固相萃取/气相色谱-质谱分析大米中氟草烟残留  

Determination of Fluroxypyr Residue in Rice by Solid Phase Extraction and Gas Chromatography-Mass Spectrometry

作　　者：高文惠[1] 郭春海[2] 王凤池[2] 罗敏[1] 栗春艳[1] 

机构地区：[1]河北科技大学生物科学与工程学院,河北石家庄050018 [2]河北出入境检验检疫局,河北石家庄050071

出　　处：《分析测试学报》2007年第2期279-281,共3页Journal of Instrumental Analysis

基　　金：河北省博士基金资助项目(06547003D-3);河北省科技攻关课题(04213036);河北省教育厅课题(Z2005202)

摘　　要：试样采用NaOH-甲醇溶液提取,经EASY柱固相萃取净化后,以甲醇为衍生剂,浓硫酸为催化剂,在93～98℃水浴条件下酯化后,以DB-5 MS柱为分离柱,气相色谱-质谱联用测定.试验结果表明,氟草烟质量浓度为0.05～2 mg/L时,与相应的峰面积或丰度成良好的线性关系,相关系数为0.999 6;添加质量浓度为0.050 0～0.200 mg/kg时,回收率为81%～98%,该法检出限为0.01 mg/kg.A method has been developed for the determination of fluroxypyr residue in rice. The sample was extracted with sodium hydroxide - methanol solution and cleaned up by solid-phase extraction （SPE） with Chromabond EASY column. The esterification was carried out in 93 -98 ℃ water bath with methanol as derivating agent and 98% H2SO4 as catalyzer. The fluroxypyr was then analyzed by gas chromatography（GC） with DB-5 MS capillary column and detected by GC -MS. The linear range of the calibration curve for fluroxypyr was 0. 05 - 2 mg/L with a correlation coefficient of 0. 999 6. The detection limit was 0.01 mg/kg and the recoveries for 0. 050 0 -0. 200 mg/kg fluroxypyr were 81% - 98% , respectively.

关 键 词：氟草烟 残留 固相萃取 气相色谱-质谱 大米 

分 类 号：O657.63[理学—分析化学] S482.49[理学—化学]