盐酸衍生-气相色谱法快速测定水果中苯丁锡残留  

Rapid determination of fenbutatin oxide residue in fruits by hydrochloric acid derivatization combined with gas chromatography

作　　者：崔宗岩 王晶 徐立英 李学民 曹彦忠 张进杰 王宪[2] CUI Zong-yan;WANG Jing;XU Li-ying;LI Xue-min;CAO Yan-zhong;ZHANG Jin-jie;WANG Xian(Qinhuangdao Entry-Exit Inspection and Quarantine Bureau,Qinhuangdao 066004;Qinhuangdao Health School,Qinhuangdao 066000)

机构地区：[1]秦皇岛出入境检验检疫局检验检疫技术中心,秦皇岛066004 [2]秦皇岛市卫生学校,秦皇岛066000

出　　处：《分析试验室》2018年第10期1189-1192,共4页Chinese Journal of Analysis Laboratory

基　　金：河北省科技计划项目(17275503D);国家质检总局科技计划项目(2016IK106)资助

摘　　要：建立了水果中苯丁锡残留量测定的气相色谱法,并建立了气相色谱-质谱(EI源)确证方法。样品经二氯甲烷提取,浓盐酸衍生,酸性氧化铝柱固相萃取净化,正己烷-乙酸乙酯(9+1,V/V)洗脱,浓缩后通过气相色谱-电子俘获检测器进行测定。结果表明:方法的定量限为0.050 mg/kg,在0.05~5.0 mg/kg添加水平范围内,5种水果中苯丁锡的平均回收率在72.4%~98.4%之间,相对标准偏差不超过12%。A method was developed for the determination of fenbutatin oxide （FBT） in fruits by gas chromatography, which was further verified by a gas chromatography-mass spectrometry （GC-MS） method. The FBT in fruit sample was firstly extracted with dichloromethane, and then derived to trineophyhin chloride （FBTC1） with hydrochloric acid. After cleaning up on an acid alumina cartridge, the sample extract was concentrated to a definite volume, and finally determined by GC- ECD. The limit of quantitation was 0. 050 mg/kg. At the spike range of 0. 5 - 5.0 mg/kg, the recoveries for FBT were in the range of 72. 4% - 98.4% , and the relative standard deviations （RSDs） did not exceed 12%.

关 键 词：苯丁锡 气相色谱-电子俘获检测法 气相色谱-质谱法 确证 水果 

分 类 号：TQ450[化学工程—农药化工] O657.7[理学—分析化学]