超高效液相色谱-串联质谱法同时测定酿酒原料中16种真菌毒素

Simultaneous Determination of 16 Fungal Toxins in Brewing Materials by Uplc-tandem Mass Spectrometry

采用Qu ECh ERS前处理技术,建立了超高效液相色谱-串联质谱(UPLC-MS/MS)检测不同酿酒原料样品(大米、糯米、小麦、高粱和玉米)中16种真菌毒素含量的分析方法。该方法是将样品经过混合溶液(乙腈∶水∶乙酸=29∶70∶1)超声萃取10min,离心,通过HLB萃取小柱进行净化除杂和富集,富集后使用甲醇复溶即完成测试样的制备,经超高效液相色谱仪分离后,采用三重四级杆串联质谱仪进行多反应离子监测模式检测。本方法 16种生物毒素在50ng/m L^1000ng/mL范围内线性关系好,相关系数r2均大于0.993,样品的平均回收率在90%~120%,检出限在5ng/mL^20ng/mL,本发明方法准确可靠、简单快捷,可用于同时检测酿酒原料中16种真菌毒素。

A method for the determination of 16 fungal toxins in different brewing materials(rice,glutinous rice,wheat,sorghum and corn)by uplc-ms/MS was established by using QuEChERS pre-treatment technique.This method is to sample after mixture(acetonitrile:water:acetic acid=29:70:1)therefore ultrasound extraction for 10 min,centrifugal,through the extraction of HLB small column purification and enrichment in removing impurity concentration after using methanol compound solvent test sample preparation is completed,after separation of ultra high performance liquid chromatograph with triple level 4 bar tandem mass spectrometer test more reactive ion monitoring mode.The 16 biotoxins in this method have good linear relations within the range of 50 ng/mL^1000 ng/mL,the correlation coefficients r2 are all greater than 0.993,the average recovery rate of samples is 90%~120%,and the detection limit is 5 ng/mL^20 ng/mL.The method is accurate,reliable,simple and fast,and can be used for the simultaneous detection of 16 fungal toxins in brewing materials.