UHPLC-MS/MS法同时测定补骨脂药材中17种成分的含量  

Simultaneous quantification of 17 components in psoraleae fructus by UHPLC-MS/MS method

作　　者：夏宁 张孝莹 成丽媛 张玥[1,2,3] 周昆 XIA Ning;ZHANG Xiaoying;CHENG Liyuan;ZHANG Yue;ZHOU Kun(Center of Drug Safety Evaluation,Tianjin University of Traditional Chinese Medicine,Tianjin 301617,China;Institute of Traditional Chinese Medicine,Tianjin University of Traditional Chinese Medicine,Tianjin 301617,China;State Key Laboratory of Component-based Chinese Medicine,Tianjin 301617,China)

机构地区：[1]天津中医药大学药物安全评价中心,天津301617 [2]天津中医药大学中医药研究院,天津301617 [3]省部共建组分中药国家重点实验室,天津301617

出　　处：《天津中医药大学学报》2024年第11期971-977,共7页Journal of Tianjin University of Traditional Chinese Medicine

基　　金：国家自然科学基金项目(81673826);组分中药国家重点实验室资助课题项目(CBCM2023203)。

摘　　要：[目的]建立UHPLC-MS/MS法同时测定25批补骨脂中17种成分的含量。[方法]采用超高效液相色谱-三重四级杆串联质谱技术检测,色谱柱为Thermofisher Scientific Hypersil GOLD(100 mm×2.1 mm 1.9μm),流动相为水(A)-乙腈(B),梯度洗脱,进样量为3μL,流速为0.2 mL/min,柱温40℃;离子源为电喷雾离子源(ESI);在多反应检测(MRM)模式下正、负离子同时测定。[结果]补骨脂素、异补骨脂素、补骨脂酚、4,5-去氢异补骨脂定、补骨脂查尔酮、异补骨脂色烯查尔酮、补骨脂二氢黄酮甲醚、补骨脂宁、补骨脂定、补骨脂甲素、补骨脂乙素、8-甲氧基补骨脂素、异补骨脂二氢黄酮、新补骨脂异黄酮、5-甲氧基补骨脂素、巴库查尔酮、Corylifol A 17种成分线性关系良好(r>0.99),平均加样回收率(n=6)为95.66%~101.38%,RSD为0.77%~3.04%;精密度、重复性,稳定性试验的RSD均小于2.57%,符合分析要求。含量测定显示,不同批次补骨脂中各成分含量差别较大。[结论]本实验建立的检测方法快速、准确、重复性好,可适用于补骨脂的质量控制研究。[Objective]To establish a UHPLC-MS/MS method for the simultaneous determination of 17 components in 25 batches of psoraleae fructus.[Methods]The UHPLC-MS/MS method was performed on Thermofisher Scientific Hypersil GOLD(100×2.1mm 1.9μm).The mobile phase was water(A)-acetonitrile(B);Gradient elution;The injection volume was 3μL.The flow rate was 0.2 mL/min and column temperature were 40℃.The ion source was ESI,the ion source temperature was 500℃.The positive and negative ions were measured simultaneously in multiple reaction detection(MRM)mode.[Results]psoralen,isopsoralen,bakuchiol,4,5-dehydroisopsoralidin,bavachalcone,isobavachromene,bavachinin,corylin,psoralidin,bavachin,isobavachalcone,8-methoxypsoralen,isobavachin,neobavaisoflavone,5-methoxypsoralen,bakuchalone,corylifol a 17 components with good linear relationship(r>0.99),the average recoveries(n=6)were 95.66%~101.38%,RSD was 0.77%~3.04%.RSDS of precision,repeatability and stability tests were all less than 2.57%,which met the requirements of analysis.The content determination showed that the content of each component in different batches of psoralen was different.[Conclusion]The method established in this experiment is rapid,accurate and reproducible,and can be applied to the quality control of psoraleae fructus.

关 键 词：补骨脂 UHPLC-MS/MS 含量测定 

分 类 号：R284.2[医药卫生—中药学]