基于UPLC-TQ MS的丹七软胶囊中8种活性成分的溶出度考察

Study on dissolution of Eight Active Ingredients in Danqi soft capsules based on UPLC-TQ MS

目的:建立丹七软胶囊溶出度的测定方法,考察丹七软胶囊中活性成分的体外溶出度,为该制剂的质量评价提供参考。方法:采用UPLC-TQ MS法测定丹七软胶囊中8种活性成分,包括5个丹酚酸类物质(丹酚酸A,丹酚酸B、迷迭香酸、丹参素、鼠尾草酸),3个三七皂苷类(三七皂苷R1、人参皂苷Rb1、人参皂苷Rg1);丹参酚酸类化合物与三七皂苷类化合物分别采用不同的流动相梯度洗脱方法;质谱采用MRM模式检测,酚酸类成分在Low Mass负离子模式下检测,三七皂苷类成分在High Mass负离子模式下检测。结果:采用桨法,以1%SDS水溶液900 m L为介质,转速为100 r·min-1,测定溶出度;丹酚酸A、丹酚酸B、迷迭香酸、丹参素、鼠尾草酸、三七皂苷R1、人参皂苷Rb1、人参皂苷Rg1的精密度分别为0.22、0.63、0.43、0.39、0.58、0.39、0.58、0.72%,加样回收率分别为101.1、99.5、98.2、98.8、98.4、102.1、101.5、100.1%;丹七软胶囊溶出均一性与溶出重复性良好;水溶性活性成分溶出较快,30 min时丹参中的酚酸类物质和三七中的三七皂苷类即可达到最大的溶出。结论:建立的溶出度试验方法操作简便、结果准确、重复性好,适用于丹七软胶囊溶出度测定;利用该方法考察了丹七软胶囊中不同活性成分的溶出规律,为中药复方制剂的质量标准评价提供了参考。

Objective： To establish a method for determination dissolution rate of Danqi soft capsule in vitro. Method：UPLC-TQ MS methods were developed for detemination of 8 main components in Danqi soft capsule（Salvianolic acid A,salvianolic acid B, rosmarinic acid, danshensu, roamoxalic acid, notoginsenoside R1, ginsenoside Rb1, ginsenoside Rg1）.Different UPLC elution gradient and mass spectrometric parameters were used for phenolic acids and saponinsin. Result：The solution containing 0.5% SDS was used as dissolution medium and the dissolution rates of 8 active components in Danqi soft capsule were determined by UPLC-TQ MS. The precision of salvianolic acid A, salvianolic acid B, danshensu,rosmarinic acid, carnosic acid, notoginsenoside R1, ginsenoside Rb1, ginsenoside Rg1 was 0.22, 0.63, 0.43, 0.39, 0.58,0.39, 0.58 and 0.72% respectively, and the recovery was 101.1, 99.5, 98.2. 98.8, 98.4, 102.1, 101.5 and 100.1%; The water-soluble active ingredients such as phenolic acids and saponins in Danqi soft capsule dissolves quickly, which can reach the maximum dissolution in 30 minutes. Conclusion： This method was steady and suitable for the test of the dissolution rate of Danqi soft capsules.