高效液相色谱–串联质谱法同时测定土壤中8种杀菌剂残留

Simultaneous determination of 8 bactericide residues in soil by high performance liquid chromatography–tandem mass spectrometry

建立高效液相色谱-串联质谱法同时测定土壤中戊唑醇、腈菌唑、腈苯唑、氟硅唑、三唑酮、丙环唑、烯唑醇、苯醚甲环唑8种杀菌剂残留量的方法。采用QuEChERS样品前处理方法对土壤样品进行提取、净化和富集,用电喷雾离子源、正负离子扫描,以多反应监测(MRM)模式进行定性和定量分析。在优化的实验条件下,8种杀菌剂的质量浓度在0.01~0.50 mg/L范围内与色谱峰面积均成良好的线性关系,相关系数均大于0.995,方法检出限为0.005~0.010 mg/kg。样品平均加标回收率为85.6%~102.2%,测定结果的相对标准偏差为4.6%~13.2%(n=5)。该方法操作简便,灵敏度和准确度高,满足土壤中戊唑醇等8种杀菌剂残留量的测定要求。

A high performance liquid chromatography-tandem mass spectrometry was established for the simultaneous determination of 8 fungicides,such as tebuconazole,acetonitrile,nitrilazole,flusilazole,triazolone,propiconazole,enazol and phenyl ether in soil.The QuEChERS sample pretreatment method was used to extract,purify and enrich for soil samples.The qualitatively and quantitatively analysis were performed by electrospray ionization source,positive and negative ions scanning,and multi response monitoring(MRM) mode.Under the optimized experimental conditions,the mass concentration of 8 fungicides had a good linear relationship with the chromatographic peak area in the range of 0.01-0.50 mg/L,the correlation coefficients were all more than 0.995,and the detection limit of the method was 0.005-0.010 mg/kg.The average recoveries of standard addition were 85.6%-102.2%,and the relative standard deviations of the determination results were 4.6%-13.2%(n=5).The method is simple,sensitive and accurate,and can meet the requirements for the determination of eight fungicides residues in soil such as tebuconazole.