分散型固相萃取-气相色谱串联质谱法测定食品中8种芳氧苯氧丙酸酯类除草剂的残留量  

Determination of 8 Kinds of Aryloxyphenoxypropionate Herbicide Residues in Foods by Dispersive Solid Phase Extration and Gas Chromatography-Tandem Mass Spectrometry

作　　者：赵增运[1] 徐星 沈伟健[1] 余可垚[1] 柳菡[1] 桂茜雯[1] 龚玉霞[1] 沈崇钰[1] 吴斌[1] 蒋原[1] 

机构地区：[1]江苏出入境检验检疫局食品实验室,江苏南京210001 [2]云南商务信息工程学校,云南昆明650204

出　　处：《质谱学报》2010年第5期306-312,共7页Journal of Chinese Mass Spectrometry Society

基　　金：质检公益性行业科研专项(No.200810099、200810219)资助

摘　　要：建立了大豆、绿茶、大米、胡萝卜、菠菜、豌豆、大蒜、草莓、蜂蜜、猪肉、鱼肉、鸡蛋等12种食品中8种芳氧苯氧丙酸酯类除草剂残留量的分散型固相萃取-气相色谱串联质谱（DSPE-GC-MS/MS）分析方法。样品由含1%冰醋酸的正己烷的饱和乙腈溶液提取,分散型固相萃取法净化,采用气相色谱-串联质谱分时段反应离子监测技术进行测定,外标法定量。所有农药在10~1 000μg.L-1范围内线性良好;方法定量限（LOQ）均低于10μg.kg-1;在10、20、40μg.kg-1三个添加水平下,大豆等12种代表性基质中所有农药的平均回收率均处于70%~120%之间,RSD≤13%;该方法选择性较好,不仅能够用于多种食品基质的残留检测,而且还能较好地解决本底成分相当复杂的大蒜基质极易出现的干扰问题。A screening method was proposed for the determination of 8 kinds of aryloxyphenoxypropionate herbicide residues in 12 kinds of food by the technique of dispersive solid phase extration and gas chromatography-tandem mass spectrometry（DSPE-GC-MS/MS）,such as soybean,green tea,rice,radish,spinach,peas,garlic,strawberry,bee honey,pork,fish and egg,etc.Pesticides interested were extracted from samples with acetonitrile（saturated by n-hexane） containing 1% acetic acid,and liquid-liquid partition was formed after added anhydrous magnesium sulfate plus sodium acetate,and then a cleanup step followed,known as dispersive solid-phase extraction named QuEChERS method.The aliquot was determined by gas chromatography-tandem mass spectrometry（GC-MS/MS） using external standard method.The linearity of method are between 20 μg·L-1 and 1 000 μg·L-1,and the LOQs of pesticides are less than 4 μg·kg-1.The method is reliable and stable.The recoveries of all pesticides are in the range of 70%—120% at the three spiked levels of 10,20 and 40 μg·kg-1 into 12 kinds of food,and the RSDs are all below 13%.The method is selective well with no interference for multiple kinds of foods,especial in the complicated garlic matrix.

关 键 词：气相色谱-串联质谱(GC/MS) 反应离子监测(SRM) 分散型固相萃取(DSPE) 芳氧苯氧丙酸酯类除草剂 食品 

分 类 号：O657.63[理学—分析化学]