凝胶渗透色谱-气相色谱-质谱联用快速测定大豆中克百威、乙草胺、甲草胺、异丙甲草胺、氟乐灵的残留量  

Determination of Residues of Carbofuran,Acetochlor,Alachlor,Metolachlor and Trifluralin in Soybean by GC / MS-GPC

作　　者：苏明明 张旭东 那晗 王琦[4] 宋大贺 张宁[4] 

机构地区：[1]大连出入境检验检疫局,辽宁大连116001 [2]锦州出入境检验检疫局,辽宁锦州121013 [3]大窑湾出入境检验检疫局,辽宁大连116001 [4]辽宁出入境检验检疫局,辽宁大连116100 [5]大连机场检验检疫局,辽宁大连116100

出　　处：《质谱学报》2012年第1期37-41,共5页Journal of Chinese Mass Spectrometry Society

摘　　要：建立了气相色谱-质谱(GC/MS)法,电子轰击离子化(EI)法同时测定及确证大豆中克百威、乙草胺、甲草胺、异丙甲草胺、氟乐灵的残留量。试样经乙腈提取,共提物中的色素和油脂用凝胶色谱(GPC)净化去除。采用GC/MS-SIM法对克百威、乙草胺、甲草胺、异丙甲草胺、氟乐灵进行定性和定量分析。结果表明,采用GPC净化,并设定收集时间在5～15min内,能够有效避免大豆中油脂峰干扰,缩短分析时间。5种农药的加标回收率为66.6%～104.9%,测定的相对标准偏差为2.2%～12.3%。5种农药在0.01～0.1mg/L范围内具有较好的线性,相关系数达0.996以上,方法中克百威、乙草胺、甲草胺、异丙甲草胺、氟乐灵的定量限均为0.01mg/kg。Carbofuran,acetochlor,alachlor,metolachlor and trifluralin in soybean were determined by gas chromatography-mass spectrometry（GC/MS） with electron impact（EI） ionization.The soybean samples were extracted with acetonitrile.The pigment and lipin were cleaned up with GPC.Carbofuran,acetochlor,alachlor,metolachlor and trifluralin were analyzed by GC/MS with selected-ion monitoring（SIM）.The results showed that GPC purification could avoid the influence of lipid collected time between 5 and 15 min.The recoveries of those pesticides are ranged from 66.2% to 104.9%,and standard deviations are from 2.2% to 12.3%.Under the optimized conditions,the calibration curves of 5 pesticides are linear in the range of 0.01—0.1 mg/L with correlation coefficients more than 0.996.The limits of quantitation of carbofuran,acetochlor,alachlor,metolachlor and trifluralin are 0.01 mg/kg.

关 键 词：气相色谱-质谱联用法 凝胶渗透色谱 大豆 克百威 氟乐灵 异丙甲草胺 甲草胺 乙草胺 残留分析 

分 类 号：O657.63[理学—分析化学]