基于超高效液相色谱-静电场轨道阱质谱技术的十二味参芍益脑合剂中12种主要化学成分定量检测研究  

Simultaneous determination of 12 components in Shierwei Shenshao Yinao mixture by ultra-performance liquid chromatography tandem hybrid orbitrap mass spectrometry

作　　者：陈刚[1] 汪生 宫鹏[3] CHEN Gang;WANG Sheng;GONG Peng(Department of Pharmacy,Taihe Hospital of Traditional Chinese Medicine,Fuyang,Anhui 236600,China;Scientific Research Center of Anhui Medical University,Hefei,Anhui 230032,China;Department of Pharmacy,The First Affiliated Hospital of Anhui Medical University,Hefei,Anhui 230022,China)

机构地区：[1]太和县中医院药剂科,安徽阜阳236600 [2]安徽医科大学科研实验中心,安徽合肥230032 [3]安徽医科大学第一附属医院药剂科,安徽合肥230022

出　　处：《安徽医药》2023年第9期1750-1756,I0001,共8页Anhui Medical and Pharmaceutical Journal

基　　金：2021年度安徽省卫生健康委科研重点项目(AHWJ2021a018)。

摘　　要：目的基于超高效液相色谱-静电场轨道阱质谱技术,同时测定十二味参芍益脑合剂中12种主要化学成分(绿原酸、栀子苷、芍药苷、芍药内酯苷、甘草苷、黄芩苷、芹菜素、甘草素、汉黄芩苷、黄芩素、汉黄芩素和千层纸素A)的含量。方法该研究起止时间为2021年3月至2022年5月。采用Waters UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8µm),以乙腈-0.1%甲酸和10 mmol/L甲酸铵水溶液为流动相,线性梯度洗脱,流速0.25 mL/min,柱温35℃,采用电喷雾离子化,平行反应监测离子扫描,以负离子模式检测16批十二味参芍益脑合剂。结果测定的12种主要化学成分在检测浓度范围内线性关系良好(r>0.99),加样回收率范围为80.58%~112.90%[相对标准差(RSD)<10%],基质效应范围为76.58%~110.80%(RSD<10%),进样精密度、重复性、稳定性均符合方法学测定要求。16批制剂检测结果显示13批质量相对稳定,其余3批有一定差异,栀子苷可以作为进一步评价制剂质量的指标。结论该方法专属性强、灵敏度高、重复性好,准确可靠,可用于十二味参芍益脑合剂中12种主要化学成分的同步含量测定。Objective To establish a method for quantification of 12 components(chlorogenic acid,geniposide,paeoniflorin,albiflorin,liquiritin,baicalin,apigenin,liquiritigenin,wogonoside,baicalein,wogonin and oroxylin A)in Shierwei Shenshao Yinao mixture by ultra-performance liquid chromatography tandem hybrid orbitrap mass spectrometry(UPLC-Q-Orbitrap-MS)technique.Methods The study started from March 2021 and ended in May 2022.The analysis was performed on a Waters ACQUITY UPLC HSS T3 column(100 mm×2.1 mm,1.8µm)with a mobile phase of acetonitrile-0.1%formic acid and 10 mmol/L ammonium formate aqueous solution for linearity gradient elution,the flow rate was 0.25 mL/min,and the column temperature was set at 35℃.Electrospray ionization source was used for determination in the parallel reaction monitoring mode under anion conditions.Results The 12 targeted compounds showed a satisfying linear relationship within the range of concentration determined(r>0.99),with an average recovery ranged from 80.58%to 112.90%(RSD<10%)and the matrix effect ranged from 76.58%to 110.80%(RSD<10%).The precision,repeatability and stability were validated and meet the requirement of quantitation.The content determination of 16 batches of preparation showed that the quality of 13 batches was relatively stable,and the other 3 batches were slightly different.Geniposide could be a potential biomarker in quality evaluation of the preparation.Conclusion This method has high specificity and sensitivity,good repeatability and accuracy,which could be successfully used for the determination of 12 chemical components in Shierwei Shenshao Yinao mixture.

关 键 词：主成分分析 十二味参芍益脑合剂 超高效液相色谱-静电场轨道阱质谱 含量测定 平行反应监测 质量控制 

分 类 号：R286.0[医药卫生—中药学] O657.63[医药卫生—中医学]