超快速液相色谱-三重四极杆/线性离子阱质谱法同时测定连翘药材中的多元活性成分  

Simultaneous Determination of Multiple Bioactive Constituents in Forsythiae Fructus by UFLC-QTRAP-MS/MS

作　　者：魏丽芳 梅余琪 邹立思[1] 刘训红[1] 陈佳丽 谈梦霞 王程成 蔡芷辰[1] 林丽群 WEI Li-fang;MEI Yu-qt;ZOULi-si;LlUXun-hong;CHEN Jin-lt;TANMeng-xia;WANG COeng-cheng;CAI Zi-chen;LIN Li-qun(School of Pharmacy,Nanjing University of ChPese Menicige,Nanjing 210023,Chinn)

机构地区：[1]南京中医药大学药学院,江苏南京214023

出　　处：《分析测试学报》2019年第12期1407-1415,共9页Journal of Instrumental Analysis

基　　金：江苏高校优势学科建设工程资助项目(YSXK-2014);江苏高校品牌专业建设工程资助项目(PPZY2015A070).

摘　　要：建立了基于超快速液相色谱-三重四极杆/线性离子阱质谱(UFLC-QTRAP-MS/MS)同时测定连翘药材中苯乙醇苷类、木脂素类、黄酮类及酚酸类共21种活性成分含量的方法。采用响应面法(RSM)优化连翘药材的提取条件;以XBridge?C18(4.6 mm×100 mm,3.5μm)色谱柱分离,水(含0.1%甲酸)-乙腈为流动相,梯度洗脱,流速为0.8 mL/min,柱温为30℃,进行多反应监测(MRM)模式检测。结果表明,最佳提取条件为:甲醇体积分数72%,液料比38∶1 mL/g,提取时间60 min。21种目标成分在一定质量浓度范围内均呈良好的线性关系,相关系数(r)均不小于0.999 0;检出限和定量下限分别为0.001~233.710 ng/mL和0.002~771.250 ng/mL;精密度、重复性和稳定性良好;平均加标回收率为98.6%~102%,相对标准偏差(RSD)为0.89%~3.8%。该方法准确、可靠,可为连翘药材内在质量的综合评价和全面控制提供参考。A comprehensive analytical method based on ultra-fast liquid chromatography coupled with triple quadrupole/linear ion trap tandem mass spectrometry(UFLC-QTRAP-MS/MS) was established for the simultaneous determination of phenylethanoid glycosides,lignans,flavonoids and phenolic acids in Forsythiae Fructus.Conditions for the herbs extraction were optimized by the response surface method(RSM).Subsequently,the extract was separated on an XBridge?C18 column(4.6 mm×100 mm,3.5 μm) by gradient elution with 0.1% aqueous formic acid solution-acetonitrile as mobile phase at a flow rate of 0.8 mL/min at 30 ℃,and analyzed under multiple-reaction monitoring(MRM) mode.Results showed that,the optimum sample extraction conditions were as follows:72% of methanol volume fraction,38 ∶1 mL/g of liquid-to-material ratio and 60 min of extraction time.Additionally,the 21 analytes showed good linearities in corresponding concentration ranges with their correlation coefficients(r) no less than 0.999 0.The limits of detection and the limits of quantitation were 0.001-233.710 ng/mL and 0.002-771.250 ng/mL,respectively.The precision,repeatability and stability of the method were all satisfactory.Average spiked recoveries ranged from 98.6% to 102% with relative standard deviations(RSD) between 0.89% and 3.8%.The method developed is accurate and reliable,and provides a new reference for the quality evaluation and control of Forsythiae Fructus.

关 键 词：连翘 超快速液相色谱-三重四极杆/线性离子阱质谱(UFLC-QTRAP-MS/MS) 响应面法(RSM) 活性成分 

分 类 号：O657.7[理学—分析化学] R914.1[理学—化学]