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葬花公子铁杆木虫 (著名写手)
General
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[求助]
求赛来昔布（Celecoxibum）在USP36以上的质量标准 已有1人参与
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| 各位大虾，紧急求助Celecoxibum的最新质量标准，最好是胶囊或制剂的，原料的EP7.5和USP35的标准我自己就有，USP36的没有，求各位帮忙！~ |
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kobeyy
金虫 (正式写手)
- 应助: 7 (幼儿园)
- 金币: 3346.6
- 散金: 5
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【答案】应助回帖
★ ★ ★ ★ ★ ★ ★ ★ ★ ★
感谢参与，应助指数 +1
葬花公子: 金币+10, ★★★很有帮助, 谢谢 2013-12-31 12:17:46
感谢参与，应助指数 +1
葬花公子: 金币+10, ★★★很有帮助, 谢谢 2013-12-31 12:17:46
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Celecoxib (sel'' e kox' ib). C17H14F3N3O2S 381.4 4-[5-(4-Methylphenyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl]benzenesulfonamide; p-[5-p-Tolyl-3-(trifluoromethyl)pyrazol-1-yl]benzenesulfonamide [169590-42-5]. DEFINITION Celecoxib contains NLT 98.0% and NMT 102.0% of C17H14F3N3O2S, calculated on the anhydrous basis. IDENTIFICATION A. Infrared Absorption 197: [Note??Methods 197A, 197K, or 197M under Infrared Absorption may be used. ] [Note??If the spectra obtained show differences, dissolve the substance to be examined and the Reference Standard separately in isopropyl alcohol, evaporate to dryness, and record the new spectra. ] B. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay. ASSAY Procedure Buffer: 2.7 g/L of monobasic potassium phosphate adjusted with phosphoric acid to a pH of 3.0 ?? 0.2 Mobile phase: Methanol, acetonitrile, and Buffer (3:1:6) Diluent: Methanol and water (3:1) System suitability solution: 0.5 mg/mL of USP Celecoxib RS and 2.4 ??/mL each of USP Celecoxib Related Compound A RS and USP Celecoxib Related Compound B RS in Diluent Standard solution: 0.5 mg/mL of USP Celecoxib RS in Diluent Sample solution: 0.5 mg/mL of Celecoxib in Diluent Chromatographic system (See Chromatography 621, System Suitability.) Mode: LC Detector: UV 215 nm Column: 4.6-mm ?? 25-cm; 5-?? packing L11 Column temperature: 60 Flow rate: 1.5 mL/min Injection size: 25 L Run time: About 1.5 times the celecoxib peak elution System suitability Samples: System suitability solution and Standard solution Suitability requirements Resolution: NLT 1.8 between celecoxib related compound A and celecoxib and NLT 1.8 between celecoxib and celecoxib related compound B, System suitability solution Relative standard deviation: NMT 0.73%, Standard solution Analysis Samples: Standard solution and Sample solution Calculate the percentage of C17H14F3N3O2S in the portion of Celecoxib taken: Result = (rU/rS) ?? (CS/CU) ?? 100 rU = = peak response from the Sample solution rS = = peak response from the Standard solution CS = = concentration of the Standard solution (mg/mL) CU = = concentration of the Sample solution (mg/mL) Acceptance criteria: 98.0%?C102.0% on the anhydrous basis IMPURITIES Inorganic Impurities Heavy Metals: NMT 20 ppm Diluent: Acetone and water (17:3) Standard solution: Dilute 1.0 mL of Standard Lead Solution, prepared as directed under Heavy Metals 231, Special Reagents, with Diluent to 20 mL. Sample solution: Dissolve 0.50 g of Celecoxib in 20 mL of Diluent. Blank solution: 20 mL of Diluent Analysis Samples: Standard solution, Blank solution, and Sample solution To each solution, add 2 mL of pH 3.5 Acetate Buffer, prepared as directed under Heavy Metals 231, Method