1 N hydrochloric acid VS. Insert the stopper in the flask, and shake. If the solution is violet, add 0.1 N hydrochloric acid VS in 1-mL portions until the solution becomes yellow, shaking after each addition. Titrate with 0.1 N sodium hydroxide VS to a violet endpoint. Calculate the net number of milliequivalents, M, of base required for the neutralization of 1 g of Croscarmellose Sodium, on the dried basis. Calculate the degree of acid carboxymethyl substitution, A: Result = 1150 × M/[7102 ? (412 × M) ? (80 × C)] M C = milliequivalents = percentage of Residue on Ignition of the Croscarmellose Sodium as determined in the test for Residue on Ignition Calculate the degree of sodium carboxymethyl substitution, S: Result = [162 + (58 × A)] × C/[7102 ? (80 × C)] = degree of acid carboxymethyl substitution, as determined above C = percentage of Residue on Ignition of the Croscarmellose Sodium as determined in the test for Residue on Ignition The degree of substitution is the sum of A + S. Acceptance criteria: The degree of substitution is 0.60–0.85, on the dried basis ? LOSS ON DRYING ?731?: Dry a sample at 105° for 6 h: it loses NMT 10.0% of its weight. ? MICROBIAL ENUMERATION TESTS ?61? and TESTS FOR SPECIFIED MICROORGANISMS ?62?: The total aerobic microbial count does not exceed 1000 cfu/g, and the total combined molds A F

Official Monographs / Crospovidone 1775
and yeasts count does not exceed 100 cfu/g. It meets the requirements of the tests for absence of Escherichia coli. ? PH ?791?: The pH of the dispersion is 5.0–7.0. Mix 1 g with 100 mL of water for 5 min. ? SETTLING VOLUME Analysis: To 75 mL of water in a 100-mL graduated cylinder, add 1.5 g of it in 0.5-g portions, shaking vigorously after each addition. Add water to make 100 mL, shake again until all of the powder is homogeneously distributed, and allow to stand for 4 h. Note the volume of the settled mass. Acceptance criteria: The volume of the settled mass is 10.0–30.0 mL ADDITIONAL REQUIREMENTS ? PACKAGING AND STORAGE: Preserve in well-closed containers. No storage requirements specified.

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Crospovidone
Portions of the monograph text that are national USP text, and are not part of the harmonized text, are marked with symbols (33) to specify this fact.

(C6H9NO)n 1-Ethenyl-2-pyrrolidinone homopolymer; 1-Vinyl-2-pyrrolidinone homopolymer [9003-39-8]. DEFINITION Crospovidone is a water-insoluble synthetic cross-linked homopolymer of N-vinyl-2-pyrrolidinone. It contains NLT 11.0% and NMT 12.8% of nitrogen (N), calculated on the dried basis. Two types of Crospovidone are available, depending on the particle size: Type A and Type B. IDENTIFICATION ? 3A. INFRARED ABSORPTION ?197K?: Previously dried in a vacuum at 105° for 1 h3 ? B. Sample: 1 g Analysis: Suspend the Sample in 10 mL of water, add 0.1 mL of 0.1 N iodine, and shake for 30 s. Add 1 mL of starch TS, and shake. Acceptance criteria: No blue color develops. ? C. To 10 mL of water add 0.1 g and shake. A suspension is formed, and no clear solution is obtained within 15 min. ? D. Sample: 20 g of the dried substance Analysis: Clean and dry the analytical sieves used in the analysis by washing the sieves in hot water. Allow to dry overnight in a drying cabinet at 105°. Place the Sample in a 1000-mL conical flask, add 500 mL of water, and shake the suspension for 30 min. Pour the suspension through a 63?m analytical sieve, previously tared, and rinse the sieve with water until the filtrate is clear. Dry the sieve and sample residue at 105° for 5 h in a drying cabinet without circulating air. Cool in a desiccator for 30 min, and weigh. Calculate the percentage sieving residue fraction of sample particles having a diameter of more than 63 ?m: Result = [(m1 ? m3) × 100]/m2 m1 m3 m2 = mass of the sieve and sample residue, after drying for 5 h (g) = mass of the sieve (g) = initial mass of the sample, calculated on a dried basis (g)

