HPLC法测定湿热痹片中盐酸小檗碱含量.doc

HPLC法测定湿热痹片中盐酸小檗碱含量[摘要] 目的:建立测定湿热痹片中盐酸小檗碱含量的HPLC法。方法:采用高效液相色谱法对湿热痹片中的盐酸小檗碱进行含量测定,色谱柱为迪马Diamonsil(TM)钻石 C18柱(4.6 mm×250 mm,5 μm),流动相为乙腈-1%磷酸溶液(48∶52,每100 毫升中加入十二烷基磺酸钠0.1 g),流速为1.0 ml/min,检测波长为265 nm,柱温为25℃,进样量为10 μl。结果:盐酸小檗碱在0.018 6～0.372 0 μg范围内线性关系良好,r=0.999 9;平均回收率为100.14%,RSD为1.35%。结论:本法操作简便、准确、重现性好,可用于湿热痹片的质量控制。 [关键词] 湿热痹片;盐酸小檗碱;高效液相色谱法;含量测定 [中图分类号]R927.2 [文献标识码]A [文章编号]1673-7210(2009)08(b)-052-03 Determination of berberine hydrochlorde in Shirebi Tablets by HPLC JIN Fenghuan1, DUAN Yanjie2 (1.Benxi Chemical Industry School, Benxi117000, China; 2.Beijing Greatwall International Cancer Center, the Second Affiliated Hospital of PLA Gerneral Hospital, Beijing100091, China) [Abstract] Objective: To establish a HPLC method to determine berberine hydrochlorde in Shirebi Tablets. Methods: The contents of berberine hydrochlorde were determined in Shirebi Tablets by HPLC. A Diamonsil(TM) C18 chromatographic column(4.6 mm×250 mm, 5 μm) was used, the mobile phase was consisted of acetonitrile-0.1% phosphoric acid solution(48∶52) at the flow rate of 1.0 ml/min, the detection wavelength was 265 nm, the column temperature was 25℃ and the sample volume was 10 μl. Results: The linear range of berberine hydrochlorde was 0.018 6-0.372 0 μg(r=0.999 9), the average recovery was 100.14% with a RSD of 1.35%. Conclusion: The method is easy to operate, and can provide accurate and reproducible results, thus is suitable for the quality control of Shirebi Tablets. [Key words] Shirebi Tablets; HPLC; Berberine hydrochlorde; Determination 湿热痹片由苍术、薏苡仁、地龙、防己、黄柏、粉萆?、防风等十多种中药材组成,具有祛风除湿、清热消肿、通络定痛的功效。用于治疗肌肉或关节红肿热痛、有沉重感、步履艰难、发热、口渴不欲饮、小便黄淡等症。其中,黄柏具有清热燥湿、泻火解毒、退虚热等作用,为方中要药。本文对该方中盐酸小檗碱进行了含量测定,报道如下。 1 仪器与试药 1.1 仪器 Agilent 1100高效液相色谱仪(包括G1379A在线脱气机、G1313A 自动进样器、G1311A四元梯度泵、G1316A柱温箱、G1314A 紫外检测器),岛津UV-2401型紫外分光光度计,恒温水浴锅,PW型超纯水制备器,KQ5200型超声波清洗器(功率 250 W,频率33 kHz)。 1.2 试药 湿热痹片(辽宁好护士集团本溪制药有限公司,批号20060502;盐酸小檗碱对照品(中国药品生物制品检定所,批号为110713-200208,供含量测定用