USP34–NF29Stavudinecapsules.doc

Stavudine Capsules(司他夫定胶囊) Stavudine Capsules contain not less than 90.0 percent and not more than 105.0 percent of the labeled amount of stavudine (C10H12N2O4).司他夫定胶囊应含司他夫定(C10H12N2O4)在90%-105%.Packaging and storage Preserve in tightly closed containers, and store at controlled room temperature. 包装和贮存：保存在密闭容器中，和可控制温度处。USP Reference standards 11 USP Stavudine RS. 参考标准：美国药典司他夫定的标准品Identification 鉴别：A: Thin-Layer Chromatographic Identification Test 201 A: 薄层色谱鉴别实验 Test solution Using sonication, dissolve a portion of Capsule contents in enough water to obtain a solution having a concentration of 0.2 mg of stavudine per mL, filter, and mix. Use the filtrate as the Test solution. 试验方案：取胶囊内容物溶于水中，使溶液浓度为0.2mg/ml，超声，过滤。滤液作为供试品溶液。Application volume: 10 L, applied in two 5-L portions. 用量：共10L，取两个平行，每个5L。Developing solvent system: a mixture of chloroform, alcohol, and water (100:50:2). 溶剂配制：氯仿、酒精、和水的混合物（比例为：100:50:2）。Procedure Proceed as directed in the chapter. Allow the spots to dry, and develop the chromatogram in the Developing solvent system until the solvent front has moved about 10 cm from the origin. Remove the plate from the developing chamber, mark the solvent front, and allow to air dry for 5 to 10 minutes. 步骤：程序，在本章的指示进行。允许的斑点，干燥，并发展在发展中的溶剂系统的色谱，直到溶剂的前锋已经从10厘米左右的起源。从发展中国家室中取出的钢板，标志的溶剂前沿，并让干燥空气为5至10分钟。B: The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that in the chromatogram of the Standard preparation, as obtained in the Assay. B：色谱含量准备的主要峰的保留时间相对应的是在标准编制的色谱，如在检测中获得。Specific rotation 781S: between 40 and 45, determined in a solution in water containing 10 mg of stavudine per mL. Disperse a sufficient quantity of Capsule content, equivalent to 200 mg of stavudine, in 50 mL of acetone. Bring to a boil, and pass through a fine-porosity filter. Precipitate the stavudine with 150 mL of heptane, filter the crystals, wash with heptane, and dry in air. 比旋度 ： 40 和 45之间，在一个解决方案，在含10毫克每毫升司他夫定的水确定。分散胶囊内容的足够数量，相当于200毫克的司他夫定在50 mL丙酮。烧开，并通过罚款孔隙过滤器。沉淀用150毫升的正庚烷司他夫定，晶体滤波器，用庚，并在空气干燥。Dissolution 711 溶散Medium: water; 900 mL. 介质：水，900 mLApparatus 2: 75 rpm. 仪器：Time: 30 minutes. 时间：Determine the amount of C10H12N2O4 dissolved by employing the following method.采用以下方法测定含量（C10H12N2O4 ） 0.01 M Ammonium acetate and Mobile phase Prepare as directed in the Assay. 0.01 M醋酸铵和流动相：作为含量分析的准备Standard solution Dissolve an accurately weighed quantity of USP Stavudine RS in water, and dilute quantitatively, and stepwise if necessary, with water to obtain a solution having a known concentration corresponding to that of the solution under test. 标准溶液-准确称量司他夫定标准品（USP），溶解于水中，并定量稀释，以获得相应的已知浓度的待测溶液。Chromatographic system (see Chromatography 621) Proceed as directed in the Assay except that the liquid chromatograph is equipped with a 254-nm detector. Chromatograph the Standard solution, and record the peak responses as directed for Procedure: the column efficiency is not less than 800 theoretical plates; the tailing factor is not more than 2; and the relative standard deviation for replicate injections is not more than 2.0%. 色谱系统（见色谱 ） - 继续除外，液相色谱仪配备一个254纳米探测器检测的指示。色谱标准溶液，并记录为程序的指示，峰值响应：柱效理论塔板数不低于800，拖尾因子不超过2个;和重复进样的相对标准偏差不超过2.0。Procedure Determine the amount of C10H12N2O4 dissolved, employing the procedure set forth in the Assay, making any necessary modifications. The injection volume is about 10 L. 程序确定C10H12N2O4量溶解，用人检测规定的程序，作出必要的修改。注射量是大约10L。Tolerances Not less than 80% (Q) of the labeled amount of C10H12N2O4 is dissolved in 30 minutes. 公差不低于80的C10H12N2O4标示量（Q）是在30分钟内溶解。Uniformity of dosage units 905: meet the requirements. 均匀的剂量单位Water, Method I 921: not more than 3.5%. Related compounds 相关化合物0.01 M Ammonium acetate and Mobile phase Prepare as directed in the Assay. 0.01 M醋酸铵和流动相：为含量分析的作准备Resolution solution Proceed as directed in the Assay. 分离度-含量的测定Standard solution Using sonication, dissolve an accurately weighed quantity of thymine in water, and dilute quantitatively, and stepwise if necessary, with water, to obtain a solution having a known concentration of about 1 g per mL. 