改良的QuEChERS-气相色谱-质谱联用法测定茶叶中多种农药残留
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摘要
建立了以QuEChERS作为前处理方法,气相色谱/质谱联用法同时测定茶叶中33种农药残留的检测方法。样品经改进的QuEChERS法进行提取净化,采用DB-5MS(30m×0.25mm×0.25μm)毛细管色谱柱分离,选择离子模式下同时测定,外标法定量。33种农药残留在0.01~3.00mg/L范围内线性关系良好,相关系数均大于0.999。方法的检出限为4.0~35μg/kg,样品平均添加回收率为82.7%~103.8%,相对标准偏差为0.73%~6.8%。方法适用于茶叶中毒死蜱、联苯菊酯等33种不同类型农药残留的同时检测。
A method was developed for simultaneous determination of 33 pesticide residues in tea by using Qu ECh ERS-GC/MS. The samples were extracted and purified by improved Qu ECh ERS method.The 33 pesticide residues were separated by DB-5 MS( 30 m × 0. 25 mm × 0. 25 μm) capillary chromatographic column,and then determined by selected ion mode with external standard method.The linear ranges of the method were 0. 01 ~ 3. 00 mg/L for the 33 pesticide residues. The correlation coefficients were more than 0. 999 for all the pesticide residues. The limits of detection were 4 ~35 μg/kg. The average recoveries were 82. 7% ~ 103. 8%. The relative standard deviations were0. 73% ~ 6. 8%. The method is stable,accurate,simple and timesaving,and can be used for the simultaneous determination of 33 different pesticide residues in tea samples.
A method was developed for simultaneous determination of 33 pesticide residues in tea by using Qu ECh ERS-GC/MS. The samples were extracted and purified by improved Qu ECh ERS method.The 33 pesticide residues were separated by DB-5 MS( 30 m × 0. 25 mm × 0. 25 μm) capillary chromatographic column,and then determined by selected ion mode with external standard method.The linear ranges of the method were 0. 01 ~ 3. 00 mg/L for the 33 pesticide residues. The correlation coefficients were more than 0. 999 for all the pesticide residues. The limits of detection were 4 ~35 μg/kg. The average recoveries were 82. 7% ~ 103. 8%. The relative standard deviations were0. 73% ~ 6. 8%. The method is stable,accurate,simple and timesaving,and can be used for the simultaneous determination of 33 different pesticide residues in tea samples.
引文
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[13]Gao Y L,Guo X J,Qiao S,et al.J.Tea Sci.,2017,37(3):243高玉玲,郭秀娟,乔石,等.茶叶科学,2017,37(3):243
[14]GB 23200.8-2016 Determination of 500 pesticides and related chemicals residues in fruits and vegetables.GB 23200.8-2016水果和蔬菜中500种农药及相关化学品残留量的测定.
[15]Liu Y M,Ge N,Wang F,et al.Chinese J.Chromatogr.,2012,33(8):782刘永明,葛娜,王飞,等.色谱,2012,33(8):782
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