五子衍宗丸的质量控制标准研究

 目的 修订五子衍宗丸的质量控制标准,提高其质量控制水平。方法 采用薄层色谱法对处方中枸杞子进行定性鉴别。采用高效液相色谱法,建立基于组合对照药材的五子衍宗丸特征图谱、南五味子检查方法和金丝桃苷、五味子醇甲的含量测定方法。采用ICP-MS,测定了五子衍宗丸中铅、镉、砷、汞、铜、铬的含量。结果 薄层鉴别分离效果好,专属性强。特征图谱提出组合对照药材概念,可同时鉴定制剂中覆盆子、菟丝子、车前子和五味子4味药材,方法学考察结果良好。通过五味子酯甲和五味子醇甲的峰面积比值限度0.20,可快速筛查制剂中是否有混品南五味子投料。在含量测定中,拟定了金丝桃苷和五味子醇甲的含量限度。重金属及有害元素检查中,发现砷、汞、铅3个元素在部分样品中有超标现象,经调研,超标原因可能由不同产品共线生产造成交叉污染所致。结论 本方法简便、准确、专属性强、重现性好,可全面和整体控制五子衍宗丸的质量。

Quality Control Study of Wuziyanzong Pills

OBJECTIVE To establish the quality standard of Wuziyanzong pills so as to improve the quality control capacity. METHODS Thin-layer chromatography (TLC) was used for the qualitative analysis of Lycii Fructus in the formula. The fingerprint of Wuziyanzong pills based on combined control herbs, the screening method of Schisandrae Sphenantherae Fructus and the determination of hyperoside and schisandrin in the formula were established by HPLC. The contents of Pb, Cd, As, Hg, Cu and Cr were determined by ICP-MS method. RESULTS The TLC identification method showed good separation effect and specificity. The fingerprint, using the combined control herbs, could simultaneously identify Rubi Fructus, Cuscutae Semen, Plantaginis Semen, and Schisandrae Chinensis Fructus with good method validation results. According to the peak area ratio of schisantherin A and schisandrin, it could screen out Schisandrae Sphenantherae Fructus in the formula when the ratio was proposed to be 0.20. In the assay, the content limits of hyperoside and schisandrin in Wuziyanzong pills were proposed. Three harmful elements, ie As, Hg and Pb exceeded the permitted limits in 19 batches of samples. This may be caused by using the same production line for different products and the samples may be contaminated by the residue of previous products. CONCLUSION The established quality standard is simple and accurate and shows good specificity and reproducibility. It could be used for the comprehensive and overall quality evaluation of Wuziyanzong pills.