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cherry8505铜虫 (小有名气)
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[求助]
求助Rabeprazole Sodium delayed-release Tablets国外药典标准
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| 求助Rabeprazole Sodium delayed-release Tablets国外药典标准，USP\EP\BP都可以，感激不尽。 |
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河边的芦苇: 金币+1, 感谢回帖交流 2013-10-01 09:13:01
cherry8505: 金币+3, ★有帮助, 很有用的信息，感谢！ 2013-10-08 10:55:31
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河边的芦苇: 金币+1, 感谢回帖交流 2013-10-01 09:13:01
cherry8505: 金币+3, ★有帮助, 很有用的信息，感谢！ 2013-10-08 10:55:31
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2013-09-29 12:12:40, 26 K
6楼2013-09-29 12:13:00
【答案】应助回帖
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cherry8505: 金币+10, ★★★很有帮助, 非常感谢，请问是说这个品种目前还没收录USP，这个只是征求意见稿吗？ 2013-09-28 09:43:06
感谢参与，应助指数 +1
cherry8505: 金币+10, ★★★很有帮助, 非常感谢，请问是说这个品种目前还没收录USP，这个只是征求意见稿吗？ 2013-09-28 09:43:06
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Rabeprazole Sodium Delayed-Release Tablets. Because there is no existing USP monograph for this dosage form, a new monograph based on validated methods of analysis is proposed. The HPLC procedures in the Assay is based on analyses performed with the Nucleosil C18 brand of L1 column. The typical retention time of rabeprazole is about 5 min. The HPLC procedure in the test for Organic Impurities is based on analyses performed with the YMC-Pak Pro C18 brand of L1 column. The typical retention time of rabeprazole is about 17.5 min. (SM3: E. Gonikberg, L. Santos, M. Marques.) Correspondence Number—C90062 Comment deadline: May 31, 2012 Add the following: Rabeprazole Sodium Delayed-Release Tablets DEFINITION Rabeprazole Sodium Delayed-Release Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of rabeprazole sodium (C18H20N3NaO3S). IDENTIFICATION • A. Ultraviolet Absorption Sample stock solution: Transfer one Tablet to a 100-mL volumetric flask, add 60 mL of 0.05 N sodium hydroxide, and sonicate at a temperature not exceeding 5 for 30 min. Dilute with 0.05 N sodium hydroxide to volume. Centrifuge a portion at a temperature not exceeding 5 for 10 min, and use a supernatant. Sample solution: 0.01 mg/mL of rabeprazole sodium in 0.05 N sodium hydroxide from the Sample stock solution Blank: 0.05 N sodium hydroxide Analysis: Using a 1-cm quartz cuvette, record the UV spectrum between 220 and 350 nm. Acceptance criteria: The spectrum of the Sample solution exhibits maximum between 289 and 293 nm. • B. The retention time of major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay. ASSAY • Procedure [ Note— Avoid exposure of the samples to moisture. Keep all solutions containing rabeprazole sodium at a temperature not exceeding 15. ] Buffer: 50 mM monobasic potassium phosphate and 50 mM dibasic sodium phosphate (40:60). Adjust to a pH of 7.0 by adding a small volume of either solution as necessary. Diluent: Methanol and 0.05 N sodium hydroxide (60:40) Mobile phase: Methanol and Buffer (60:40) Standard solution: 0.1 mg/mL of USP Rabeprazole Sodium RS in Diluent. [ Note— This solution is stable for 48 h when stored at a temperature not exceeding 15. ] Sample stock solution: Transfer a quantity of Tablets equivalent to 100 mg of rabeprazole sodium (based on the label claim) to a 100-mL volumetric flask, add 30 mL of 0.05 N sodium hydroxide, and sonicate at a temperature not exceeding 5 for 30 min, until Tablets are completely disintegrated. Add 45 mL of methanol, and allow the solution to equilibrate at room temperature. Dilute with Diluent to volume, and stir the solution for 10 min. Centrifuge a portion at a temperature not exceeding 15 for 10 min, and use the supernatant. [ Note— This solution is stable for 48 h when stored at a temperature not exceeding 15. ] Sample solution: 0.1 mg/mL of rabeprazole sodium in Diluent from the Sample stock solution Chromatographic system (See Chromatography 621 , System Suitability.) Mode: LC Detector: UV 290 nm Column: 4.6-mm × 15-cm; 5-µm packing L1 Temperatures Column: 30 Sample: Not exceeding 15 Flow rate: 1 mL/min Injection volume: 10 µL System suitability Sample: Standard solution Suitability requirements Resolution: NLT 2.0 between rabeprazole related compound D and rabeprazole [ Note— USP Rabeprazole Sodium RS contains rabeprazole related compound D as a minor component. The relative retention times for rabeprazole related compound D and rabeprazole are 0.7 and 1.0, respectively. ] Tailing factor: NMT 2.0 for rabeprazole Relative standard deviation: NMT 1.0% for rabeprazole Analysis