微波辅助-分散固相萃取/超高效液相色谱-串联质谱法测定血水草中8种生物碱  

Determination of Eight Alkaloids in Eomecon Chionantha Hance with Microwave-Assisted and Dispersive Solid Phase Extraction Combined with Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：樊轻亚[1] 汪学猛 FAN Qingya;WANG Xuemeng(Xinyang Vocational and Technical College,Xinyang 464000)

机构地区：[1]信阳职业技术学院,河南信阳464000

出　　处：《分析科学学报》2023年第4期431-438,共8页Journal of Analytical Science

基　　金：河南省科技厅科技攻关项目(172102310315);中共河南省委教育工委高校“双带头人”教师党支部书记工作室建设项目资助。

摘　　要：建立了微波辅助-分散固相萃取技术(dSPE)结合超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定血水草中8种生物碱的方法。采用单因素实验考察了微波辅助-分散固相萃取中各因素对血水草中8种生物碱萃取率的影响,最佳萃取条件为:微波功率560 W,微波提取时间4 min;以PSA和GCB混合吸附剂为净化剂,两种吸附剂的用量均为125 mg,净化萃取时间3 min。分散固相萃取后以乙腈-0.02 mol/L甲酸铵溶液(含0.1%甲酸)为流动相进行梯度洗脱,利用UPLC-MS/MS进行分析。结果表明:8种生物碱在1~200 mg/L范围内线性关系良好,相关系数均不低于0.991,检出限为0.05~0.12 mg/L,定量限在0.19~0.40 mg/L之间。三个浓度添加水平下,8种生物碱的回收率在91.2%~98.1%之间,相对标准偏差(RSD)为1.2%~2.9%。采用该方法对6个产地的血水草进行了检测,样品中8种生物碱的含量在0~0.78 mg/g之间,RSD在1.2%~2.9%之间。本文所建立萃取分析方法准确性好,灵敏度高,操作快速简单,可满足血水草中生物碱检测的要求。A method for the determination of eight alkaloids in Eomecon chionantha Hance was developed by microwave-assisted and dispersive solid-phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry(UPHLC-MS/MS).Experimental conditions on the extraction of eight alkaloids were optimized by single factor optimization.The optimum conditions showed that Microwave power was 560 W,and microwave extraction time was 4 min and the dosage of PSA and GCB mixed adsorbent was 125 mg,and purification time was 3 min.The analytes were separated by gradient elution using acetonitrile-0.02 mol/L ammonium formate solution(containing 0.1%formic acid)as mobile phase of UPLC-MS/MS.The linear range of eight alkaloids was 1[WT5,7]-[WT]200 mg/L,and the correlation coefficients were not lower than 0.991.The limits of detection were in the range of 0.05[WT5,7]-[WT]0.12 mg/L and the limits of quantitation were in the range of 0.19[WT5,7]-[WT]0.40 mg/L.The recoveries for the eight alkaloids at three spiked levels were in the range of 91.2%[WT5,7]-[WT]98.1%with relative standard deviations of 1.1%[WT5,7]-[WT]2.9%.The method was used to determine the contents of eight alkaloids in the samples from 6 different sources,and the contents of eight alkaloids were in the range of 0[WT5,7]-[WT]0.78 mg/g,and RSD was 1.2%[WT5,7]-[WT]2.9%.The method was accurate,sensitive,rapid and simple,and is suitable to the extraction of the eight alkaloids from Eomecon chionantha Hance.

关 键 词：血水草 生物碱 分散固相萃取 超高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]