基于GC-MS/MS的柑橘中农药残留测定及干扰物鉴定  

Determination of Pesticide Residues in Citrus and Identification of Interferents Based on GC-MS/MS

作　　者：王多娇 张圆 李岩 陈民辉 张渊 万素琴 WANG Duojiao;ZHANG Yuan;LI Yan;CHEN Minhui;ZHANG Yuan;WAN Suqin(Jiangsu Institute for Food and Drug Control,Nanjing 210008,China)

机构地区：[1]江苏省食品药品监督检验研究院,江苏南京210008

出　　处：《现代食品》2025年第3期189-196,共8页Modern Food

摘　　要：目的:建立基于改良QuEChERS前处理技术结合气相色谱-串联质谱(Gas Chromatography-Tandem Mass Spectrometry,GC-MS/MS)的检测方法,用于柑橘中42种农药残留的分析,同时通过质谱图库比对解决柠檬中水胺硫磷、沃柑中氯唑磷检测时出现的假阳性干扰问题。方法:在优化提取溶剂及提取温度后,通过冷冻、萃取、净化、氮吹浓缩等步骤制备样品;复溶后采用VF1701色谱柱(30 m×0.25 mm,0.25μm)分离,GC-MS/MS动态多反应监测模式采集数据,结合基质匹配标准曲线与内标法定量。针对假阳性干扰物,切换至全扫描模式,利用NIST质谱库进行谱图匹配与结构鉴定。结果:该方法线性关系良好,定量限、加标回收率及精密度均符合多残留检测要求。通过全扫描模式结合NIST数据库,确认水胺硫磷与氯唑磷的假阳性干扰物来源于柑橘基质中的共提取成分,有效避免了误判。结论:该方法兼具高灵敏度和抗干扰能力,不仅适用于柑橘中农药残留的定量检测,还为农药残留检测中未知化合物的鉴定提供了新思路,对提升检测结果可靠性具有重要意义。Objective:To establish a detection method based on a modified QuEChERS pretreatment technique coupled with gas chromatography-tandem mass spectrometry(GC-MS/MS)for the analysis of 42 pesticide residues in citrus fruits.Additionally,to address false-positive interference issues observed in the detection of isocarbophos in lemons and chlorethoxyfos in orah mandarin through mass spectral library matching.Method:After optimizing the extraction solvent and extraction temperature,the samples were prepared through freezing,extraction,purification,and nitrogen blowing concentration.After reconstitution,separation was performed using a VF1701 chromatographic column(30 m×0.25 mm,0.25μm),with data acquired in dynamic multiple reaction monitoring mode via GC-MS/MS.Quantification was achieved using matrix-matched standard curves and the internal standard method.For false-positive interference,the full scan mode was employed,and structural identification of co-extracted matrix components was conducted using the NIST mass spectral library.Result:The method demonstrated good linearity,with limits of quantification,spiked recoveries,and precision meeting the requirements for multi-residue detection.Full scan mode combined with the NIST library confirmed that false-positive interferences for isocarbophos and chlorethoxyfos originated from co-extracted matrix components in citrus,effectively avoiding misidentification.Conclusion:This method combines high sensitivity and anti-interference capability,making it suitable for both quantitative detection of pesticide residues in citrus and the identification of unknown compounds in pesticide analysis.It provides a novel approach to enhance the reliability of detection results,holding significant importance for improving analytical accuracy.

关 键 词：气相色谱-串联质谱 农药残留 干扰物 鉴定 

分 类 号：O657.63[理学—分析化学]