QuEChERS-气相色谱-串联质谱法测定红糖中172种农药残留  

Determination of 172 kinds of pesticide residues in brown sugar by QuEChERS-gas chromatography-tandem mass spectrometry

作　　者：杨昆 黄咪孙 蔡翔宇 覃金兰 黄恺 秦泽华 YANG Kun;HUANG Mi-Sun;CAI Xiang-Yu;QIN Jin-Lan;HUANG Kai;QIN Ze-Hua(Technical Center of Nanning Customes District,Nanning 530201,China;School of Public Health,Guangxi Medical University,Nanning 530021,China;Nanning Intellectual Property Protection Center,Nanning 530028,China)

机构地区：[1]南宁海关技术中心,南宁530201 [2]广西医科大学公共卫生学院,南宁530021 [3]南宁市知识产权保护中心,南宁530028

出　　处：《食品安全质量检测学报》2025年第4期97-103,共7页Journal of Food Safety and Quality

基　　金：南宁海关科技计划项目(2023NNHG05)。

摘　　要：目的建立QuEChERS-气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)检测红糖中172种农药残留的方法。方法样品加入超纯水充分溶解后经正己烷高速匀浆提取,氮吹浓缩,QuEChERS法净化,采用GC-MS/MS检测技术,以分段时间选择反应监测模式(selective reaction monitoring,SRM)模式进行数据采集,配制基质匹配曲线及溶剂曲线进行定量检测。结果172种农药在10~200 ng/mL质量浓度的线性范围内线性关系良好,线性相关系数在0.9962~0.9999之间,定量限为0.01 mg/kg,在1、2、10倍定量限的浓度下各进行6次重复的加标实验,平均加标回收率在71.0%~113.0%之间,相对标准偏差为0.49%~17.00%(n=6)。结论该方法利用QuEChERS法净化,一次进样可以检测上百种农药,具有快速、简便、高通量、经济等特点,适用于红糖中多种农药残留的检测。Objective To establish the detection of 172 kinds of pesticide residues in brown sugar by QuEChERS-gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods The samples were fully dissolved in ultrapure water and extracted by high-speed homogenization of n-hexane,nitrogen blowing and concentration,and purified by QuEChERS method,and the data was collected in selective reaction monitoring mode by GC-MS/MS detection technology,and quantitatively detected by matrix curve and solvent curve.Results The 172 kinds of pesticides had a good linear relationship in the linear range of 10-200 ng/mL,and the linear correlation coefficient was between 0.9962 and 0.9999,the limit of quantification of the method was 0.01 mg/kg,performed 6 repeated spiked experiments at concentrations 1,2,and 10 times the limit of quantification each,the recovery rate of spikes was between 71.0%-113.0%,and the relative standard deviation(n=6)was 0.49%-17.00%.Conclusions This method can detect hundreds of pesticides in one injection,which is fast,simple,high-throughput and economical,and is suitable for the detection of a variety of pesticide residues in brown sugar.

关 键 词：QUECHERS 农药残留 气相色谱-串联质谱法 红糖 

分 类 号：TS247[轻工技术与工程—制糖工程] O657.63[轻工技术与工程—食品科学与工程]