新型脱脂前处理技术联合净化-同位素稀释-超高效液相色谱-串联质谱法测定花生中15种真菌毒素  

Simultaneous determination of 15 mycotoxins in peanuts by ultra high performance liquid chromatography-tandem mass spectrometry with QuEChERS EMR-Lipid approach and stable isotope dilution

作　　者：潘晨[1] 于建[1] 吴思霖 简龙海[1] 郑荣[1] 王柯[1] PAN Chen;YU Jian;WU Si-lin;JIAN Long-hai;ZHENG Rong;Wang Ke(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《上海预防医学》2020年第5期368-374,共7页Shanghai Journal of Preventive Medicine

基　　金：上海市科委长三角科技联合攻关领域项目(18395810300)。

摘　　要：【目的】建立新型脱脂前处理(QuEChERS EMR-Lipid)技术联合净化-同位素稀释-超高效液相色谱-串联质谱法检测花生中15种真菌毒的方法。【方法】样品用含2%甲酸的乙腈-水(50∶50,V/V)溶液提取,通过QuEChERS EMR-Lipid技术净化后,以五氟苯基柱为分离柱,用甲醇-0.01%甲酸水溶液进行梯度洗脱,采用超高效液相色谱-串联质谱(UPLC-MS/MS)测定、多反应模式(MRM)监测和同位素内标法定量。【结果】该方法测定花生中15种真菌毒素在一定范围内线性良好(r>0.995),检出限为0.1~10μg/kg,平均回收率为81.2%~115.3%,相对标准偏差(RSD,n=6)为2.1%~10.7%。【结论】该方法操作简便、灵敏度高,适用于花生中15种真菌毒素的快速准确检测。[Objective]To develop a method for the simultaneous determination of 15mycotoxins in peanuts by ultra high performance liquid chromatography-tandem mass spectrometry with QuEChERS EMR-Lipid approach and stable isotope dilution.[Methods]The samples were extracted by 2%formic acid acetonitrile-water(50∶50,V/V)and then purified with QuEChERS EMR-Lipid approach.The mycotoxins were fully separated on a pentafluorophenyl column under a gradient elution with methonal-0.01%formic acid aqueous solution.The mycotoxins were analyzed by UPLC-MS/MS with multiple reaction monitoring(MRM)mode and quantified by isotope internal standard method.[Results]Fifteen mycotoxins had good linear relationship in the certain correlation ranges with the correlation coefficients all above 0.995 and the detection limits were 0.1-10μg/kg.The mean recoveries ranged from 81.2%to 115.3%with RSD(n=6)varying from 2.1%to 10.7%.[Conclusion]The method is simple,highly sensitive,practical,and proves to be suitable for quantitative analysis of 15 mycotoxins in peanuts.

关 键 词：新型脱脂前处理 同位素稀释 超高效液相色谱-串联质谱法 真菌毒素 花生 

分 类 号：R114[医药卫生—卫生毒理学]