复方益母口服液中水溶性生物碱盐酸水苏碱HPLC法测定研究.docVIP

复方益母口服液中水溶性生物碱盐酸水苏碱HPLC法测定研究 　　[摘要] 目的 建立复方益母口服液中水溶性生物碱-盐酸水苏碱的含量测定方法。 方法 用雷氏盐沉淀法处理样品，对提纯出的盐酸水苏碱采用HPLC法测定含量。色谱柱为Agela Venusil XBP NH2柱（4.6 mm×250 mm，5 μm），以乙腈-醋酸溶液（用少量醋酸调节溶液的pH值至3.00±0.15）（77∶23）为流动相，流速为1.0 mL/min，柱温为35℃，检测波长200 nm。 结果 复方益母口服液中盐酸水苏碱的进样量在1.083 1～32.491 8 μg范围内线性关系良好（r = 0.999 9），平均回收率为91.1%，RSD = 3.7%（n = 6）。 结论 该方法精确可靠，专属性强，可作为复方益母口服液中盐酸水苏碱的质量控制方法。 　　[关键词] 复方益母口服液；HPLC法；盐酸水苏碱；雷氏盐沉淀法 　　[中图分类号] R927.2 [文献标识码] A [文章编号] 1674-4721（2012）06（a）-0063-03 　　Determination of water soluble alkaloids-stachydrine hydrochloride in Complex Yimu Oral Liquid by HPLC 　　LV Haihong 　　Institute for Food and Drug Control of Henan Province, Zhengzhou 450003, China 　　[Abstract] Objective To establish a method for the content determination of water soluble alkaloids-stachydrine hydrochloride in Complex Yimu Oral Liquid. Methods The sample solution was prepared with the method of Reinecke salt precipitation and was determined the content by HPLC. The column was Agela Venusil XBP NH2 column (4.6 mm×250 mm，5 μm) and CH3CN-H2O (pH was adjusted to 3.00±0.15 by acetic acid) (77∶23) was used as the mobile phase, with the flow rate of 1.0 mL/min. The column temperature was at 35℃ and the detection wavelength was 200 nm. Results The good linear ranges were between 1.083 1-32.491 8 μg for stachydrine hydrochloride (r = 0.999 9, n = 6) and the average rate of recovery was 91.1% with RSD = 3.7% (n = 6). Conclusion The method is accurate, reliable, specific and with good reproducibility. It can be used for the quality control of stachydrine hydrochloride in Complex Yimu Oral Liquid. 　　[Key words] Complex Yimｕ Ｏｒａｌ Liquid; Stachydrine hydrochloride; HPLC; Reinecke salt precipitation 　　复方益母口服液是由益母草、当归、川芎等药经加工制成的口服液，具有活血行气，化瘀止痛的功能，用于气滞血瘀所致的痛经，原为国家药品标准新药转正标准第19册收载品种[1]。益母草是君药，其指标性成分是盐酸水苏碱，原标准采用薄层扫描法（TLCS）测定水苏碱含量，由于方剂中并存其他的生物碱，TLCS法对水苏碱的选择性和专属性均差，含量不准确。为此，特研究起草了HPLC法测定复方益母口服液中盐酸水苏碱的含量，专属性强，准确性好，可为标准提高提供修订依据。 　　1 仪器与试药 　　戴安高效液相色谱仪UltiMate3000系列。盐酸水苏碱对照品（中国药品生物制品检定所，批号：110712-200709，供含量测定用）；复方益