Samples: Standard solution and Sample solution Calculate the percentage of the labeled amount of rabeprazole sodium (C18H20N3NaO3S) in the portion of Tablets taken: Result = ( r U / r S ) × ( C S / C U ) × 100 r U = peak response of rabeprazole from the Sample solution r S = peak response of rabeprazole from the Standard solution C S = concentration of USP Rabeprazole Sodium RS in the Standard solution (mg/mL) C U = nominal concentration of rabeprazole sodium in the Sample solution (mg/mL) Acceptance criteria: 90.0%–110.0% PERFORMANCE TESTS • Dissolution 711 [ Note— Avoid exposure of the samples to moisture. ] 0.6 M Tris buffer: 69.05 g/L of tris(hydroxymethyl)aminomethane in water Acid stage medium: 0.1 N hydrochloric acid; 700 mL Buffer stage medium: After 2 h, add 300 mL of 0.6 M Tris buffer, and adjust with 2 N hydrochloric acid or 2 N sodium hydroxide to a pH of 8.0 ± 0.05. Apparatus 2: 100 rpm Time: 2 h for Acid stage, and 30 min for Buffer stage Diluent, Buffer, Mobile phase, and Chromatographic system: Proceed as directed in the Assay. • Acid Stage Acid stage standard solution: 0.2 mg/mL of USP Rabeprazole Sodium RS in Diluent. [ Note— Keep at a temperature not exceeding 15. ] Acid stage sample solution: Run the test in Acid stage medium for 2 h. Transfer the Tablet to a 100-mL volumetric flask. Add 30 mL of 0.05 N sodium hydroxide, and sonicate at a temperature not exceeding 5 for 30 min, until Tablets are completely disintegrated. Add 45 mL of methanol, mix, immediately cool the solution in an ice-water bath, and then allow the solution to equilibrate at room temperature. Dilute with Diluent to volume, and stir the solution for 10 min. Centrifuge a portion at a temperature not exceeding 15 for 10 min, and use the supernatant. [ Note— Keep at a temperature not exceeding 15 prior to analysis. ] System suitability Sample: Acid stage standard solution Suitability requirements Tailing factor: NMT 2.0 for rabeprazole Relative standard deviation: NMT 1.0% for rabeprazole Analysis Samples: Acid stage standard solution and Acid stage sample solution Calculate the percentage of the labeled amount of rabeprazole sodium (C18H20N3NaO3S) dissolved during the Acid stage: Result = [L ( r U / r S ) × ( C S × V)] × 100/L L = label claim (mg/Tablet) r U = peak response from the Acid stage sample solution r S = peak response from the Acid stage standard solution C S = concentration of the Acid stage standard solution V = final volume of the Acid stage sample solution, 100 mL Tolerances: NMT 10% of the labeled amount of rabeprazole sodium (C18H20N3NaO3S) is dissolved. The percentage of the labeled amount of rabeprazole sodium dissolved at the time specified conforms to Acceptance Table 3 in Dissolution 711 . • Buffer Stage Tris-hydrochloric acid buffer: 0.1 N hydrochloric acid and 0.6 M Tris buffer (7:3). Adjust with 2 N hydrochloric acid or 2 N sodium hydroxide to a pH of 8.0. Buffer stage standard solution: Prepare a 0.6 mg/mL solution of USP Rabeprazole Sodium RS in 0.5 N sodium hydroxide. Mix 10.0 mL of this solution with 30.0 mL of Tris-hydrochloric acid buffer. [ Note— Keep at a temperature not exceeding 15. ] Buffer stage sample solution: Run the test in Acid stage medium for 2 h. Stop the paddle, and immediately remove the Tablet. Restart the paddle at 100 rpm. Add 300 mL of Buffer stage medium previously equilibrated at 37.0 ± 0.5 to the Acid stage medium in the vessel. Adjust with 2 N hydrochloric acid or 2 N sodium hydroxide to a pH of 8.0 ± 0.05. Stop the paddle, and add the Tablet to the vessel. Run the test for 30 min. Pass a portion of the solution under test through a suitable filter. Mix 3.0 mL of the filtrate with 1.0 mL of 0.5 N sodium hydroxide. [ Note— Keep at a temperature not exceeding 15 prior to analysis. ] System suitability Sample: Buffer stage standard solution Suitability requirements Tailing factor: NMT 2.0 for rabeprazole Relative standard deviation: NMT 1.0% for rabeprazole Analysis Samples: Buffer stage standard solution and Buffer stage sample solution Calculate the percentage of the labeled amount of rabeprazole sodium (C18H20N3NaO3S) dissolved during the Buffer stage: Result = ( r U / r S ) × ( C S /L) × V × 100 r U = peak response from the Buffer stage sample solution r S = peak response from the Buffer stage standard solution C S = concentration of the Buffer stage standard solution L = label claim (mg/Tablet) V = final volume of Buffer stage medium, 1000 mL Tolerances: NLT 75% (Q) of the labeled amount of rabeprazole sodium (C18H20N3NaO3S) is dissolved. The percentage of the