气相色谱法同时测定大豆中13种苯氧羧酸类除草剂的残留量  

Simultaneous Determination of Multiple Phenoxy Acid Herbicide Residues in Soybean by Gas Chromatography

作　　者：匡华[1] 储晓刚[2] 侯玉霞[1] 祁彦[2] 

机构地区：[1]中国农业大学理学院,北京100094 [2]中国检验检疫科学研究院,北京100025

出　　处：《中国食品卫生杂志》2006年第6期503-508,共6页Chinese Journal of Food Hygiene

基　　金：国家"十五"食品安全重大专项(2001BA804A17)

摘　　要：为检测大豆中的苯氧羧酸类除草剂残留,建立了大豆中13种苯氧羧酸类除草剂(对氯苯氧乙酸、对氯苯氧丙酸、苯氧丁酸、麦草畏、2甲4氯苯氧乙酸、2甲4氯苯氧丙酸、2甲4氯苯氧丁酸、2,4-滴、3,4-滴、2,4,5-涕、2,4,5-涕丙酸、2,4-滴丙酸、2,4-滴丁酸)多残留量的气相色谱检测方法。样品经过正己烷预除脂后用乙腈和50mmol/L盐酸混和液(体积比7+3)提取,提取液经过与乙腈饱和的正己烷液液分配除脂,阴离子交换柱净化后用五氟溴苄衍生化。衍生产物经硅胶柱净化后,采用气相色谱(GC)-电子捕获检测器(ECD)检测,外标法定量。13种苯氧羧酸类除草剂在质量浓度0.005～0.1mg/kg之间,与峰面积呈线性关系,相关系数为0.9954～0.9993;0.01和0.1mg/kg2个水平的加标回收率均在70%以上,相对标准偏差小于20%,方法的检测限(S/N≥3)满足主要贸易国最大残留限量要求。A technique for simultaneous determination of 13 phenoxy acid herbicide residues in soybean was developed. Phenoxy acid herbicides were extracted with acetonitrile-50 mmol/L HCl （volume ratio was 7 ＋ 3）, followed by liquld-liquid partition with n-hexane. The soybean extract was further cleaned up by anion exchange column and derivatized with pentafluorobenzyl bromide. The resulting esters were determined by gas chromatography equipped with electron capture detector. The pre-treatment method was critically examined. Recoveries of two fortified levels （0.01 and 0.1 mg/kg） were above 70%. and the coefficients of variation were less than 20%. It showed that this method can meet the requirements of multi-residue analysis in the inspection of import/export soybean commodities.

关 键 词：色谱法 气相 豆科 农药残留量 除莠剂 

分 类 号：R155.5[医药卫生—营养与食品卫生学]