QuEChERs结合气相色谱-串联质谱法测定不同果蔬基质中33种有机磷类农药残留量  

Determination of 33 organophosphorus pesticide residues in different fruitand vegetable substrates by QuEChERs combined with gas chromatography-tandem mass spectrometry

作　　者：夏仕青 吴桃丽 薛云 李晓慧 XIA Shi-qing;WU Tao-li;XUE Yun;LI Xiao-hui(Department of Surveillance,Center for Disease Control and Prevention,Qianxinan Prefecture,Guizhou Province,Xingyi,Guizhou 562400,China)

机构地区：[1]贵州省黔西南州疾病预防控制中心监测检验科,贵州兴义562400

出　　处：《现代预防医学》2024年第3期523-528,共6页Modern Preventive Medicine

摘　　要：目的 采用QuECh ERs前处理结合气相色谱-串联质谱技术,建立四种不同果蔬基质(普通型、高色素型、高脂肪型及高糖型)中33种有机磷类农药残留量快速检测方法,为不同水果、蔬菜中多种有机磷农药同时检测和食品安全风险评估提供技术支持。方法 样品经乙腈及柠檬酸钠-柠檬酸氢二钠缓冲液同时提取,乙二胺-N-丙基硅烷(PSA)、十八烷基硅烷键合硅胶(C18)及石墨化炭黑(GCB)三种吸附剂净化,氮吹浓缩后用丙酮复溶,采用气相色谱-串联质谱仪在多反应离子监测(MRM)模式下进行检测,内标法定量。结果 四种不同果蔬基质中33种有机磷类农药在50~500μg/L的浓度范围内相关系数均大于0.995 0,方法检出限为1.50~5.04μg/kg,定量限为5.01~16.78μg/kg;在添加0.040~0.200 mg/kg水平范围内,农药的平均回收率为71.4%~119.1%,相对标准偏差均低于12%。结论 该方法简单快速、准确度高、精密度好,适用于不同果蔬基质中33种有机磷类农药残留的快速检测和定量分析。Objective To establish a rapid method for the determination of 33 organophosphorus pesticide residues in four different fruit and vegetable substrates(common type,high pigment type,high fat type,and high sugar type)by QuEChERs pretreatment combined with gas chromatography-tandem mass spectrometry(GC-MS),so as to provide technical support for simultaneous detection and food safety risk assessment of organophosphorus pesticides in different fruits and vegetables.Methods The samples were extracted with acetonitrile and sodium citrate-disodium hydrogen citrate buffer at the same time,purified with ethylenediamine-N-propyl silane(PSA),octadecylsilane bonded silica gel(C18),and graphitized carbon black(GCB).After nitrogen blowing concentration,the samples were re-dissolved with acetone and detected by gas chromatography-tandem mass spectrometry under multi-reaction ion monitoring(MRM)mode.Quantifications were based on internal standard curves.Results The method had good linear relationship in the range of 50μg/L to 500μg/L,with the correlation coefficients greater than 0.9950.The detection limits were within 1.50 to 5.04μg/kg,and the limits of quantification were within 5.01 to 16.78μg/kg.In the range of 0.040 to 0.200 mg/kg,the average recoveries ranged from 71.4%to 119.1%,with the relative standard deviations less than 12%.Conclusion The method is simple and rapid,with high accuracy and precision,which is suitable for the rapid detection and quantitative analysis of 33 organophosphorus pesticide residues in different fruit and vegetable substrates.

关 键 词：有机磷类农药 果蔬 QUECHERS 气相色谱-串联质谱法 

分 类 号：O657.71[理学—分析化学] TS255.7[理学—化学]