标准溶液-准确称量胸腺嘧啶,溶于水中,并使用超声波溶解，配制成约1微克每毫升已知浓度的溶液。Test solution Use the Assay preparation. 测试溶液为分析作准备。Chromatographic system Proceed as directed in the Assay. The relative standard deviation for replicate injections of the Standard solution is not more than 3.0%. 色谱系统含量的测定。标准溶液重复进样的相对标准偏差不超过3.0。Procedure Proceed as directed in the Assay, recording the chromatograms for a period of time that is 2.5 times the retention time of stavudine, and measure the responses of all the peaks. Calculate the quantity of thymine in each Capsule taken by the formula: (CVD/N)(rU / rS),步骤含量测定，司他夫定的保留时间是2.5倍的时间内记录色谱图，测量所有峰的反应。计算公式所采取的每一个胶囊数量胸腺嘧啶：(CVD/N) (rU / rS),in which C is the concentration, in mg per mL, of the Standard solution; V is the volume, in mL, used to prepare the Test solution; D is the dilution factor of the Test solution; N is the number of Capsules taken to prepare the Test solution; and rU and rS are the peak responses obtained from the Test solution and the Standard solution, respectively. Not more than 1.0% of thymine is found. Calculate the percentage of unknown impurities, not including thymine, in the portion of Capsules taken by the formula: C标准溶液的浓度（mg / mL） V测试溶液的体积，D供试溶液的稀释倍数， N制备供试液的胶囊数量，rU供试溶液的峰面积， rS标准溶液的峰面积，100(ri / rs),ri杂质的峰面积，rs所有峰的峰面积的总和in which ri is the peak response for each impurity; and rs is the sum of the responses of all the peaks: not more than 0.2% of any individual impurity is found; and not more than 2.0% of total impurities, including thymine, is found. The quantitation limit is 0.05% of the total sample related peak response. 任何个人的杂质不超过0.2;总杂质不超过2.0。胸腺嘧啶定量检测限为0.05。Assay NOTEAll solutions must be prepared immediately prior to use and remain refrigerated until use. 注意所有溶液都必须在临用前配制或保藏于冷藏。0.01 M Ammonium acetate Dissolve 0.77 g of ammonium acetate in about 900 mL of water in a 1000-mL volumetric flask. Dilute with water to volume, and mix. 0.01 M醋酸铵称取0.77 g 醋酸铵在1000 mL容量瓶中，加900ml水 溶解约。 再用水稀释至刻度，并充分混合。Mobile phase Prepare a filtered and degassed mixture of 0.01 M Ammonium acetate and acetonitrile (95:5). 流动相0.01 M醋酸铵和乙腈混合（95:5）过滤和脱气。Resolution solution Dissolve accurately weighed quantities of thymine and thymidine in water, and dilute quantitatively, and stepwise if necessary, with water to obtain a solution having a known concentration of 0.1 g per mL of each component per mL. 分离度准确称量一定数量胸腺嘧啶和胸苷，分别溶解于水中，并定量稀释，分别制成0.1微克每毫升每毫升的已知浓度。Standard preparation Using sonication,dissolve an accurately weighed quantity of USP Stavudine RS in water, and dilute quantitatively,and stepwise if necessary,with water to obtain a solution having a concentration of about 0.1 mg per mL. 标准溶液准确称量的一定数量的司他夫定标准品，溶解于水，并超声。配制成浓度为0.1毫克每毫升的溶液。Assay preparation Open not fewer than 3 Capsules, and dissolve the contents quantitatively in water. Dilute quantitatively, and stepwise if necessary, with water, to obtain a solution having a concentration of about 0.1 mg of stavudine per mL. 供试液制备打开不少于3个的胶囊，用一定量的水溶解的胶囊的内溶物。定量稀释，制成浓度约为0.1毫克每毫升司他夫定的溶液。Chromatographic system (see Chromatography 621) The liquid chromatograph is equipped with a 268-nm detector and a 4.6-mm 3.3-cm column that contains packing L1. The flow rate is about 0.7 mL per minute. Chromatograph the Resolution solution, and record the peak responses as directed for Procedure: the resolution, R, between thymine and thymidine is not less than 2.0, and thymine is resolved from the void volume. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the retention time for the stavudine peak is between 2.8 and 5.0 minutes; the column efficiency is not less than 800 theoretical plates; the tailing factor is not more than 1.8; and the relative standard deviation for replicate injections is not more than 2.0%. 色谱系统（参考色谱 ）液相色谱仪，270nm检测波长，4.6mm*3.3 cm色谱柱（填料L1），其中包含包装的L1。流速是每分钟约0.7毫升。色谱仪的分辨率的解决方案，并记录为程序的指示，峰值响应的决议，研究胸腺嘧啶和胸腺嘧啶之间，不小于2.0，而胸腺嘧啶是从空隙体积解决。色谱标准编制，并记录峰值响应，为程序的指示：司他夫定峰的保留时间是2.8和5.0分钟之间;，柱效理论塔板数不低于800，拖尾因子不超过1.8;重复进样的相对标准偏差不超过2.0。Procedure Separately inject equal volumes (about 20 L) of the