MPFC-QuECHERS结合超高效液相色谱串联质谱法快速测定铁皮石斛中56种农药残留
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(1. 贵州省分析测试研究院,贵州 贵阳 550014;2. 贵州省装备制造职业学院,贵州 贵阳 550081;3. 贵州省检测技术研究应用中心,贵州 贵阳 550014)

作者简介:

李占彬,男,贵州省分析测试研究院副研究员,博士。

通讯作者:

陆洋(1969—),男,贵州省分析测试研究院研究员,硕士。E-mail:luyang98@163.com

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基金项目:

贵州省科技支撑计划项目(编号:黔科合服企[2021]6号);中央引导地方科技发展资金(编号:黔科中引地[2021]4026);贵州省科技创新平台(编号:黔科合服企[2019]4001)


Rapid determination of 56 pesticide residues in Dendrobium officinale by MPFC-QuEChERS method combined with ultra-performance liquid chromatography-tandem mass spectrometry
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(1. Guizhou Academy of Testing Analysis, Guiyang, Guizhou 550014, China; 2. Guizhou Equipmet Manufacturing Vocational College, Guiyang, Guizhou 550081, China; 3. Guizhou Testing Technology Research and Application Center, Guiyang, Guizhou 550014, China)

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    摘要:

    目的:对铁皮石斛的农药残留量进行风险分析与评估。方法:建立了超滤型净化分散固相萃取(MPFC-QuEChERS)结合超高效液相色谱—串联质谱法快速测定铁皮石斛中56种农药残留的分析方法。样品经0.1%甲酸—乙腈溶液提取,QuEChERS盐析包分层,经超滤净化柱单步净化,采用电喷雾正负离子切换(ESI),动态多反应监测(DMRM)模式进行分析,基质外标法定量。结果:56种农药残留在1.0~250.0 μg/L线性范围内线性关系良好(R2>0.99)。方法的检出限(LOD)为1~5 μg/kg,定量限(LOQ)为3.0~15.0 μg/kg。56种农药残留在各自定量限1,2,10倍加标水平下,平均回收率为75.1%~107.0%,相对标准偏差(RSD)为2.7%~18.9%。采用该方法对20批次铁皮石斛中农药残留进行检测,结果显示,5份样品中检出烯酰吗啉、嘧菌酯、腈苯唑、丙环唑、苯醚甲环唑、啶氧菌酯6种农药,含量范围在0.066 7~1.872 mg/kg。结论:超滤型净化QuEChERS结合超高效液相色谱—串联质谱法测定农药残留具有前处理简单、快速高效等优特点,可用于铁皮石斛中多种农药残留快速筛查和分析。

    Abstract:

    Objective: In order to analyze the risk of pesticide residues in D. officinale, a method for rapid determination of 56 pesticide residues in D. officinale by a kind of ultrafiltration purification column(MPFC-QuEChERS) combined with ultra-performance liquid chromatography- tandem mass spectrometry(UHPLC-MS/MS)was developed. Methods: The samples were extracted with acetonitrile contained 0.1% formic acid, salted out, shaken, centrifuged, and single-step purified by a MPFC-QuEChERS purification column. Mass spectrometer was operated in the positive and negative ion mode using select reaction monitoring for qualitative and quantitative analysis. Results: The result showed that, the 56 kinds of pesticides showed good linearity when they were in 1.0~250.0 μg/L (R2>0.99). The limits of detection (LOD) was 1~5 μg/kg. Three levels of 1, 2 and 10 times of LOQ were added to the sample, the average recovery of each substance in D. officinale was 75.1% to 107.0%, of which the RSDs were 2.7%~18.9%. Conclusion: This method was used to detect pesticide residues in 20 batches of D. officinale. The results showed that 6 kinds of pesticides were detected in 5 samples with the contents ranging from 0.066 7 mg/kg to 1.872 mg/kg. The method is simple, fast and efficient, and could be used for rapid screening and analysis of pesticide residues in D. officinale.

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李占彬,赵丽君,黄永桥,等. MPFC-QuECHERS结合超高效液相色谱串联质谱法快速测定铁皮石斛中56种农药残留[J].食品与机械,2023,39(7):48-55,84.
LI Zhan-bin, ZHAO Li-jun, HUANG Yong-qiao, et al. Rapid determination of 56 pesticide residues in Dendrobium officinale by MPFC-QuEChERS method combined with ultra-performance liquid chromatography-tandem mass spectrometry[J]. Food & Machinery,2023,39(7):48-55,84.

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  • 收稿日期:2022-11-04
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  • 在线发布日期: 2023-10-20
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