投稿时间:2018-10-15      点此下载全文 HTML
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白国涛 中华人民共和国呼和浩特海关, 呼和浩特 010020 baigt@163.com 
刘来俊 中华人民共和国呼和浩特海关, 呼和浩特 010020  
盛万里 中华人民共和国呼和浩特海关, 呼和浩特 010020  
陈丽梅 中华人民共和国呼和浩特海关, 呼和浩特 010020  
张慧 中华人民共和国呼和浩特海关, 呼和浩特 010020  
中文摘要:建立了黄瓜中氟啶虫酰胺、丁苯吗啉、氟吡菌酰胺、氟啶虫胺腈、环酰菌胺、氟吡菌胺、唑嘧菌胺、氟吗啉、烯肟菌酯和烯肟菌胺10种农药残留的QuEChERS-气相色谱-串联质谱检测方法。样品采用QuEChERS方法,经乙腈涡旋振荡提取,无水硫酸镁和氯化钠盐析后,取5 mL提取液,加入含125 mg PSA、900 mg无水MgSO4和25 mg GCB的组合净化剂进行净化,采用Agilent HP-5 MS Ultra Inert色谱柱分离,气相色谱-串联质谱仪多反应监测(MRM)模式测定,基质匹配标准曲线外标法定量。结果表明:在检测浓度范围内,10种农药的质量浓度与其对应的峰面积间呈良好线性关系,决定系数均大于0.99;10种农药的平均回收率在76%~105%之间,相对标准偏差在4.0%~12%之间,定量限在0.001~0.05 mg/kg之间。该方法简便、快速、可靠,适用于黄瓜中10种农药残留的快速检测和分析确证。
中文关键词:气相色谱-串联质谱  黄瓜  农药残留  QuEChERS  烯肟菌胺  烯肟菌酯  氟吗啉
Determination of ten pesticide residues in cucumber using QuEChERS-gas chromatography-tandem mass spectrometry
Abstract:A multiresidue analytical method for the determination of 10 pesticide (flonicamid、fenpropimorph、fluopyram、sulfoxaflor、fenhexamid、fluopicolide、ametoctradin、flumorph、enestroburin and fenaminstrobin) residues in cucumber was developed using QuEChERS-gas chromatography-tandem mass spectrometry (GC-MS/MS).The target compound were extracted with acetonitrile by QuEChERS method. After salting out of anhydrous magnesium sulfate (MgSO4) and sodium chloride (NaCl), 5 mL extraction solvent was cleaned up and purified by a mixed sorbent of 125 mg PSA, 900 mg MgSO4 and 25 mg GCB. The samples was then separated on an Agilent HP-5 MS Ultra Inert column and wsa detected by GC-MS/MS system with the external standard method using matrix matched calibration curves. Results showed that linear relationships between peak area and mass concentration of 10 pesticides were achieved with a determination coefficient of 0.99. The recoveries ranged from 76% to 105% at four spiked levels in cucumber and the relative standard deviations (RSDs) ranged from 4.0% to 12%. The limits of quantification (LOQs) of the method were from 0.001 mg/kg to 0.05 mg/kg. This new method is suitable for the rapid and accurate determination of the 10 pesticide residues in cucumber.
Key words:gas chromatography-tandem mass spectrometry  cucumber  pesticide residues  QuEChERS  fenaminstrobin  enestroburin  flumorph
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