| 两种离子化技术气相色谱-串联质谱法测定青菜与草莓中3种有机锡类农药残留 |
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| 基金项目:PORTSIM 11TH RESEARCH ADVISORY COMMITTEE(RAC)MEETING(Analysis for Red Palm Oil Product Registration in China)(PORTSIM 061/2017) |
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| 中文摘要:采用电子轰击(EI)和正化学(PCI)两种电离源技术，建立了气相色谱-串联质谱(GC-MS/MS)同时测定青菜和草莓中三环锡、三苯锡、苯丁锡农药残留的分析方法。样品经氢溴酸消解，丙酮-正己烷提取，经衍生后由Florisil固相萃取柱净化，分别采用EI和PCI两种电离源进行选择反应监测模式测定，采用基质匹配外标法定量。结果显示，在005~10 mg/L质量浓度范围内，3种有机锡农药呈良好线性，相关系数均大于0998。两种方法中目标物的定量下限分别为0019~0042 mg/kg和0009~0042 mg/kg，均能满足国内外的限量要求。在005、010、020 mg/kg加标水平下，目标物的平均回收率为701%~939%，相对标准偏差(RSD)均小于10%。两种方法线性均较好，灵敏度较高，可用于水果蔬菜中有机锡农药的测定，且两种方法可实现互补，有助于提高定性和定量的可靠性。 |
| 中文关键词:气相色谱-串联质谱 电子轰击电离源 正化学电离源 有机锡 青菜 草莓 |
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| Determination of Three Organo tin Pesticide Residues in Green Vegetables and Strawberry by GC-MS/MS with Two Ionization Techniques |
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| Abstract:A method was developed for the simultaneous determination of fenbutatin oxide,triphenyltin and cyhexatin pesticide residues in green vegetables and strawberry by gas chromatography-tandem mass spectrometry(GC-MS/MS) with two ionization techniques,ie.electron impact ionization(EI) and positive chemical ionization(PCI).The samples were firstly digested with hydrobromic acid,then extracted with acetone-hexane,finally derived with sodium tetraethylborate.After purification with Florisil solid phase extraction column,the samples were analyzed by GC-MS/MS with EI and PCI sources under SRM mode.Three kinds of organo tin pesticide residues showed good linear relationships in the range of 005-10 mg/L with correlation coefficients larger than 0998.The limits of quantitation for the target objects were in the range of 0019-0042 mg/kg and 0009-0042 mg/kg,respectively,which could meet the requirements for the maximun residue limits(MRLs) of organotin pesticide residues at home and abroad.The average recoveries for three organotin residues at three spike levels of 005,010,020 mg/kg were in the range of 701%-939% with the relative standard deviations less than 10%.With good linearity and high sensitivity,the proposed methods could be used for the determination of organotin pesticide residues in green vegetables and strawberry.Forthermore,the two methods could complement each other to improve the reliabilities of qualitation and quantitation. |
| Key Words:gas chromatography-tandem mass spectromety(GC-MS/MS) electron impact ionization (EI) positive chemical ionization (PCI) organo tin green vegetables strawberry |
| 引用本文：王红，沈伟健,蔡理胜，吴斌，丁涛，姜珊，余可垚，王晓研.两种离子化技术气相色谱-串联质谱法测定青菜与草莓中3种有机锡类农药残留[J].分析测试学报,2018,37(5):594-598. |
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