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johncena木虫 (小有名气)
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[求助]
急求usp35版药典中Rivastigmine Tartrate 的质量标准
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| 如题，哪位虫友有pdf的话麻烦发我一份，在目录上查询应该是在p4580和p4581,谢谢！ |
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泡泡-211
至尊木虫 (知名作家)
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【答案】应助回帖
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johncena: 金币+3, ★★★★★最佳答案, 感谢你的帮助！ 2012-09-02 13:24:28
感谢参与，应助指数 +1
johncena: 金币+3, ★★★★★最佳答案, 感谢你的帮助！ 2012-09-02 13:24:28
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Rivastigmine Tartrate C14H22N2O2 · C4H6O6 400.42 Ethylmethylcarbamic acid, 3-[(S)-1-(dimethylamino)ethyl]phenyl ester, (2R ,3R )-2,3-dihydroxybutanedioate; (S)-3-[1-(Dimethylamino)ethyl]phenyl ethylmethylcarbamate, hydrogen tartrate [129101-54-8]. Rivastigmine 250.34 [123441-03-2]. DEFINITION Rivastigmine Tartrate contains NLT 98.0% and NMT 102.0% of the labeled amount of C14H22N2O2 · C4H6O6 , calculated on the anhydrous basis. IDENTIFICATION • A. Infrared Absorption 197K • B. The retention time of the major peak of the Sample solution corresponds to that of the System suitability solution, as obtained in the test for Organic Impurities, Procedure 2: Enantiomeric Purity. ASSAY • Procedure Buffer: 8.6 mg/mL of monobasic ammonium phosphate. Adjust with ammonia solution to a pH of 7.0. Mobile phase: Methanol, acetonitrile, and Buffer (15:15:70) System suitability solution: 0.05 mg/mL each of USP Rivastigmine Related Compound A RS and USP Rivastigmine Related Compound B RS in Mobile phase Standard solution: 0.2 mg/mL of USP Rivastigmine Tartrate RS in Mobile phase Sample solution: 0.2 mg/mL of Rivastigmine Tartrate in Mobile phase Chromatographic system (See Chromatography 621 , System Suitability.) Mode: LC Detector: UV 215 nm Column: 4.6-mm × 25-cm; 5-μm packing L7 Flow rate: 1.2 mL/min Injection size: 20 μL [Note— The flow rate may be adjusted to 1.5 mL/min, if needed, to achieve a recommended retention time of rivastigmine at about 10 min. ] System suitability Samples: System suitability solution and Standard solution Suitability requirements Resolution: NLT 1.5 between rivastigmine related compound A and rivastigmine related compound B, System suitability solution Column efficiency: NLT 5000 theoretical plates, Standard solution Tailing factor: NMT 3.0, Standard solution Relative standard deviation: NMT 2.0%, Standard solution Analysis Samples: Standard solution and Sample solution Calculate the percentage of C14H22N2O2 · C4H6O6 in the portion of Rivastigmine Tartrate 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%–102.0% on the anhydrous basis IMPURITIES Inorganic Impurities • Residue on Ignition 281 : NMT 0.1% • Heavy Metals, Method II 231 : NMT 20 ppm Organic Impurities • Procedure 1 Mobile phase and System suitability solution: Proceed as directed in the Assay. Standard solution: 1.0 μg/mL of USP Rivastigmine Tartrate RS in Mobile phase Sample solution: 1.0 mg/mL of Rivastigmine Tartrate in Mobile phase Chromatographic system: Proceed as directed in the Assay. (See Chromatography 621 , System Suitability.) System suitability Samples: System suitability solution and Standard solution Suitability requirements Resolution: NLT 1.5 between rivastigmine related compound A and rivastigmine related compound B, System suitability solution Relative standard deviation: NMT 10%, Standard solution Analysis [Note— The run time is 8 times the retention time of the rivastigmine peak. ] Samples: Standard solution and Sample solution Calculate the percentage of any