一测多评技术在3种丹参制剂质量控制中的可行性分析

目的建立一测多评法(QAMS)同时测定3种丹参制剂(丹参片、复方丹参片和冠心丹参胶囊)中丹参酮类成分丹参酮IIA(TIIA)、二氢丹参酮I(DTI)、隐丹参酮(CT)、丹参酮I(TI)]量,探讨QAMS技术在中药制剂质量评价中的准确性和可行性。方法采用HPLC法测定TIIA、DTI、CT和TI;以丹参片、复方丹参片和冠心丹参胶囊为研究对象,采用QAMS技术,以TIIA为内参物,建立DTI、CT、TI与TIIA之间的相对校正因子(fi/s),比较保留时间差、相对保留值和线性回归定位法对待测成分的定位效果;并用外标法对样品进行定量计算,比较实测值与QAMS计算值之间的差异,以验证其准确性。结果所建立的HPLC法测定TIIA、DTI、CT和TI准确可行;在线性范围内,DTI、CT、TI与TIIA之间的fi/s分别为0.734、0.916、0.774,在不同测试条件下待测成分的fi/s准确可靠;相对保留值法能够对待测成分进行准确定位,DTI、CT、TI与TIIA之间的相对保留值分别是0.314、0.518、0.561,外标法和QAMS测定结果无显著性差异。3种丹参制剂定量测定结果显示不同厂家即使是同一厂家不同批次,产品的内在质量存在一定差异。结论所建立的丹参酮类成分QAMS适用于多种丹参制剂的质量控制,可为其他丹参制剂的质量评价提供参考;同时,应进一步加强对以上3种中药制剂的控制与监管。

Feasibility study of QAMS for quality control on three kinds of related preparations of Salvia miltiorrhiza

Objective To establish a quantitative analysis method of multi-components by single marker (QAMS) for the simultaneous determination of four tanshinonestanshinone IIA (TII_A),dihydrotanshinone I (DTI),cryptotanshinone (CT),and tanshinone I (TI)],and to explore its accuracy and feasibility on quality evaluation of traditional chinese medicine preparations about three kinds of related preparations of Salvia miltiorrhiza.Methods An HPLC method was used to calculate relative correction factors (f_i/s) between other three components with TII_A.The component positioning methods were compared including retention time difference value,relative retention value,and linear regression methods.Meanwhile,the contents of tanshinones in different preparations of S.miltiorrhiza were determinated by the external standard method (ESM),including Danshen Tablet,Compound Danshen Tablet,and Guanxin Danshen Capsule.Measured content value was compared with calculated content value to evaluate the accuracy of QAMS method.Results Within a certain range,the f_i/s of DTI,TI,and CT to TII_A were 0.734,0.916,and 0.774,respectively,with the good repeatability in different experimental conditions.The f_i/s between other three components with TII_A was accurate and reliable,and there was no significant difference between QAMS and ESM method.Besides,the relative retention value method could be used to accurately locate the measuring component.The relative retention values of DTI,TI,and CT to TII_A were 0.314,0.518,and 0.561,respectively.The contents of three kinds of S.miltiorrhiza preparations showed there were some differences in the intrinsic quality of the products from different factories,even from different batches of the same manufacturer.Conclusion The QAMS method could be used for quality control about related preparations of S.miltiorrhiza and provide references for quality evaluation of other preparations.At the same time,the above three kinds of traditional Chinese medicine preparations should be further strengthened the control and supervision.