超高效液相色谱-串联质谱法同时测定陈年老茶中16种真菌毒素残留

建立一种超高效液相色谱-串联质谱法测定不同种类陈年老茶中16 种真菌毒素的方法.样品经甲酸-乙腈(10:90,V/V)溶液提取,提取液加入QuEChERS盐包振摇离心,过OASIS PRIME HLB小柱和dSPE净化管处理,以ACQUITYUPLCHSST3C18色谱柱分离,采用电喷雾正离子的多反应离子监测模式,茶叶...

Simultaneous Determination of 16 Mycotoxin Residues in Aged Tea by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed for the simultaneous determination of 16 mycotoxins from different types of aged tea. The sample was extracted with formic acid-acetonitrile(10:90, V/V), added with a blend of QuEChERS(quick, easy, cheap, effective, rugged, and safe) extraction salts, shaken and centrifuged;the extract was cleaned up by passing through an OASIS PRIME HLB cartridge and a dispersive solid-phase extraction(dSPE) purification tube, separated on an ACQUITY UPLC HSS T3C18 column, detected using an electrospray ionization source in the positive ion multiple reaction monitoring(MRM) mode, and quantified using tea matrix matching standard solution. The 16 mycotoxins showed a good linear relationship within their respective concentration ranges with correlation coefficients > 0.999. The average recoveries from tea matrix spiked at three different levels ranged between 63.4% and 109.7%, with relative standard deviations(RSDs) between 1.7% and 11.3%. The method limits of detection(LODs) ranged from 0.03 to 7.00 μg/kg. Among 121 aged tea samples selected for analysis, aflatoxin B1 was detected from one oolong tea sample at a concentration of 34.0 μg/kg, and ochratoxin A was also detected from one black tea sample at a concentration of 1.6 μg/kg. The method proved to be stable, accurate, sensitive and fast, and could meet the requirements for the analysis of multiple toxic residues in a variety of tea samples.