individual impurity in the portion of Rivastigmine Tartrate taken: Result = (rU /rS ) × (CS /CU ) × (1/F) × 100 rU = = peak response for each impurity from the Sample solution rS = = peak response from the Standard solution CS = = concentration of USP Rivastigmine Tartrate RS in the Standard solution (mg/mL) CU = = concentration of Rivastigmine Tartrate in the Sample solution (mg/mL) F = = relative response factor (see Impurity Table 1) Acceptance criteria Individual impurities: See Impurity Table 1. Total impurities: NMT 0.5% Impurity Table 1 Name Relative Retention Time Relative Response Factor Acceptance Criteria, NMT (%) Tartrate 0.18 — Disregard Phenol impuritya 0.28 1.6 0.3 DPTTAb 0.46 0.83 0.15 Nor impurityc 0.57 1.2 0.15 Rivastigmine 1.0 1.0 — Carbamate impurityd 4.1 1.3 0.15 Ether impuritye 6.5 1.4 0.15 Any other impurity — 1.0 0.1 a (S)-3-[1-(Dimethylamino)ethyl]phenol. b (+)-Di-(p-toluoyl)-d-tartaric acid (rivastigmine related compound A). c (S)-3-[1-(Dimethylamino)ethyl]phenyl dimethylcarbamate (rivastigmine related compound B). d 3-Nitrophenyl ethyl(methyl)carbamate. e (S)-N,N-Dimethyl-1-[3-(4-nitrophenoxy)phenyl]ethanamine. • Procedure 2: Enantiomeric Purity Buffer: Transfer 1.78 g of dibasic sodium phosphate dihydrate and 1.38 g of monobasic sodium phosphate into a 1000-mL volumetric flask. Dissolve in and dilute with water to volume. Adjust with phosphoric acid to a pH of 6.0. Mobile phase: Transfer 20 mL of acetonitrile and 205 μL of N,N-dimethyloctylamine to a 1000-mL volumetric flask, and dilute with Buffer to volume. Standard solution: 0.1 μg/mL of USP Rivastigmine Tartrate R-Isomer RS in Mobile phase Sensitivity solution: 0.05 μg/mL of USP Rivastigmine Tartrate R-Isomer RS in Mobile phase, Standard solution System suitability solution: 100 μg/mL of USP Rivastigmine Tartrate RS and 0.1 μg/mL of USP Rivastigmine Tartrate R-Isomer RS in Mobile phase Sample solution: 100 μg/mL of Rivastigmine Tartrate in Mobile phase Chromatographic system (See Chromatography 621 , System Suitability.) Mode: LC Detector: UV 200 nm Column: 4.0-mm × 10-cm; packing L41 Flow rate: 0.5 mL/min Injection size: 20 μL System suitability Samples: Standard solution, Sensitivity solution, and System suitability solution Suitability requirements Resolution: NLT 0.8 between the enantiomer peaks, System suitability solution [Note— The elution order is the R-enantiomer, followed by the rivastigmine peak, which is the S-enantiomer. ] Signal-to-noise ratio: NLT 10, Sensitivity solution Relative standard deviation: NMT 10%, Standard solution Analysis Samples: Standard solution and Sample solution Calculate the percentage of the R-enantiomer in the portion of Rivastigmine Tartrate taken: Result = (rU /rS ) × (CS /CU ) × 100 rU = = peak response of R-enantiomer from the Sample solution rS = = peak response of R-enantiomer from the Standard solution CS = = concentration of R-enantiomer in the Standard solution (μg/mL) CU = = concentration of Rivastigmine Tartrate in the Sample solution (μg/mL) Acceptance criteria: NMT 0.3% of the R-enantiomer SPECIFIC TESTS • Water Determination, Method Ia 921 : NMT 0.5% ADDITIONAL REQUIREMENTS • Packaging and Storage: Preserve in tight containers, and store at room temperature. • USP Reference Standards 11 USP Rivastigmine Tartrate RS USP Rivastigmine Related Compound A RS Di-p-toluoyl-d-(+)-tartaric acid monohydrate. C20H20O9 404.37 USP Rivastigmine Related Compound B RS N,N-Dimethylcarbamic acid-3-[1-(dimethylamino)ethyl]phenyl ester. C13H20N2O2 236.32 USP Rivastigmine Tartrate R-Isomer RS |
2楼2012-08-31 17:11:47
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