目的建立基于保肝、安神功效的疏肝安神颗粒多指标质量评价方法。方法采用UHPLC-MS-MS法,液相条件:色谱柱为Phenomenex C 18(2.1 mm×50 mm,5μm),流动相为乙腈-0.1%甲酸(梯度洗脱),流速为0.7 mL/min,进样量为10μL;质谱检测条件:采用ESI离子源,检测离子对为柴胡皂苷A 782.3/456.1、茯苓酸A 497.1/423.3、茯苓酸B 483.1/409.3、丹参酮ⅡA 295.1/277.0(249.0、191.1)、丹酚酸B 717.0/320.9(519.0)、芍药苷525.0/326.9(449.1);共测定10批颗粒样品。结果各组分精密度RSD值为0.40%~1.98%,稳定性RSD值为0.57%~2.44%,重复性RSD值为0.35%~2.70%,符合2015年版《中国药典》相关要求;10批疏肝安神颗粒样品中,柴胡皂苷A的质量分数为0.256~0.372 mg/g,茯苓酸A的为0.008~0.012 mg/g,茯苓酸B的为0.062~0.082 mg/g,丹酚酸B的为3.058~4.401 mg/g,芍药苷的为2.494~2.566 mg/g。结论本方法快速、科学、高效,所选指标均为活性成分,能够较准确地评价疏肝安神颗粒的质量。
Objective To establish a multiple indexes evaluation method for Shugan Anshen granules based on their liver protection and tranquilizing effect. Methods UHPLC-MS-MS was used to determine the active components with a Phenomenex C18(2.1 mmm×50 mm,5 μm) and a mobile phase containing acetonitrile and 0.1% formic acid with the gradient elution,the flow rate was 0.7 mL/min,the injection volume was 10 μL,and the mass detection mode was ESI. The ion pairs were as follows: saikosaponin A 497.1/423.3,pachymic acid A 497.1/423.3,pachymic acid B 483.1/409.3,tanshinone ⅡA 295.1/277.0,249.0,191.1,salvianolic acid B 717.0/320.9,519.0,paeoniflorin 525.0/326.9,449.1. 10 batches of the samples were analyzed. Results The analytical method established in the study had precision(in the form of RSD) of 0.40%-1.98%,RSDs for stability were 0.57%-2.44%,and the values for that of repeatability were 0.35%-2.70%,which were all in line with criterial of China Pharmacopeia(current edition). The contents of Saikosaponin A were 0.256-0.372 mg/g,the contents of Pachymic acid A were 0.008-0.012 mg/g,the contents of Pachymic acid B were 0.062-0.082 mg/g,the contents of Salvianolic acid B were 3.058-4.401 mg/g,and the contents of Paeoniflorin were 2.494-2.566 mg/g in 10 batches of Shugan Anshen granules. Conclusion The method is fast,scientific and effective,and the selected indicators are all active ingredients,which can accurately evaluate the quality of Shugan Anshen granules.
Journal of Guangdong Pharmaceutical University