QuEChERS处理-超高效液相色谱-串联质谱法快速检测鲜乳中54 种农药残留

doi:10.7506/rykxyjs1671-5187-20240816-080

乳业科学与技术 ›› 2024, Vol. 47 ›› Issue (6): 43-50.DOI: 10.7506/rykxyjs1671-5187-20240816-080

QuEChERS处理-超高效液相色谱-串联质谱法快速检测鲜乳中54 种农药残留

杨琦，焦昕哲，孟虎，房忠芳，张耀武，赵丽莉，张倩婷

（1.西安市产品质量监督检验院，陕西西安 710065；2.西安市质量与标准化研究院，陕西西安 710065；3.富平县检验检测中心，陕西富平 711700）

出版日期:2024-12-04 发布日期:2024-12-04

Rapid Determination of 54 Pesticide Residues in Fresh Milk by QuEChERS Pretreatment and Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

YANG Qi, JIAO Xinzhe, MENG Hu, FANG Zhongfang, ZHANG Yaowu, ZHAO Lili, ZHANG Qianting

(1. Xi’an Supervision and Inspection Institute of Product Quality, Xi’an 710065, China; 2. Xi’an Institute of Quality and Standardization, Xi’an 710065, China; 3. Fuping County Inspection and Testing Center, Fuping 711700, China)

Published:2024-12-04 Online:2024-12-04

摘要/Abstract

摘要： 建立鲜乳中54 种农药残留的快速检测方法。采用QuEChERS（quick, easy, cheap, effective, rugged, safe）处理，超高效液相色谱-串联质谱进行高通量检测分析。对流动相、提取溶剂、提取溶剂体积、提取盐包配方、净化包配方分别进行优化，同时进行基质效应和方法学评价。结果显示，54 种目标物的线性范围为5.0～100.0 μg/L，相关系数（r）均大于0.999，定量限均为10.0 μg/kg，加标平均回收率为67.78%～119.38%，测定值相对标准偏差（n＝6）均小于9%。该方法简便、快速，灵敏度、准确度高，能够满足鲜乳中54 种农药残留的高通量检测分析要求。

关键词: QuEChERS处理；超高效液相色谱-串联质谱法；农药残留；鲜乳

Abstract: A high-throughput method for the screening and quantitation of 54 pesticide residues in fresh milk was developed by quick, easy, cheap, effective, rugged, safe (QuEChERS) extraction followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The study optimized the composition of mobile phase, extraction solvent, extraction solvent volume, extraction salt packet formulation, and purification packet formulation. Furthermore, the matrix effect was evaluated and methodological evaluation were carried out. The results showed that the linear range was 5.0–100.0 μg/L for all 54 pesticides, with correlation coefficients (r) higher than 0.999. The limit of quantification (LOQ) was 10.0 μg/kg for all target analytes, and the average recoveries from spiked samples were 67.78%–119.38%, with relative standard deviations (RSDs) (n = 6) lower than 9%. The method is simple, rapid, sensitive, and accurate. It can meet the requirements of the simultaneous detection and analysis of 54 pesticide residues in fresh milk.

Key words: quick, easy, cheap, effective, rugged, safe pretreatment; ultra-high performance liquid chromatography-tandem mass spectrometry; pesticide residues; fresh milk

中图分类号:

TS252.7

杨琦，焦昕哲，孟虎，房忠芳，张耀武，赵丽莉，张倩婷. QuEChERS处理-超高效液相色谱-串联质谱法快速检测鲜乳中54 种农药残留[J]. 乳业科学与技术, 2024, 47(6): 43-50.

YANG Qi, JIAO Xinzhe, MENG Hu, FANG Zhongfang, ZHANG Yaowu, ZHAO Lili, ZHANG Qianting. Rapid Determination of 54 Pesticide Residues in Fresh Milk by QuEChERS Pretreatment and Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Journal of Dairy Science and Technology, 2024, 47(6): 43-50.

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QuEChERS处理-超高效液相色谱-串联质谱法快速检测鲜乳中54 种农药残留

Rapid Determination of 54 Pesticide Residues in Fresh Milk by QuEChERS Pretreatment and Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

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