固相微萃取-气相色谱-质谱法检测30种农药残留  

Determination of different kinds of pesticides by SPME-GC/MS

作　　者：朱涛[1] 朱莉萍[1] 周宏琛[1] 倪永付[1] 闫秋成 王勇[1] 

机构地区：[1]济宁出入境检验检疫局,济宁272000

出　　处：《分析试验室》2013年第3期115-120,共6页Chinese Journal of Analysis Laboratory

摘　　要：建立使用一种萃取头同时检测蔬菜中30种农药的GC-MS分析方法。采用了SPME-GC/MS自动进样技术,比较聚二甲基硅氧烷(PDMS)、聚丙烯酸酯(PA)、聚二甲基硅氧烷-二乙烯基苯(PDMS/DVB)、聚乙二醇-二乙烯基苯(CW/DVB)4种固定相涂层的分析效果,选择了目标物萃取效率较高、干扰物萃取较少的PDMS。通过正交实验设计,选择不同的萃取温度、萃取时间、振荡速度进行试验,最终确定振荡速度250 r/min,萃取温度70℃,萃取时间60 min作为萃取条件。对不同的无机盐浓度对标准品溶液和加入基质标准品溶液的提取效率的影响分别进行了试验,确定用10%(w/V)NaCl溶液增加提取液离子强度。试验过程中优化分析的色谱条件和质谱条件,进样到分析结束时间可控制在40 min。该方法检测蔬菜样品中混合标准溶液的回收率为43%～119%,相对标准偏差在3.4%～19%之间。Solid-phase micro-extraction （SPME） fibers were successfully used to analyse 30 kinds of pesticides by SPME-GC/MS with auto-control model in the study. The extraction effects of fibers with different coatings （PDMS, PA ,PDMS/DVB, CW/DVB） were compared. PDMS was selected for its higher extracting effects than the others. Orthogonal test was designed in the study, several parameters were settled： extraction temperature （60 and 70℃ ）, extraction time（30 and 60 min）, extraction speed （250 and 500 r/min）. And the concentration of inorganic salts were considered （water, 10% NaCl, NaCl-saturated solution）. It indicated 10% NaCl had better effects in the experiments. The whole process could be finished in 40 minutes. The method has the advantages of sensitivity and simplicity. The LOD were 0. 001 - 0. 95 μg/kg（ S/N = 3 ）, the recoveries （n = 6 ） were 43% 119%, and the RSDs were 3.4% -18.7%.

关 键 词：SPME—GC MS 萃取头 振荡速度 萃取温度 萃取时间 无机盐浓度 

分 类 号：O657.63[理学—分析化学]