QuEChERS-气相色谱-三重四极杆质谱法同时测定黑茶中10种酰胺类除草剂残留

Simultaneous determination of 10 kinds of amide herbicide residues in dark tea by QuEChERS with Gas Chromatography-Triple Quadrupole Mass Spectrometry

目的:建立QuEChERS前处理净化技术结合气相色谱-三重四极杆质谱法(GC-MS/MS)同时测定黑茶中10种酰胺类除草剂的检测方法。方法:样品经乙腈提取后,经QuEChERS净化,以TG-5 SIL MS色谱柱(30 m×0.25 mm×0.25μm)分离,采用多反应监测(MRM)模式对酰胺类除草剂进行分析,基质匹配外标法定量。结果:10种酰胺类除草剂在质量浓度0.001~0.500 mg/L内线性关系良好,相关系数(R 2)>0.999;检出限和定量限分别为0.001~0.002,0.002~0.008 mg/kg;平均回收率为80.3%~103.2%,相对标准偏差为0.9%~7.3%(n=6)。结论:该方法适用于黑茶中酰胺类除草剂的快速检测分析。

Objective:A method for simultaneous determination of 10 amide herbicide residues in dark tea was developed by QuEChERS method coupled with gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS).Methods:After being extracted by acetonitrile and purified by QuChERS,the samples were separated by TG-5 SIL MS column(30 m×0.25 mm×0.25μm),then detected bymultiple reaction monitoring mode(MRM).Blank matrix matching standard curve was used in quantitative analysis.Results:The calibration curves had a good liner relationship in the range of 0.001~0.500 mg/L with the correlation coefficients greater than 0.999.The limits of detection(LODs)and limits of quantitation(LQDs)of the method were in the range 0.001~0.002 mg/kg and 0.002~0.008 mg/kg,respectively.The average recoveries were 80.3%~103.2%,and the relative standard deviations were between 0.9%and 7.3%.Conclusion:The method can be applied to the simultaneous detection of amide herbicides in dark tea.