五氟苄基溴衍生-气相色谱-电子俘获检测法和气相色谱质谱法测定蜂蜜中二氯喹啉酸  

Determination of quinclorac in honey by pentafluorobenzyl bromide derivatization-gas chromatography-electron capture detection and gas chromatography-mass spectrometry

作　　者：祁朝阳 黄学者 祖铁红 李阿丹[1] 崔宗岩 QI Zhaoyang;HUANG Xuezhe;ZU Tiehong;LI Adan;CUI Zongyan(College of Environmental and Chemical Engineering,Yanshan University,Qinhuangdao 066004,China;Technology Center of Qinhuangdao Customs,Qinhuangdao 066004,China)

机构地区：[1]燕山大学环境与化学工程学院,秦皇岛066004 [2]秦皇岛海关技术中心,秦皇岛066004

出　　处：《分析试验室》2024年第12期1735-1740,共6页Chinese Journal of Analysis Laboratory

基　　金：海关总署科研项目(2022HK023);河北省自然科学基金面上项目(B2021203005)资助。

摘　　要：建立了测定蜂蜜中二氯喹啉酸残留量的五氟苄基溴(PFBBr)衍生-气相色谱-电子俘获检测法(GC-ECD)和气相色谱质谱法(GC-MS)。在蜂蜜溶液调节pH 6.0±0.5后,样品经强阴离子交换型固相萃取柱(SAX)净化,5%甲酸-甲醇(V/V)洗脱,氮吹后丙酮复溶,PFBBr衍生,GC-ECD和GC-MS法测定。结果表明:GC-ECD和GC-MS法的定量限分别为0.05 mg/kg和0.01 mg/kg;2种方法分别在0.05~0.5 mg/kg和0.01~0.1 mg/kg添加水平下,平均回收率在82.3%~92.1%之间,相对标准偏差(RSD)在3.0%~6.5%之间。将本方法应用于74批蜂蜜样品的检测,4批样品中检出二氯喹啉酸,含量均不超过0.01 mg/kg。Two methods were developed for the determination of quinclorac in honey by pentafluorobenzyl bromide(PFBBr)derivatization-gas chromatography-electronncapture detection(GC-ECD)and ggas chromatography-mass spectrometry(GC-MS).At pH 6.0,the sample solution was purified on a SAX solid phase extraction cartridge,followed by elution using 5%formic acid-methanol(V/V).The eluent was dried under nitrogen flow and redissolved with acetone,then it was derivatized with PFBBr,and finally detected using GCECD or GC-MS.The limits of quantification for GC-ECD and GC-MS were 0.05 mg/kg and 0.01 mg/kg,respectively.At the spiked level ranges of 0.05-0.5 mg/kg and 0.01-0.1 mg/kg,the recoveries of the two detection methods were 82.3%-92.1%,and the relative standard deviations were 3.0%-6.5%.The proposed methods were applied for the detection of 74 honey samples.The quinclorac were detected in 4 samples and the contents were less than 0.01 mg/kg.

关 键 词：二氯喹啉酸 蜂蜜 衍生化 气相色谱-质谱法 气相色谱-电子俘获检测法 

分 类 号：S896.1[农业科学—特种经济动物饲养] X592[农业科学—畜牧兽医]