牡丹皮配方颗粒中芍药苷亚硫酸酯定量分析方法的建立及应用  

Establishment and Application of Quantitative Analysis Method for Paeoniflorin Sulfonate in Cortex Moutan Formula Granules

作　　者：王劲 付美芳 赵丹彤 WANG Jin;FU Meifang;ZHAO Dangtong(Heze Institute for Food and Drug Control,Shandong Heze 274000,China;School of Pharmacy,Shandong University of Traditional Chinese Medicine,Shandong Jinan 250355,China)

机构地区：[1]菏泽市食品药品检验检测研究院,山东菏泽274000 [2]山东中医药大学药学院,山东济南250355

出　　处：《中国医药导刊》2024年第9期896-901,共6页Chinese Journal of Medicinal Guide

基　　金：山东省药品质量风险监测项目-配方颗粒专项(2022-11);菏泽市社会科学规划课题(2022-135)。

摘　　要：目的:建立牡丹皮配方颗粒中芍药苷亚硫酸酯的定量分析方法,采用该方法对市售16批牡丹皮配方颗粒中芍药苷亚硫酸酯含量进行测定,考察牡丹皮饮片经硫熏后对配方颗粒中芍药苷含量的影响。方法:采用高效液相色谱-三重四级杆质谱联用技术,色谱柱为Aglient Eclipse Plus C18(2.1 mm×150 mm,3µm),流动相为乙腈-0.1%甲酸水,梯度洗脱,柱温35℃,流速0.4 mL·min-1,质谱采用电喷雾(ESI)离子源、负离子模式、多反应监测(MRM)的扫描方式进行检测。结果:牡丹皮配方颗粒中芍药苷亚硫酸酯检测质量浓度的线性范围为0.050~1.000µg·mL-1(r=0.999),精密度、重复性、稳定性(24 h)试验的RSD均小于2.5%;平均加样回收率为96.68%(RSD=2.17%,n=9);检出限为3.1µg·g^(-1),定量下限为10.3µg·g^(-1)。16批市售牡丹皮配方颗粒中芍药苷亚硫酸酯含量范围11.9~21.8µg·g^(-1)。结论:所建方法可为评估牡丹皮饮片的硫熏程度对牡丹皮配方颗粒质量的影响提供新参考。Objective:To establish a method for quantitative analysis of paeoniflorin sulfonate in Cortex Moutan formula granules,determine the content of paeoniflorin sulfonate in 16 batches of cortex moutan formula granules by this method,and analyze the influence of sulfur fumigation on the content of paeoniflorin.Methods:The analysis was performed with Aglient triple quadrupole mass spectrom-eter by electrospray ionization(ESI-)mode and on Agilent Eclipse Plus C18 column(2.1 mm×150 mm,3µm).The mobile phase was ace-tonitrile(A)-0.1%phosphoric acid solution(B)with gradient elution at a flow rate of 0.4 mL·min-1.The colume temperature was 35℃.Results:Good linearity(r=0.999)was observed in the range of 0.050-1.000µg·mL-1.RSD of precision,repeatability and stability(24 h)tests were all lower than 2.5%.The average recovery rate was 96.68%(RSD=2.17%,n=9).The limit of detection was 3.1µg·g^(-1).The limit of quantitation was 10.3µg·g^(-1).The content of paeoniflorin sulfonate in 16 batches of cortex moutan formula granules ranged from 11.9 to 21.8µg·g^(-1).Conclusion:This method provides new reference for evaluating the influence of sulfur fumigation of peony peel pieces on the quality of cortex moutan formula granules.

关 键 词：牡丹皮配方颗粒 芍药苷亚硫酸酯 硫熏 芍药苷 

分 类 号：R284.1[医药卫生—中药学]