QuEChERS结合超高效液相色谱-串联质谱法检测鲫鱼中11 种邻苯二甲酸单酯

doi:10.7506/spkx1002-6630-20250415-118

食品科学 ›› 2025, Vol. 46 ›› Issue (19): 281-289.doi: 10.7506/spkx1002-6630-20250415-118

• 安全检测 • 上一篇

QuEChERS结合超高效液相色谱-串联质谱法检测鲫鱼中11 种邻苯二甲酸单酯

张帅，王钰，谢鹏飞，刘会佳，陈莉君，黄以超，刘开永，周典兵，刘宇欣，刘旭，宋伟

（1.合肥海关技术中心，安徽省食品安全监测与品控重点实验室，安徽合肥 230022；2.安徽医科大学公共卫生学院，安徽合肥 230032）

发布日期:2025-09-16
基金资助:
合肥海关科研项目（2023HFK002）；海关总署科研项目（2024HK109）

Determination of 11 Phthalate Monoesters in Crucian Carp by QuEChERS Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

ZHANG Shuai, WANG Yu, XIE Pengfei, LIU Huijia, CHEN Lijun, HUANG Yichao, LIU Kaiyong, ZHOU Dianbing, LIU Yuxin, LIU Xu, SONG Wei

(1. Anhui Provincial Key Laboratory of Food Safety Monitoring and Quality Control, Technology Center of Hefei Customs, Hefei 230022, China; 2. School of Public Health, Anhui Medical University, Hefei 230032, China)

Published:2025-09-16

摘要/Abstract

摘要： 开发基于QuEChERS法的鲫鱼中邻苯二甲酸单酯（phthalate monoesters，mono-PAEs）的快速前处理体系，结合超高效液相色谱-串联质谱（ultra-high performance liquid chromatography-tandem mass spectrometry，UPLC-MS/MS）建立多残留检测方法。鱼肉样品（1.00 g）经98%乙腈甲酸提取，QuEChERS净化，氮吹近干，乙腈∶水（1∶1，V/V）溶液复溶，过膜，进样分析。11 种mono-PAEs均有良好的线性关系（决定系数R2≥0.999 03）；检出限和定量限分别为3.00 μg/kg和10.00 μg/kg；在10、20、100、200 μg/kg添加量水平下的加标回收实验中，mono-PAEs在鱼肉中的回收率范围分别为68.12%～109.93%、74.43%～112.46%、84.92%～109.48%和82.18%～108.92%，相对标准偏差分别为1.06%～8.50%、0.82%～4.07%、0.63%～2.14%和0.79%～2.66%。该方法重现性良好且回收率符合检测要求，具有操作简便、灵敏度高等特点，可满足鲫鱼基质中多种mono-PAEs的痕量分析需求。

关键词: 邻苯二甲酸单酯；鲫鱼；超高效液相色谱-串联质谱；QuEChERS

Abstract: A rapid sample preparation system based on the quick, easy, cheap, effective, rugged, safe (QuEChERS) method was developed for the multi-residue detection of phthalate monoesters (mono-PAEs) in crucian carp by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples (1.00 g) underwent extraction with 98% acetonitrile in formic acid, purified using the QuEChERS method, blown down to near dryness under nitrogen gas, reconstituted in acetonitrile:water (1:1, V/V) solution, and filtered through a membrane filter before injection for analysis. The calibration curves for 11 mono-PAEs exhibited good linearity (R2 ≥ 0.999 03). The limits of detection and quantification were 3.00 and 10.00 μg/kg, respectively. At four spiked concentration levels of 10, 20, 100 and 200 μg/kg, the recoveries of these mono-PAEs ranged from 68.12% to 109.93%, 74.43% to 112.46%, 84.92% to 109.48%, and 82.18% to 108.92%, respectively, with relative standard deviation (RSD) of 1.06% to 8.50%, 0.82% to 4.07%, 0.63% to 2.14%, and 0.79% to 2.66%, respectively. The method exhibited good reproducibility, its recoveries meeting the testing requirements, was simple to operate and sensitive. Therefore, it could meet the need for the trace analysis of multiple mono-PAEs in crucian carp matrices.

Key words: phthalate monoesters; crucian carp; ultra-high performance liquid chromatography-tandem mass spectrometry; quick, easy, cheap, effective, rugged, safe

中图分类号:

张帅，王钰，谢鹏飞，刘会佳，陈莉君，黄以超，刘开永，周典兵，刘宇欣，刘旭，宋伟. QuEChERS结合超高效液相色谱-串联质谱法检测鲫鱼中11 种邻苯二甲酸单酯[J]. 食品科学, 2025, 46(19): 281-289.

ZHANG Shuai, WANG Yu, XIE Pengfei, LIU Huijia, CHEN Lijun, HUANG Yichao, LIU Kaiyong, ZHOU Dianbing, LIU Yuxin, LIU Xu, SONG Wei. Determination of 11 Phthalate Monoesters in Crucian Carp by QuEChERS Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, 2025, 46(19): 281-289.

QuEChERS结合超高效液相色谱-串联质谱法检测鲫鱼中11 种邻苯二甲酸单酯

Determination of 11 Phthalate Monoesters in Crucian Carp by QuEChERS Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

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