颜鸿飞, 李拥军, 王美玲, 戴华. 微波辅助萃取-分散固相萃取-气相色谱质谱法测定茶叶中23种农药残留[J]. 分析测试技术与仪器, 2013, 19(4): 206-213.
引用本文: 颜鸿飞, 李拥军, 王美玲, 戴华. 微波辅助萃取-分散固相萃取-气相色谱质谱法测定茶叶中23种农药残留[J]. 分析测试技术与仪器, 2013, 19(4): 206-213.
YAN Hong-fei, LI Yong-jun, WANG Mei-ling, DAI Hua. Residual Analysis of 23 Pesticides in Tea by Microwave Assisted Extraction/Dispersive Solid Phase Extraction Purification and Gas Chromatography-mass Mpectrometry[J]. Analysis and Testing Technology and Instruments, 2013, 19(4): 206-213.
Citation: YAN Hong-fei, LI Yong-jun, WANG Mei-ling, DAI Hua. Residual Analysis of 23 Pesticides in Tea by Microwave Assisted Extraction/Dispersive Solid Phase Extraction Purification and Gas Chromatography-mass Mpectrometry[J]. Analysis and Testing Technology and Instruments, 2013, 19(4): 206-213.

微波辅助萃取-分散固相萃取-气相色谱质谱法测定茶叶中23种农药残留

Residual Analysis of 23 Pesticides in Tea by Microwave Assisted Extraction/Dispersive Solid Phase Extraction Purification and Gas Chromatography-mass Mpectrometry

  • 摘要: 建立了微波辅助萃取-分散固相萃取净化-气相色谱质谱法(GC-MS)快速测定茶叶中23种农药残留量的方法. 茶叶样品用乙腈进行微波辅助萃取(MAE),提取液经分散固相萃取(DSPE)净化处理. 采用DB-17MS毛细管色谱柱分离后,选择离子监测模式下(SIM)质谱法进行测定. 23种农药组分在0.01~0.50 mg/mL质量浓度范围内呈线性关系,相关系数r2大于0.995,方法测定低限(10S/N)为0.005~0.01 mg/kg. 以空白绿茶为基体,在4个标准添加水平0.01、0.05、0.10、0.25 mg/kg进行加标回收试验,加标平均回收率为70%~105%,相对标准偏差为3.0%~8.2%.

     

    Abstract: A gas chromatographic-mass spectrometric(GC-MS) method has been developed for the simultaneous determination of 23 pesticide residues in tea. The pesticides included organophosphorus,pyrethroids and herbicides pesticides. The target analytes were extracted with acetonitrile using the microwave-assisted extraction(MAE) and the cleaned up using the dispersive solid phase extraction (DSPE).After being separated on a DB-17 MS capillary column, the target analytes were detected by GC-MS under the selected ion monitoring (SIM) mode and were quantified by the internal standard method. The correlation coefficents (r2) of 23 pesticides were greater than 0.995 in the concentration range of 0.01 to 0.50 mg/L. The limits of quantitation (LOQ) were varied from 0.005 to 0.01 mg/kg. It was found that the average recoveries ranged from 70% to 105% at the four spiked levels of 0.01,0.05,0.10,0.25 mg/kg in blank green tea, and their relative standard deviations (RSDs) were from 3.0% to 8.2% under optimized conditions.

     

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