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基于QuEChERS-高效液相色谱串联质谱法测定水果中44种农药残留

Determination of 44 Pesticide Residues in Fruits Based on QuEChERS-High Performance Liquid Chromatography Tandem Mass Spectrometry

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【作者】 张方圆丁少曼李欣洁吴伟聪何杞悦方丽

【Author】 ZHANG Fangyuan;DING Shaoman;LI Xinjie;WU Weicong;HE Qiyue;FANG Li;Guangdong Provincial Engineering Research Center for Efficacy Component Testing and Risk Substance Rapid Screening of Health Food; Institute of Analysis, Guangdong Academyof Sciences (China National Analytical Center, Guangzhou), Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology;

【通讯作者】 丁少曼;方丽;

【机构】 广东省科学院测试分析研究所(中国广州分析测试中心),广东省化学测量与应急检测技术重点实验室,广东省保健食品功效成分检测与风险物质快速筛查工程技术研究中心

【摘要】 基于QuEChERS(Quick, Easy, Cheap, Effective, Rugged and Safe)-高效液相色谱串联质谱技术(High performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS),建立了测定水果中44种农药残留的方法。对样品的提取溶剂、净化方式进行了改良,同时对液相色谱条件和质谱采集参数进行了优化,并对基质效应进行了分析和评价。采用乙腈为提取溶剂,QuEChERS(900mg MgSO4+150 mg PSA)净化,HPLC-MS/MS测定,基质匹配标准曲线定量。在0~100 ng/mL浓度范围内,线性关系良好,相关系数(R2)>0.99。44种农药的检出限为0.0001~1.0μg/kg,定量限为0.0005~3.4μg/kg。3水平加标试验的回收率为70.3%~119.6%,相对标准偏差为0.8%~19.0%。方法前处理简单、分析快速、定量准确、灵敏度高,适用于水果中多农药残留的测定。

【Abstract】 Based on QuEChERS(Quick, Easy, Cheap, Effective, Rugged and Safe)-high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS), a method for the determination of 44 pesticide residues in fruits was established. The extraction solvent and purification methods of the samples were improved, the liquid chromatography conditions and mass spectrometry collection parameters were optimized, and the matrix effects were analyzed and evaluated. Acetonitrile was used as the extraction solvent, QuEChERS(900 mg MgSO4+150 mg PSA) was used to purification, followed by determination using HPLC-MS/MS, and then, matrix matching standard curve quantification was performed. The linear relationship of 44 pesticides was good within the concentration range of 0–100 ng/mL, with a correlation coefficient(R~2)>0.99. The detection limit was 0.0001–1.0 μg/kg, with a quantitation limit of 0.0005–3.4 μg/kg. The recoveries for the three-level spiking test were 70.3%–119.6%,and the relative standard deviation(RSD) was 0.8%–19.0%. The method has the advantages of simple pretreatment, rapid analysis, accurate quantification, and high sensitivity, rengering it suitable for the determination of multi pesticide residues in fruits.

【基金】 广东省重点领域研发计划“食品安全”重点专项(2019B020211001)
  • 【文献出处】 食品科技 ,Food Science and Technology , 编辑部邮箱 ,2023年11期
  • 【分类号】O657.63;TS255.7
  • 【被引频次】1
  • 【下载频次】223
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