UPLC-MS/MS检测烟草中腈菌唑残留

该文采用Qu ECh ERS方法提取净化烟草样品,建立了超高效液相色谱-串联质谱(UPLC-MS/MS)检测烟草中腈菌唑的残留分析方法。以1%乙酸乙腈提取溶剂,PSA和GCB作为净化剂,超高效液相色谱分离,电喷雾电离、正离子扫描,三重四级杆串联质谱以多反应监测扫描方式进行检测,以碎片离子对m/z289.116/70.028进行定性分析、m/z 289.116/125.041进行基质匹配标准品的外标法定量。标准曲线线性方程为Y=21295x+156791,R2=0.9991,其线性范围在1~500μg·L-1。结果表明,在0.01~5mg·kg-1添加水平范围内,腈菌唑在烟草中平均回收率在88.3%~93.0%,变异系数在5.2%~7.3%,检出限(LOD)为0.029μg·kg-1,定量限(LOQ)为0.03μg·kg-1。该方法简单、快速,适用于大量烟草样品中腈菌唑的残留检测。

Determination of Myclobutanil Residues in Tobacco Using UPLC-MS/MS

A rapid and sensitive analytical method for determination of myclobutanil residues in tobacco samples has been established based on QuEChERS and UPLC-MS/MS.The sample was extracted by 1%acetic acid acetonitrile and then purified by primary secondary amine(PSA)and graphitized carbon black(GCB).The mass spectrometerw as operated with electrospray in the positive ion mode( ESI+).The myclobutanil were quantified by external stan-dard method and matched standard solution used to compensate for matrix effect.The myclobutanil results were on the intension of the characteristic m/z 289.116/70.028 ion and m/z 289.116/125.041 ion .Under the optimal condi-tions ,the calibration curve showed a good linearity in the range of 1~500μg · L- 1 with a correlation coefficient of 0. 9991 Average recoveries of myclobutanil in tobacco at three levels (0.01mg · kg-1,0.5mg · kg-1 and 5mg · kg-1) ranged from 88.3%to 93.0%with relative standard deviations(RSDs)from 5.2%to 7.3%(n=5).Limits of detec-tions(LOD)of thifluzamide were 0.029μg·kg-1,while limits of quantifications(LOQ)were 0.03μg·kg-1,respective-ly.The method is simple,rapid and accurate,and it can meet the requirements of the domestic and international legis-lation.The method adapts to confirm residues of thifluzamide in rice,corn and potato.