Accessed from 128.83.63.20 by nEwp0rt1 on Tue Nov 29 21:22:37 EST 2011

1776 Crospovidone / Official Monographs
Acceptance criteria: If the sieving residue fraction is more than 15%, the substance is classified as Type A; if the sieving residue fraction is NMT 15%, the substance is classified as Type B. ASSAY ? NITROGEN DETERMINATION, Method II ?461? Sample: 0.1 g Analysis: Proceed as directed, using the Sample. In the Procedure, omit the use of hydrogen peroxide, and use 5 g of a powdered mixture of potassium sulfate, cupric sulfate, and titanium dioxide (33:1:1), instead of potassium sulfate and cupric sulfate (10:1). Heat until a clear, light green solution is obtained. Heat for an additional 45 min, and proceed as directed for Procedure, beginning with “Cautiously add to the digestion mixture 70 mL of water”. Acceptance criteria: 11.0%–12.8% on the dried basis IMPURITIES ? RESIDUE ON IGNITION ?281?: NMT 0.1%, determined on 1.0 g ? 3HEAVY METALS, Method II ?231?: NMT 10 ppm3 ? PEROXIDES Sample suspension A: [NOTE—Use for Type A.] 40 mg/mL in water. To 25 mL of this suspension add 2 mL of titanium trichloride–sulfuric acid TS. Allow to stand for 30 min, and filter. Sample suspension B: [NOTE—Use for Type B.] 16 mg/mL in water. To 25 mL of this suspension add 2 mL of titanium trichloride–sulfuric acid TS. Allow to stand for 30 min, and filter. Compensation liquid A: [NOTE—Use for Type A.] 40 mg/mL in water. Filter, take 25 mL, and add 2 mL of a 13% solution of sulfuric acid. Compensation liquid B: [NOTE—Use for Type B.] 16 mg/mL in water. Filter, take 25 mL, and add 2 mL of a 13% solution of sulfuric acid. Analysis: Measure the absorbance of the filtrate at 405 nm against the appropriate compensation liquid. Acceptance criteria: NMT 0.35. For Type A, this corresponds to NMT 400 ppm expressed as H2O2; for Type B, this corresponds to NMT 1000 ppm expressed as H2O2. ? VINYLPYRROLIDINONE Mobile phase: Acetonitrile and water (1:9) Sample solution: 25 mg/mL of suspension in methanol. Shake for 60 min. Leave the bulk to settle, and pass through a filter of 0.2-?m pore size. Reference stock solution A: 5 ?g/mL of vinylpyrrolidinone in methanol Reference stock solution B: 100 ?g/mL of vinylpyrrolidinone and 5 mg/mL of vinyl acetate in methanol Reference solution A: A 1-in-20 solution of Reference stock solution A in Mobile phase Reference solution B: A 1-in-100 solution of Reference stock solution B in Mobile phase Chromatographic system (See Chromatography ?621?, System Suitability.) Mode: LC Detector: UV Analytical wavelength: 235 nm Precolumn: 4-mm × 2.5-cm; 5-?m packing L1 Column: 4-mm × 25-cm; 5-?m packing L1 Column temperature: 40° Flow rate: 1 mL/min Injection size: 50 ?L. [NOTE—After each injection of the Sample solution, wash the precolumn by passing the Mobile phase backwards, at the same flow rate as applied in the test, for 30 min.] System suitability Samples: Reference solution A and Reference solution B Suitability requirements Resolution: NLT 2.0 between vinylpyrrolidone and vinyl acetate, Reference solution B

NF 30
Relative standard deviation: NMT 2.0% for 6 injections, Reference solution A Analysis Samples: Sample solution and Reference solution A Record the chromatograms, and measure the responses for the vinylpyrrolidinone peak. Acceptance criteria: The area of the peak from the Sample solution is NMT the area of the principal peak from Reference solution A (NMT 10 ppm). SPECIFIC TESTS ? LOSS ON DRYING ?731?: Dry 0.5 g at 105° to constant weight: it loses NMT 5.0% of its weight. ? WATER-SOLUBLE SUBSTANCES Sample: 25.0 g Analysis: Transfer the Sample to a 400-mL beaker, add 200 mL of water, and stir on a magnetic stirrer, using a 5-cm stirring bar, for 1 h. Transfer to a 250-mL volumetric flask with the aid of 25 mL of water. Add water to volume. Allow the bulk of the solids to settle. Pass 100 mL of the relatively clear supernatant through a membrane filter of 0.45-?m pore size, protected against clogging by superimposing a membrane filter of 3-?m pore size. While filtering, stir the solution above the filter manually or with a mechanical stirrer, taking care not to physically damage the membrane filter. Transfer 50.0 mL of the clear filtrate to a tared 100-mL beaker, evaporate to dryness, and dry at 110° for 3 h. Acceptance criteria: The weight of the residue does not exceed 75 mg (1.5%). ADDITIONAL REQUIREMENTS ? 3PACKAGING AND STORAGE: Preserve in tight containers.3 ? 3LABELING: The label states the type (Type A or Type B).3 ? 3USP REFERENCE STANDARDS ?11? USP Crospovidone RS3

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Gamma Cyclodextrin

(C6H10O5)8 Cyclooctaamylose; Cyclomaltooctaose [17465-86-0].

1297.12

DEFINITION Gamma Cyclodextrin is composed of 8 alpha-(1–4) linked Dglycopyranosyl units. It contains NLT 98.0% and NMT 102.0% of cyclooctaamylose (C6H10O5)8, calculated on the dried basis. IDENTIFICATION ? A. INFRARED ABSORPTION ?197K? ? B. The retention time of the major peak from the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.

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