I. Mix, and add to each solution 1.2 mL of thioacetamide?Cglycerin base TS. Mix immediately, and allow to stand for 2 min. Pass the solutions through a filter of 0.45-?? pore size. Compare the spots on the filters obtained from each of the solutions. Acceptance criteria: The brownish-black color of the spot resulting from the Sample solution is not more intense than that of the spot resulting from the Standard solution. The test is invalid if the Standard solution does not show a brownish-black color compared to the Blank solution. Residue on Ignition 281: NMT 0.2%, using a platinum crucible Organic Impurities Procedure Buffer, Mobile phase, Diluent, System suitability solution, Sample solution, and Chromatographic system: Proceed as directed in the Assay. Standard solution: 0.5 ??/mL of USP Celecoxib RS in Diluent System suitability Samples: System suitability solution and Standard solution Suitability requirements Resolution: NLT 1.8 between celecoxib related compound A and celecoxib and NLT 1.8 between celecoxib and celecoxib related compound B, System suitability solution Signal-to-noise ratio: NLT 20, Standard solution Analysis Samples: Standard solution and Sample solution Calculate the percentage of each impurity in the portion of Celecoxib taken: Result = (rU/rS) ?? (CS/CU) ?? 100 rU = = peak response for each impurity in the Sample solution rS = = peak response of celecoxib in the Standard solution CS = = concentration of celecoxib in the Standard solution (mg/mL) CU = = concentration of Celecoxib in the Sample solution (mg/mL) Acceptance criteria Individual impurities: See Table 1. [Note??Disregard any impurity peak less than 0.05%. ] Table 1 Name Relative Retention Time Acceptance Criteria, NMT (%) Celecoxib related compound Aa 0.9 0.4 Celecoxib 1.0 ?? Celecoxib related compound Bb 1.1 0.10 Individual unspecified impurity ?? 0.10 Total impurities ?? 0.5 a 4-[5-(3-Methylphenyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl]benzenesulfonamide. b 4-[3-(4-Methylphenyl)-5-(trifluoromethyl)-1H-pyrazol-1-yl]benzenesulfonamide. SPECIFIC TESTS Water Determination, Method I 921: NMT 0.5%, using a 400-mg sample ADDITIONAL REQUIREMENTS Packaging and Storage: Preserve in tight containers, protected from light and moisture. Store at room temperature. USP Reference Standards 11 USP Celecoxib RS p-[5-p-Tolyl-3-(trifluoromethyl)pyrazol-1-yl]benzenesulfonamide. C17H14F3N3O2S 381.4 USP Celecoxib Related Compound A RS 4-[5-(3-Methylphenyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl]benzenesulfonamide. C17H14F3N3O2S 381.4 USP Celecoxib Related Compound B RS 4-[3-(4-Methylphenyl)-5-(trifluoromethyl)-1H-pyrazol-1-yl]benzenesulfonamide. C17H14F3N3O2S 381.4 Auxiliary Information?? Please check for your question in the FAQs before contacting USP. Topic/Question Contact Expert Committee Monograph Hillary Z Cai Scientific Liaison, Small Molecules (301) 230-3379 (SM22010) Monographs - Small Molecules 2 Reference Standards RS Technical Services 1-301-816-8129 rstech@usp.org USP37?CNF32 Page 2246 Pharmacopeial Forum: Volume No. 36(6) Page 1519 Chromatographic Column?? CELECOXIB Chromatographic columns text is not derived from, and not part of, USP 37 or NF 32. |
2楼2013-12-25 15:56:00
kobeyy
金虫 (正式写手)
- 应助: 7 (幼儿园)
- 金币: 3346.6
- 散金: 5
- 红花: 4
- 帖子: 436
- 在线: 203.8小时
- 虫号: 341450
- 注册: 2007-04-08
- 性别: GG
- 专业: 色谱分析
3楼2013-12-25 15:56:36