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食品研究与开发:2019,40(16):95-99
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QuEChERS-气相色谱质谱联用法测定辣椒中的咪鲜胺及2,4,6-三氯苯酚残留量
(1.甘肃省商业科技研究所有限公司,甘肃 兰州 730010;2.甘肃中商食品质量检验检测有限公司,甘肃 兰州 730010)
Determination of Prochloraz and 2,4,6-Trichlorophenol in Pepper Using QuEChERS-Gas Chromatogarphy-Mass Spectrometry
(1.Gansu Institute of Business and Technology Co.,Ltd.,Lanzhou 730010,Gansu,China;2.Gansu Zhongshang Food Quality Test and Detection Co.,Ltd.,Lanzhou 730010,Gansu,China)
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投稿时间:2018-10-25    
中文摘要: 建立 QuEChERS(quick、easy、cheap、effective、rugged、safe)-气相色谱-质谱联用快速测定辣椒中咪鲜胺及其代谢物2,4,6-三氯苯酚残留量的方法。样品经乙腈-乙酸(99 ∶1,体积比)提取剂后,以无水硫酸镁和N-丙基乙二胺(primary secondary amine,PSA)净化,并利用气相色谱-串联质谱进行检测。研究不同提取溶剂和无水硫酸镁PSA量(3 ∶1,质量比)对提取净化效率的影响。结果表明:在最优试验条件下,咪鲜胺及其代谢物2,4,6-三氯苯酚在0.01 μg/mL~1.00 μg/mL 范围内线性关系均良好,相关系数分别为 0.999 1 和 0.999 2,检出限为 0.003 3 mg/kg;在 0.02、0.10、0.50 μg/mL 3 个添加水平下平均回收率为96.70%~100.64%,相对标准偏差(n=7)为2.33%~4.28%。该方法具有快速、便捷、安全、清洁和成本低的特点,可用于辣椒中咪鲜胺及其代谢物2,4,6-三氯苯酚残留的快速测定。
Abstract:To develop a rapid method for the determination of residues of prochloraz and its metabolite 2,4,6-trichlorophenol in pepper by QuEChERS(quick,easy,cheap,effective,rugged,safe)-gas chromatography-mass spectrometry(GC-MS).The samples were extracted by acetonitrile-acetic acid(99 ∶1,volume ratio),purified by anhydrous magnesium sulfate and primary secondary amine(PSA),and determined by GC-MS.Effects of different extraction solvents and anhydrous magnesium sulfate PSA (3 ∶1,mass ratio)on the determination of prochloraz and its metabolite 2,4,6-trichlorophenol were investigated.The results showed that prochloraz and its metabolite 2,4,6-trichlorophenol had a good linearity in the range of 0.01 μg/mL-1.00 μg/mL,the correlation coefficients were 0.999 1 and 0.999 2 under the optimal conditions.The limit of detection for prochloraz and its metabolite 2,4,6-trichlorophenol were 0.003 3 mg/kg.Their average recoveries at spiked levels of 0.02,0.10 and 0.50 μg/mL were 96.70%-100.64%with relative standard deviations(n=7)of 2.33%-4.28%.Therefore,the advantages of this method were simple,efficient,quick,convenient,safe,clean,lowcost and could be suitable for the analysis of prochloraz and 2,4,6-trichlorophenol residues in pepper.
文章编号:201916018     中图分类号:    文献标志码:
基金项目:甘肃省科技重大专项计划项目(17ZD2WA003);甘肃省国际科技合作计划项目(1604WKCA001);对发展中国家援助项目(KY201501005);甘肃省重点实验室专项项目(1606RTSA337);甘肃省科技创新平台专项项目(1605JTCA011);甘肃省重点实验室建设计划(1309RTSA025);青海省科技计划项目(2017-HZ809)
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