| 超高效液相色谱-串联质谱法同时检测大米中15种常用农药的残留 |
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投稿时间：2018-01-03
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| 引用本文：黄兰淇,陈秀,张正炜,等.超高效液相色谱-串联质谱法同时检测大米中15种常用农药的残留[J].农药学学报,2018,20(3):354-362. |
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| 基金项目:上海市农业技术推广服务中心青年人才成长计划[沪农青字（2016）第4-3号] |
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| 中文摘要:建立一种超高效液相色谱-串联质谱同时检测大米中甲氨基阿维菌素苯甲酸盐等15种常用农药残留的方法，考察了基质效应、提取溶剂种类、提取方法以及不同净化方法对15种农药回收率的影响。样品经V（乙腈）：V（丙酮）：V（水）=16：2：2混合溶液匀浆提取，分散固相萃取法净化，电喷雾正离子（ESI+）模式电离，多反应监测（MRM）模式检测，外标法定量。结果表明：在0.005~1 mg/L范围内，甲氨基阿维菌素苯甲酸盐等15种农药的质量浓度与对应的峰面积间线性关系良好，相关系数（r）≥ 0.99；在0.01、0.1、1和4 mg/kg 4个添加水平下，15种农药在大米中的平均回收率在82%~116%之间，相对标准偏差在1.2%~12%之间（n=5）。方法检出限为0.000 5~0.005 mg/kg，定量限为0.01 mg/kg。用该方法对上海市郊20个批次的大米样品进行测定，均未检出农药残留超标。该方法操作简单、快速、准确，适用于大米中甲氨基阿维菌素苯甲酸盐等15种常用农药残留的同时检测。 |
| 中文关键词:超高效液相色谱-串联质谱 QuEChERS方法 大米 农药 多残留 |
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| Determination of 15 pesticides residues in rice by ultra performance liquid chromatography-tandem mass spectrometry |
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| Abstract:A method was established for the residue detection of 15 pesticides in rice by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The influences of the matrix effects, the types of extraction solvent, extraction methods and different purification methods were all investigated. After homogenized mixing, samples were extracted by V (acetonitrile):V (acetone):V (water)=16:2:2 and cleaned up by disperse solid phase extraction. The samples were then detected by MS/MS with positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode and quantified by external standard method. The results showed that the correlation coefficient (r) of 15 pesticides including emamectin benzoate were higher than 0.99 in the concentration ranged from 0.005 mg/L to 1 mg/L. The mean spiked recoveries of 15 pesticides at 0.01, 0.1, 1 and 4 mg/kg spiked levels ranged from 82% to 116% with the relative standard deviations (RSD, n=5) between 1.2% and 12%. The limits of detection were 0.000 5-0.005 mg/kg, and the limits of quantitation for the method were 0.01 mg/kg. Twenty batches of rice from the outskirts of Shanghai municipality were determined by the established method. Excessive pesticide residues were not detected in all the rice samples. This new method is practical, fast and accurate, which meets the requirements for the determination of 15 pesticides including emamectin benzoate in rice at the same time. |
| Key words:ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) QuEChERS method rice pesticide multi-residue |
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