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wonboy木虫 (著名写手)
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[求助]
求助USP35 S2 quetiapine fumarate
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【答案】应助回帖
★ ★ ★ ★ ★ ★ ★
感谢参与，应助指数 +1
痴夷子皮: 金币+2, 正解，欢迎常来哦。 2013-04-01 09:53:45
wonboy: 金币+5, ★有帮助, 貌似JP16的S1和印度药典2010版有收录，不过都没办法查到 2013-04-01 19:42:09
感谢参与，应助指数 +1
痴夷子皮: 金币+2, 正解，欢迎常来哦。 2013-04-01 09:53:45
wonboy: 金币+5, ★有帮助, 貌似JP16的S1和印度药典2010版有收录，不过都没办法查到 2013-04-01 19:42:09
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Not official USP-NF text QUETIAPINE FUMARATE PF LGS# Brand Type of Test Additional Information 37(3) L7 ZORBAX RX-C8 Assay 4.6 mm x 25 cm, 5 µm. 37(3) L7 Symmetry C8 Organic Impurities 3.9 mm x 15 cm, 5 µm. 好像尚未正式出版。 |
2楼2013-04-01 09:50:06
3楼2013-04-01 09:52:46
4楼2013-04-01 11:01:22
wonboy
木虫 (著名写手)
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5楼2013-04-01 12:18:28
【答案】应助回帖
★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★
wonboy: 金币+25, ★★★★★最佳答案, 灰常感谢！貌似JP16的S1和印度药典2010版有收录，不过都没办法查到 2013-04-01 19:42:34
痴夷子皮: 金币+2, 3Q，辛苦了，欢迎常来哦。 2013-04-02 08:27:40
wonboy: 金币+25, ★★★★★最佳答案, 灰常感谢！貌似JP16的S1和印度药典2010版有收录，不过都没办法查到 2013-04-01 19:42:34
痴夷子皮: 金币+2, 3Q，辛苦了，欢迎常来哦。 2013-04-02 08:27:40
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Quetiapine Fumarate (C21H25N3O2S)2 · C4H4O4 883.09 Ethanol, 2-[2-(4-dibenzo[b,f][1,4]thiazepin-11-yl-1-piperazinyl)ethoxy]-, (E)-2-butenedioate (2:1) (salt); 2-[2-(4-Dibenzo[b,f][1,4]thiazepin-11-yl-1-piperazinyl)ethoxy]ethanol fumarate (2:1) salt [111974-72-2.]. DEFINITION Quetiapine Fumarate contains NLT 98.0% and NMT 102.0% of (C21H25N3O2S)2 · C4H4O4 , calculated on the dried basis. IDENTIFICATION • A. Infrared Absorption 197K • 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: 2.6 g/L of dibasic ammonium phosphate. Adjust with phosphoric acid to a pH of 6.5. Mobile phase: Methanol, acetonitrile, and Buffer (54:7:39) System suitability solution: 1.0 mg/mL of USP Quetiapine System Suitability RS in Mobile phase Standard solution: 0.08 mg/mL of USP Quetiapine Fumarate RS in Mobile phase Sample solution: 0.08 mg/mL of Quetiapine Fumarate in Mobile phase Chromatographic system (See Chromatography 621 , System Suitability.) Mode: LC Detector: UV 230 nm Column: 4.6-mm × 25-cm; 5-µm packing L7 Flow rate: 1.3 mL/min Injection size: 50 µL System suitability Samples: System suitability solution and Standard solution [ NOTE— The relative retention times for quetiapine impurity I and quetiapine are about 0.9 and 1.0, respectively. ] Suitability requirements Resolution: NLT 1.5 between the quetiapine impurity I and quetiapine peaks, System suitability solution Tailing factor: NMT 2.0 for the quetiapine peak, Standard solution Relative standard deviation: NMT 2.0%, Standard soluion Analysis Samples: Standard solution and Sample solution Calculate the percentage of quetiapine fumarate ((C21H25N3O2S)2 · C4H4O4 ) in the portion of Quetiapine Fumarate taken: Result = ( r U / r S ) × ( C S / C U ) × 100 r U = peak response from the Sample solution r S = peak response from the Standard solution C S = concentration of USP Quetiapine Fumarate RS in the Standard solution (mg/mL) C U = concentration of Quetiapine Fumarate in the Sample solution (mg/mL) Acceptance criteria: 98.0%–102.0% on the dried basis OTHER COMPONENTS • Content of Fumaric Acid Sample: 200 mg of Quetiapine Fumarate Titrimetric system (See Titrimetry 541 .) Mode: Direct titration Titrant: 0.1 N tetrabutylammonium hydroxide in methanol/isopropyl alcohol VS Endpoint detection: Potentiometric Blank: 50 mL of dimethylformamide Analysis: Dissolve the Sample in 50 mL of dimethylformamide, and titrate with 