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中国精品科技期刊2020
杨志敏, 吴福祥, 许晓辉, 许淑琴, 陈婷, 丁辉. 基于动态多反应监测模式下的高效液相色谱-串联质谱法同时测定枸杞中44种农药残留[J]. 食品工业科技, 2020, 41(1): 201-208. DOI: 10.13386/j.issn1002-0306.2020.01.032
引用本文: 杨志敏, 吴福祥, 许晓辉, 许淑琴, 陈婷, 丁辉. 基于动态多反应监测模式下的高效液相色谱-串联质谱法同时测定枸杞中44种农药残留[J]. 食品工业科技, 2020, 41(1): 201-208. DOI: 10.13386/j.issn1002-0306.2020.01.032
YANG Zhi-min, WU Fu-xiang, XU Xiao-hui, XU Shu-qin, CHEN Ting, DING Hui. Determination of 44 Kinds of Pesticide Residues in Wolfberry by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Dynamic Multi-reaction Monitoring[J]. Science and Technology of Food Industry, 2020, 41(1): 201-208. DOI: 10.13386/j.issn1002-0306.2020.01.032
Citation: YANG Zhi-min, WU Fu-xiang, XU Xiao-hui, XU Shu-qin, CHEN Ting, DING Hui. Determination of 44 Kinds of Pesticide Residues in Wolfberry by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Dynamic Multi-reaction Monitoring[J]. Science and Technology of Food Industry, 2020, 41(1): 201-208. DOI: 10.13386/j.issn1002-0306.2020.01.032

基于动态多反应监测模式下的高效液相色谱-串联质谱法同时测定枸杞中44种农药残留

Determination of 44 Kinds of Pesticide Residues in Wolfberry by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Dynamic Multi-reaction Monitoring

  • 摘要: 目的:建立一种基于动态多反应监测模式同时检测枸杞中44种农药残留的高效液相色谱-串联质谱的分析方法。方法:样品经10 mL超纯水复水,用0.1%甲酸-乙腈提取,经PSA、C18、MgSO4填料净化,T3色谱柱分离,0.1%甲酸水和乙腈流动相体系梯度洗脱,在正离子模式下采用动态多反应监测模式(d-MRM)检测,基质匹配外标法定量。结果:44种农药在0.002~0.200 mg/L范围内线性关系良好(R2>0.9943),方法检出限范围为0.01~3.30 μg/kg,3个添加水平的回收率为60.2%~115.3%,相对标准偏差为0.63%~8.27%。测定了市售枸杞样品20批,共检出农药残留14种,其中多菌灵、啶虫脒、吡虫啉的检出率高达95%。结论:该方法操作快速、简便、准确、可靠,适用于枸杞中44种农药残留的同时检测。

     

    Abstract: Objective:An analysis method for the simultaneous determination of 44 kinds of pesticide residues in wolfberry was established by high performance liquid chromatography-tandem mass spectrometry with dynamic multi-reaction monitoring. Methods:The samples were rehydrated with 10 mL uitra-pure water,extracted with acetonitrile(containing 1% formic acid),purified up with PSA,C18 and MgSO4,separated by a T3 column with 0.1% formic acid solution and acetonitrile as the mobile phases in gradient program,analyzed using HPLC-MS/MS in dynamic multiple reaction monitoring(d-MRM)mode and quantified by matrix-matched external standard method. Results:The 44 kinds of pesticides showed good linearity when they were in 0.002~0.200 mg/L(R2>0.9943). The limits of detection of the 44 kinds of pesticides were in 0.01~3.30 μg/kg,the recoveries were within 60.2%~115.3%,RSD were 0.63%~8.27%. The pesticide residues in the samples of wolfberry purchased from the market were detected by this method,a total of 14 kinds of pesticide residues were detected,and the detection rate of carbendazim,chlorphenamidine,imidacloprid were up to 95%. Conclusions:The method was rapid,simple,accurate and reliable. It was suitable for simultaneous detection of 44 kinds of pesticide residues in wolfberry.

     

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