labeled amount of rabeprazole sodium dissolved at the time specified conforms to Acceptance Table 4 in Dissolution 711 . • Uniformity of Dosage Units 905 : Meet the requirements IMPURITIES • Organic Impurities [ Note— Avoid exposure of the samples to moisture. Keep all solutions containing rabeprazole sodium at 5 ± 3 during all steps of sample preparation. An ice-water bath should be used when possible to minimize sample degradation. ] Buffer: Water, 0.1 N sodium hydroxide solution, and 0.1 M sodium borate solution (625:255:120). Adjust to a pH of 11.3 with 0.1 N sodium hydroxide or 0.1 M sodium borate as necessary. Diluent: Acetonitrile and Buffer (20:80). [ Note— Keep the Diluent at 5 ± 3 during all steps of sample preparation to minimize sample degradation. ] Ammonium acetate solution: 5 g/L of ammonium acetate in water. [ Note— Filter through a C18 extraction disk if late-eluting interfering peaks appear in the chromatogram. ] Solution A: Acetonitrile and Ammonium acetate solution (5:95) Solution B: Methanol and Ammonium acetate solution (85:15) Mobile phase: See Table 1. Table 1 Time (min) Solution A (%) Solution B (%) 0.0 100 0 20.0 0 100 22.0 0 100 22.1 100 0 30.0 100 0 Standard solution: 0.25 mg/mL of USP Rabeprazole Sodium RS in Diluent Peak identification solution: 2.5 µg/mL each of USP Rabeprazole Sodium RS, USP Rabeprazole Related Compound A RS, USP Rabeprazole Related Compound C RS, USP Rabeprazole Related Compound D RS, and USP Rabeprazole Related Compound E RS in Diluent. [ Note— Store this solution in the freezer. Before use, defrost it at 2 –8, and shake well. ] Sample stock solution: Crush a quantity of Tablets equivalent to 100 mg of rabeprazole sodium (based on the label claim), and transfer the crushed Tablets to a 100-mL volumetric flask. Add 60 mL of Diluent, swirl to mix, dilute with Diluent to volume, and shake to mix. Sonicate the solution at 5 ± 3 for 10 min. Centrifuge a portion at a temperature not exceeding 5 for 10 min, and use a supernatant. Sample solution: 0.25 mg/mL of rabeprazole sodium in Diluent from the Sample stock solution Chromatographic system (See Chromatography 621 , System Suitability.) Mode: LC Detector: UV 290 nm Column: 4.6-mm × 15-cm; 5-µm packing L1 Temperatures Column: 35 Autosampler: Not exceeding 5 Flow rate: 1 mL/min Injection volume: 10 µL System suitability Samples: Standard solution and Peak identification solution Suitability requirements Resolution: NLT 1.5 between rabeprazole related compound D and rabeprazole, Peak identification solution Tailing factor: NMT 2.0 for rabeprazole, Standard solution Relative standard deviation: NMT 1.0% for rabeprazole, Standard solution Analysis Sample: Sample solution Calculate the percentage of each impurity in the portion of Tablets taken: Result = ( r U / r T ) × (1/F) × 100 r U = peak response of each impurity r T = sum of all the peak responses, each divided by the corresponding value of the relative response factor from Table 2 F = relative response factor (see Table 2) Acceptance criteria: See Table 2. Table 2 Name Relative Retention Time Relative Response Factor Acceptance Criteria, NMT (%) Rabeprazole picolinic ether analog (rabeprazole related compound A)a 0.38 2.7 0.2 Rabeprazole picolinium saltb 0.49 0.65 0.5 Mercaptobenzimidazole (rabeprazole related compound C)c 0.56 3.8 0.2 Rabeprazole sulfone analog (rabeprazole related compound D)d 0.97 0.90 1.0 Rabeprazole 1.00 — — Rabeprazole sulfide analog (rabeprazole related compound E)e 1.13 1.3 0.2 Any unspecified impurity — 1.0 0.2 Total impurities — — 1.8 a 4-(1H -Benzimidazol-2-yloxy)-3-methylpicolinic acid. b 1-(1H -Benzimidazol-2-yl)-4-(3-methoxypropoxy)-3-methylpyridinium-2-carboxylate. c 1H -Benzimidazole-2-thiol. d 2-[[[4-(3-Methoxypropoxy)-3-methyl-2-pyridyl]methyl]sulfonyl]benzimidazole. e 2-[[4-(3-Methoxypropoxy)-3-methyl-2-pyridyl]methylthio]benzimidazole. ADDITIONAL REQUIREMENTS • Packaging and Storage: Preserve in tight containers. Store at controlled room temperature. • USP Reference Standards 11 USP Rabeprazole Sodium RS USP Rabeprazole Related Compound A RS 4-(1H -Benzimidazol-2-yloxy)-3-methylpicolinic acid, sodium salt. C14H10N3NaO3 291.24 USP Rabeprazole Related Compound C RS 1H -Benzimidazole-2-thiol. C7H6N2S 150.20 USP Rabeprazole Related Compound D RS 2-[[[4-(3-Methoxypropoxy)-3-methyl-2-pyridyl]methyl]sulfonyl]benzimidazole. C18H21N3O4S 375.44 USP Rabeprazole Related Compound E RS 2-[[4-(3-Methoxypropoxy)-3-methyl-2-pyridyl]methylthio]benzimidazole. C18H21N3O2S 343.44 |
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