0.1 N tetrabutylammonium hydroxide in methanol/isopropyl alcohol VS. Calculate the percentage of fumaric acid (C4H4O4 ) in the portion of the Quetiapine Fumarate taken: Result = [(V B) × N × F × 100]/W V = volume of titrant needed for the Sample (mL) B = volume of titrant needed for the Blank (mL) N = titrant normality (mEq/mL) F = equivalency factor for fumaric acid, 116.07 mg/mEq W = weight of the Sample (mg) Acceptance criteria: 13.0%–13.3% on the dried basis IMPURITIES • Residue on Ignition 281 : NMT 0.1% • Heavy Metals, Method II 231 : NMT 20 ppm • Organic Impurities Buffer: Dissolve 3.3 g of dibasic ammonium phosphate in 900 mL of water. Adjust with phosphoric acid to a pH of 7.0. Dilute with water to 1 L. Solvent mixture: Acetonitrile and methanol (67:33) Solution A: Solvent mixture and Buffer (41:59) Solution B: Solvent mixture and water (80:20) Mobile phase: See Table 1. Return to original conditions, and requilibrate the column. Table 1 Time (min) Solution A (%) Solution B (%) 0 90 10 13 90 10 25 10 90 38 10 90 38.1 90 10 50 90 10 System suitability solution: 1 mg/mL of USP Quetiapine System Suitability RS in Solution A Standard solution: 1 µg/mL of USP Quetiapine Fumarate RS in Solution A Sample solution: 1.0 mg/mL of Quetiapine Fumarate in Solution A Chromatographic system (See Chromatography 621 , System Suitability.) Mode: LC Detector: UV 240 nm Column: 3.9-mm × 15-cm; 5-µm packing L7 Flow rate: 1 mL/min Injection size: 20 µL System suitability Samples: System suitability solution and Standard solution Suitability requirements Resolution: NLT 2.0 between the quetiapine impurity I and quetiapine peaks, System suitability solution Tailing factor: NMT 2.0 for the quetiapine peak, Standard solution Relative standard deviation: NMT 5.0%, Standard solution Analysis Samples: Standard solution and Sample solution Calculate the percentage of any individual impurity in the portion of Quetiapine Fumarate taken: Result = ( r U / r S ) × ( C S / C U ) × (1/F) 100 r U = peak response for each impurity from the Sample solution r S = peak response for quetiapine from the Standard solution C S = concentration of USP Quetiapine Fumarate RS in the Standard solution (mg/mL) C U = concentration of Quetiapine Fumarate in the Sample solution (mg/mL) F = relative response factor (see Table 2) [ NOTE— Disregard if the limit is less than 0.05%. ] Acceptance criteria: See Table 2. Table 2 Name Relative Retention Time Relative Response Factor Acceptance Criteria, NMT (%) Quetiapine impurity Ba 0.5–0.8 1.7 0.15 Quetiapine impurity Gb 0.6 1.7 0.15 Quetiapine impurity Ic 0.9 1.0 0.15 Quetiapine 1.0 — — Any other unknown individual impurity — — 0.10 Total impurities — — 0.3 a 11-(Piperazin-1-yl)dibenzo[b,f][1,4]thiazepine. b Dibenzo[b,f][1,4]thiazepin-11(10H )-one. c 2-[4-(Dibenzo[b,f][1,4]thiazepin-11-yl)piperazin-1-yl]ethanol. SPECIFIC TESTS • Loss on Drying 731 : Dry a sample to constant weight at 105: it loses NMT 0.5% of its weight. ADDITIONAL REQUIREMENTS • Packaging and Storage: Preserve in well-closed containers, protected from light. Store at room temperature. • USP Reference Standards 11 USP Quetiapine Fumarate RS USP Quetiapine System Suitability RS It contains more than 98% of quetiapine fumarate and each of the following impurities:quetiapine impurity B: 11-(piperazin-1-yl)dibenzo[b,f][1,4]thiazepine; quetiapine impurity G: dibenzo[b,f][1,4]thiazepin-11(10H )-one; and quetiapine impurity I: 2-[4-(dibenzo[b,f][1,4]thiazepin-11-yl)piperazin-1-yl]ethanol. 1S (USP35) |
6楼2013-04-01 13:46:49
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anemone1982
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9楼2013-04-01 14:04:19
