HPLC法测定复方茵陈注射液中间体盐酸小檗碱

HPLC determination of berberine hydrochloride in intermediate products of compound Yinchen injection

目的:建立复方茵陈注射液中间体中盐酸小檗碱的HPLC含量测定方法。方法:采用HPLC法测定盐酸小檗碱含量,并进行了方法学验证。色谱柱:安捷伦C18(4.6 mm×250 mm,5μm);流动相:乙腈-0.1%磷酸(20:80);流速1.0 mL·min-1;检测波长为267 nm。结果:色谱分离度好,阴性对照无干扰;盐酸小檗碱在0.056～0.560μg范围内具有良好的线性关系;回收率为102.7%,RSD=1.3%(n=5);重复性RSD=1.5%(n=6);精密度RSD=1.4%(n=6);监测46批复方茵陈注射液中间体表明:渗漉液(Ⅱ)和三次醇沉液(Ⅲ)中盐酸小檗碱的含量分别为10.31～13.29 mg·mL-1和0.49～0.68 mg·mL-1。结论:本HPLC方法稳定、准确,暂拟的中间体质量控制内控标准能够更有效地监控上述中间体的质量,实现对复方茵陈注射液的生产过程质量控制。对2年间的46批制剂中间体[渗漉液(Ⅱ)和三次醇沉液(Ⅲ)]实行监测,结果表明,复方茵陈注射液生产工艺稳定,产品质量有保障。

Objective：To establish a method to determinate berberine hydrochloride in semi-finished products of Fufang Yinchen injection by HPLC.Methods：A column of Agilent-C18（4.6 mm×250 mm,5 μm） was adopted;The mobile phase consisted of acetonitrile and 0.1% phosphoric acid（20：80）;the flow rate was 1.0 mL.min-1;The detection wavelength was 267 nm.Results：The assay displayed good linearity over the concentration range of 0.056-0.560 μg of berberine hydrochloride.The average recovery was 102.7% and the RSD was 1.3%（n=5）.The precision and repeatability were good with the RSD of 1.4%（n=6） and 1.5%（n=6）,respectively.Forty-six batches of intermediates of Fufang Yinchen injection are monitored.It indicated that the content of berberine hydrochloride in percolating liquid（Ⅱ） and alcohol deposit fluid（Ⅲ） were 10.31-13.29 mg·mL-1 and 0.49-0.68 mg·mL-1,respectively.Conclusion：The developed method is accurate and practical.The quality control standards for intermediates of Fufang Yinchen Injection were formulated for the moment,and the quality of such injection can be controlled in production process.Forty-six batches of intermediates of preparations for two years have been monitored.The results shows that production process of Fufang Yinchen injection is stable,and the quality of products is safe.