凝胶渗透色谱净化－气相色谱－质谱法测定烟草中酰胺类除草剂  

GC-MS Determination of Acetanilide Herbicides in Tobacco After Purification with Gel Permeation Chromatography

作　　者：王岚[1] 和顺琴[1,2] 廖臻[1] 吴娜[1,2] 杨帅[1] 胡秋芬[2] 

机构地区：[1]云南省烟草化学重点实验室,云南烟草科学研究院,昆明650106 [2]云南民族大学化学与生物技术学院,昆明650031

出　　处：《理化检验（化学分册）》2011年第9期1077-1079,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：云南中烟工业公司基金项目(2008SB01)

摘　　要：提出了气相色谱-质谱法测定烟草中酰胺类除草剂异丙甲草胺、双苯酰草胺和敌草胺的残留量的方法。样品用乙酸乙酯-环己烷（1＋1）混合溶剂提取，所得提取液用凝胶渗透色谱进行净化，用乙酸乙酯-环己烷（1＋1）混合溶剂作流动相。采用气相色谱分离后，选择离子监测模式下质谱法进行测定。异丙甲草胺、双苯酰草胺和敌草胺的检出限（3S／N）分别为0．45，0．50，0．30ng·g-1。加入两个浓度水平的混合标准溶液进行了回收试验，所得回收率在90．0％～102．0％之间，相对标准偏差（n=6）在2．5％～3．2％之间。A method for determination ot resmual amount6 u, diphenamide and napropamide, in tobacco by CK2-MS was proposed. Samples were extracted with mixed solvent of ethyl acetate and n hexane （1＋1）. The extract obtained was purified by gel permeation chromatography using mixed solvent of ethyl acetate and n-hexane （1＋1） as mobile phase. The eluates were taken for separation by GC and the contents of 3 acetanilide herbicides were determined by MS under select ion monitoring （SIM） mode. Values of detection limit （3S/N） found were 0.45 ng · g-1 for metoiachlor, 0.50 ng · g-1 for diphenamide, and 0. 30 ng· g-1 for napropamide. Tests for recovery were made by addition of mixed standard solution at 2 different concentration levels, values of recovery found were in the range of 90. 0%- 102.0%, with values of RSD＇s （n=6） range of 2. 6 %- 3.2 %

关 键 词：气相色谱-质谱法 凝胶净化色谱 酰胺类除草剂 烟草 

分 类 号：O657.63[理学—分析化学]