一测多评结合内标加入法测定吐根及其制剂中生物碱类成分的含量

Simultaneous assay with standard addition method of alkaloids in ipecacuanhae and the preparation by quantitative analysis of multi-components by single marker

目的建立以盐酸小檗碱为加入内标,测定吐根药材及其制剂中盐酸吐根碱、盐酸吐根酚碱的一测多评测定方法。方法采用高效液相色谱法,以Capcell pak C18 MGⅡ(250 mm×4.6 mm,5μm)为色谱柱,乙腈(A)-体积分数0.1%磷酸溶液(B)为流动相,梯度洗脱,流速为1.0 mL·min-1,柱温30℃,检测波长为205 nm。以外加的盐酸小檗碱为内参物,分别建立盐酸吐根碱、盐酸吐根酚碱的相对校正因子,利用该相对校正因子计算药材及其制剂中该两种成分的量;同时利用外标法测定盐酸吐根碱、盐酸吐根酚碱的量,比较两种测定方法的差异,采用方差分析比较不同产地吐根药材的两种成分的含量差异。结果在线性范围内,盐酸小檗碱与盐酸吐根碱、盐酸吐根酚碱的相对校正因子分别为0.499 5、0.439 2,在不同实验条件下相对校正因子重现性良好,两种生物碱类成分的计算值与实测值无显著性差异。结论采用一测多评法测定吐根药材及其制剂中生物碱类成分准确且可行,可用于吐根药材及其制剂的质量控制。

Objective To establish a method for simultaneous assay of 2 kinds of alkaloids in Ipecacuanhae and its preparation by quantitative analysis of multi-components by single marker(QAMS).Methods The chromatographic separation was performed on a MGII(250 mm×4.6 mm,5 μm)with gradient elution using acetonitrile and 0.1% phosphoric acid as mobile phase.The detection wavelength was at the 205 nm.Using the added berberine as the internal reference,the content of the two components in Cephaeline hydrochloride and the preparations were calculated by the relative correction factor(RCF).The method was evaluated by comparison of the quantitative results between external standard method and QAMS method.Variance analysis was used to compare 2 components in Ipecacuanhae from different places.Results Within the linear range,the RCFs of Emetine hydrochloride,Cephaeline hydrochloride were 0.499 5,0.439 2,respectively,with good repeatability in different experimental conditions.There was no significant difference between the QAMS method and ESM method.There is little difference in the content of Emetine hydrochloride.Conclusion It is feasible and accurate to control the quality of Ipecacuanhae and its preparation with QAMS.