冠心颗粒的标准研究

Study on standard of Guanxin Keli

目的建立冠心颗粒的质量标准。方法采用薄层色谱法(TLC)对冠心颗粒中丹参、三七进行定性鉴别;采用2015年版《中国药典》微生物限度检查法进行验证试验,并对2批次样品进行微生物限度检查;采用高效液相色谱法对丹酚酸B进行含量测定:色谱柱为Kromasil C18(250 mm×4.6 mm,5μm),流动相为以甲醇-乙腈-1%甲酸水溶液(29∶9∶62),流速为1.0 m L/min检测波长为286 nm。结果 TLC鉴别斑点清晰、分离较好,阴性对照无干扰;2批冠心颗粒微生物计数方法适用性试验需氧菌总数、霉菌和酵母菌总数各菌的回收率均在50%~200%,且均未检出大肠埃希菌,验证组可检出大肠埃希菌,该方法可行;丹酚酸B在0.06~0.54 mg/m L与峰面积呈良好的线性关系(r=0.9998),平均加样回收率为98.61%,RSD=1.24%(n=6);2批样品含量测定结果均符合要求。结论本方法所用定性、定量及微生物限度检查方法准确可靠、重现性好,能有效控制冠心颗粒的药品质量。

Objective To establish the quality standard of Guanxin Keli. Methods TLC method was used for the quali- tative identification of Salvia miltiorrhiza Bge., Panax notoginseng （Burk） F.H.Chen; the method validation was conduct- ed by using microbial limit test in Chinese Pharmacopoeia 2015. 2 batches of Guanxin granules were tested under the validated method. HPLC was used to determine the content of salvianolie acid B. The determination was performed on KromasilCl8 （250 mm×4.6 mm, 5μm） column with mobile phase consisted of methanol-acetonitrile-l% formic acid wa- ter （29：9：62） at the flow rate of 1.0 mL/min. The detection wavelength was set at 286 nm. Results TLC spots were clear and well-separated without negative interference. The recoveries of each validation strain for the total aerobic micribial count, total yeasts and mold count were among 50%-200%, and did not test E. coll. This validation of method could test E. coli, and was capable. The linear range of salvianolic acid B was 0.06-0.54 mg/mL （r = 0.9998） with an average recovery of 98.61%, RSD = 1.24% （n = 6）; the content of two batehs samples were satisfactory. Conclusion The method is simple, accurate and reproducible. It is effective in controlling the quality of Guanxin Keli and providing the basis for improving the quality standas of Guanxin Keli.