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微热助吹扫捕集-超高压液相色谱-串联质谱法快速测定蔬菜中12种半挥发性农药残留

Rapid determination of 12 semi-volatile pesticide residues in vegetables by miniaturized thermal-assisted purge-and-trap coupled with ultra high pressure liquid chromatography-tandem mass spectrometry

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【作者】 陈正毅李运达张卓旻李攻科

【Author】 CHEN Zhengyi;LI Yunda;ZHANG Zhuomin;LI Gongke;School of Chemistry, Sun Yat-sen University;

【通讯作者】 张卓旻;李攻科;

【机构】 中山大学化学学院

【摘要】 将微热助吹扫捕集技术与超高压液相色谱-串联质谱(UHPLC-MS/MS)结合,建立了蔬菜中12种半挥发性农药残留的快速分析方法。系统优化了前处理条件,在10 min内即可完成样品前处理过程。12种半挥发性农药残留在各自范围内线性关系良好,相关系数(R~2)为0.991 8~0.999 7;检出限为0.3~1.3μg/kg,定量限为1.0~4.3μg/kg。实际样品的加标回收率为80.0%~120.0%,日内和日间精密度均小于10%。该方法具有基质净化效果好、前处理过程简单和分析速度快等优点,可用于蔬菜中多种半挥发农药残留的同时快速分析。

【Abstract】 A method for the analysis of 12 semi-volatile pesticide residues in vegetables was developed by miniaturized thermal-assisted purge-and-trap coupled with ultra high pressure liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS). Under the optimized conditions, the sample preparation could be completed within 10 min. The linear relationships of the 12 semi-volatile pesticide residues were good within their corresponding concentration ranges. The correlation coefficients were in range of 0.991 8-0.999 7. The limits of detection and limits of quantification were in range of 0.3-1.3 μg/kg and 1.0-4.3 μg/kg, respectively. The recoveries ranged from 80.0% to 120.0%, with intra-day and inter-day RSDs of less than 10%. This proposed method is quick and simple, and is suitable for the simultaneous and rapid analysis of semi-volatile pesticide residues in vegetables.

【基金】 国家自然科学基金(21675178,21575167,21976213);广东省公益研究与能力建设专项基金(2015A030401036);广州市科技计划项目(201604020165);广东省食品安全重点领域研发计划(2019B020211001)~~
  • 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2020年01期
  • 【分类号】O657.63;TS255.7
  • 【被引频次】4
  • 【下载频次】206
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