维生素B1片USP35

维生素B1片USP35 Thiamine Hydrochloride Tablets 维生素B1片 DEFINITION 定义 Thiamine Hydrochloride Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of thiamine hydrochloride (C12H17ClN4OS?HCl). 本品含C12H17ClN4OS?HCl.不少于标示量的90.0%，不多于标示量的 110.0%。 IDENTIFICATION 鉴别 • A. Sample solution: Triturate a quantity of powdered Tablets, equivalent to 10 mg of thiamine hydrochloride, with 10 mL of 0.5 N sodium hydroxide, and filter. 供试品溶液:取本品细粉适 量，相当于含10mg维生素B1，加入10 mL 0.5 N氢氧化钠，过滤。 Analysis: To 5 mL of the Sample solution add 0.5 mL of potassium ferricyanide TS and 5 mL of isobutyl alcohol, shake the mixture vigorously for 2 min, and allow the liquid layers to separate. Illuminate from above by a vertical beam of UV light, and observe the air–liquid meniscus at a right angle to this beam. Acceptance criteria: The air–liquid meniscus shows a vivid blue fluorescence, which disappears when the mixture is slightly acidified, but reappears when it is again made alkaline. 分析:向5 mL供试品溶液中加入0.5 mL铁氰化钾试液和5 mL异丁醇，强力振摇2分钟， 放置使分层。垂直紫外光照射，与光线垂直角度观察弯液面。 可接受:弯液面显深湖蓝色荧光，当混合液稍酸化时，荧光消失，再使成碱性时，荧 光又出现。 • B. Sample solution: Triturate a quantity of powdered Tablets, equivalent to 10 mg of thiamine hydrochloride, with 10 mL of water, and filter. 供试品溶液:取本品粉末适量，相当于含10 mg维生素B1，加水10ml，过滤。 Analysis 1: To 2 mL of the Sample solution add iodine TS. 分析1:向2 mL供试品溶液中加入碘试液。 Acceptance criteria 1: A red-brown precipitate is formed. 可接受标准1:产生红棕色沉淀。 Analysis 2: To 2 mL of the Sample solution add mercuric chloride TS. 分析2:向2 mL供试 品溶液中加入氯化汞试液。 Acceptance criteria 2: A white precipitate is formed. 可接受标准2:产生白色沉淀。 Analysis 3: Identification Tests—General 191, Chloride 分 析3: -一般鉴别试验191氯化物 Acceptance criteria 3: Meet the requirements 可接受标准3:应符合。 • C. Sample solution: Use the remainder of the Sample solution from Identification test B. 供试品溶液:使用鉴别试验B供试品溶液的剩余样品。 Analysis: Add 1 mL of lead acetate TS and 1 mL of 2.5 N sodium hydroxide. 分析:加入1 ml醋酸铅试液和1ml 2.5 N氢氧化钠 Acceptance criteria: A yellow color is produced. Heat the mixture for several min on a steam bath: the color changes to brown, and, on standing, a precipitate of lead sulfide separates. 可接受标准:显黄色。蒸气浴加热几分钟，颜色变为棕色，静置，分离出硫化铅沉淀。 ASSAY 含量测定 • THIAMINE ASSAY 531 维生素B1含量测定531 Assay preparation: Place NLT 20 Tablets in a flask of suitable size, half fill the flask with 0.2 N hydrochloric acid, and heat on a steam bath, with frequent agitation, until the Tablets have dissolved or have disintegrated so that a uniform dispersion is obtained. Cool, transfer the contents of the flask to a volumetric flask, and dilute with 0.2 N hydrochloric acid to volume. If the mixture is not clear, either centrifuge it or filter it through paper known not to adsorb thiamine. Dilute a portion of the clear solution with 0.2 N hydrochloric acid to obtain a 0.2 µg/mL solution of thiamine hydrochloride. 供试品溶液:将本品至少20片放入合适的烧瓶中，加入0.2N盐酸至烧瓶一半，蒸气浴加 热，频繁搅动，直到片剂溶解或崩解，混匀。冷却，将Proceed as directed in the chapter. 分析:依本章指导进行 Acceptance criteria: 90.0%–110.0% 可接受标准:90.0%–110.0%。 PERFORMANCE TESTS 性能试验 • DISSOLUTION, Procedure for a Pooled Sample 711 溶出度:按溶出池中的测定法<711> Medium: Water; 900 mL 溶出介质:水，900ml Apparatus 2: 50 rpm 装置2:50 rpm Time: 45 min 时间:45分钟 Standard solution: A known concentration of USP Thiamine Hydrochloride RS in Medium 对照品溶液:溶出介质中含已知浓度的USP维生素B1对照品。 Sample solution: Filtered portion of the solution under test, suitably diluted with the Medium if necessary 供试品溶液:试验下过滤溶液，如有必要用溶出介质稀释。 Mobile phase: A mixture of methanol, glacial acetic acid, and water (27:1:73) containing 1.40 mg/mL of sodium 1-hexanesulfonate 流动相:甲醇-冰醋酸-水(27:1:73)混合液中约含1.40 mg/mL1-己烷磺酸钠。 Chromatographic system 色谱系统 (See Chromatography 621, System Suitability.) 参见色谱法，系统适应性 Mode: LC 方法:液相色谱法 Detector: UV 280 nm 器:UV 280 nm Column: 3.9-mm × 30-cm; packing L1 色谱柱:3.9-mm × 30-cm; 填充剂 L1 Flow rate: 1 mL/min 流速:1 mL/min Injection size: 10 µL 进样量:10 µL System suitability 系统适应性 Sample: Standard solution 样品:对照品溶液 Suitability requirements 适应性要求 Relative standard deviation: NMT 3.0% 相对标准偏差:不大于3.0% Analysis 分析 Samples: Standard solution and Sample solution 样品:对照品溶液和供试品溶液 Calculate the percentage of the labeled amount of thiamine hydrochloride (C12H17ClN4OS?HCl) dissolved: 计算溶出的维生素B1(C12H17ClN4OS?HCl)标示量的百分含量: Result = (rU/rS) × (CS × D × V/L) × 100 rU rS CS = = peak area of thiamine from the Sample solution 供试品溶液硫胺的峰面积 = = peak area of thiamine from the Standard solution 对对照品溶液中硫胺峰面积 = = concentration of USP Thiamine Hydrochloride RS in the Standard solution (mg/mL) U对照品溶液种USP维生素B1浓度(mg/mL) = = dilution factor for the Sample solution 供试品溶液的稀释因子 = = volume of Medium, 900 mL 溶出介质的体积900 mL = = labeled amount of thiamine hydrochloride (mg/Tablet) 盐酸硫胺的标示量(mg/片) D V L Tolerances: NLT 75% (Q) of the labeled amount of thiamine hydrochloride (C12H17ClN4OS?HCl) is dissolved. 限度- C12H17ClN4OS?HCl的溶出量不得少于标示量的75% (Q)。 • UNIFORMITY OF DOSAGE UNITS 905: Meet the requirements 剂量单位均匀度905:应符合规定。 ADDITIONAL REQUIREMENTS 附加要求 • PACKAGING AND STORAGE: Preserve in tight, light-resistant containers. 包装和储存:遮光，密闭容器包装 • USP REFERENCE STANDARDS 11 USP Thiamine Hydrochloride RS USP对照品<11> USP 盐酸硫胺对照品