气相色谱-质谱法无基质效应测定冷冻韭菜中的腐霉利  

Determination of Procymidone Residues in Frozen Leek by Gas Chromatography-mass Spectrometry Method

作　　者：许文娟[1] 刘永强[1] 丁葵英[1] 郭礼强[1] 张轩恺 XU Wen-juan;LIU Yong-qiang;DING Kui-ying;GUO Li-qiang;ZHANG Xuan-kai(Weifang Entry-exit Inspection and Quarantine Bureau,Weifang 261041,Shandong,China;Weifang NO.1 Middle School,Weifang 261041,Shandong,China)

机构地区：[1]潍坊出入境检验检疫局,山东潍坊261041 [2]潍坊第一中学,山东潍坊261041

出　　处：《食品研究与开发》2018年第21期156-160,共5页Food Research and Development

基　　金：国家质检总局科研基金项目(2016IK208);山东出入境检验检疫局科研基金项目(SK201704)

摘　　要：建立冷冻韭菜中腐霉利残留的气相色谱-质谱检测方法。冷冻韭菜不经微波消解,直接用乙酸乙酯提取其中的腐霉利,硅胶柱净化,气相色谱-质谱分析,溶剂标准曲线外标法定量。结果表明,腐霉利在0.05μg/mL～0.7μg/mL范围内线性关系良好,相关系数为:0.999 9;在0.006、0.01、0.2 mg/kg 3个添加水平下的平均回收率为95.4%～98.5%,相对标准偏差为1.22%～3.08%,方法的检出限为0.002 mg/kg,定量限为0.006 mg/kg,与QuEChERS(quick,easy,cheap,effective,rugged,safe)等常用的前处理方法比,该方法溶剂更安全,操作简单,且无基质效应,定量时无需配制基质匹配标准曲线,具有实际应用价值。Procymidone in frozen leek sample was extracted by ethyl acetate,purified by silica gel column and then analyzed by gas chromatography-mass spectrometry(GC/MS)using external standard method.The results showed that,procymidone in frozen leek performed good linear from 0.05μg/mL to 0.7μg/mL,with relative coefficient of 0.999 9.The recoveries ranged from 95.4%to 98.5%with relative standard deviations of 1.22%-3.08%in adding level of 0.006,0.01 and 0.2 mg/kg.The limit of detection was 0.002 mg/kg and the limit of quantification was 0.006 mg/kg.Comparing with common methods such as the QuEChERS(quick,easy,cheap,effective,rugged,safe)method,it was safer,easier operation,more convenient quantification without matrix matching standard curve,exhibiting practical application value.

关 键 词：冷冻韭菜 腐霉利 气相色谱-质谱 基质效应 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]