气相色谱测定小麦和稻米中11种多溴联苯醚  

Determination of 11 Kinds of Polybrominated Diphenyl Ether in Wheat and Rice by Gas Chromatography

作　　者：张炜 杨永坛 蔡娣 张洁琼 李森 李丽 Zhang Wei;Yang Yongtan;Cai Di;Zhang Jieqiong;Li Sen;Li Li(Academy of National Food and Strategic Reserves Administration,Beijing 100037)

机构地区：[1]国家粮食和物资储备局科学研究院,北京100037

出　　处：《中国粮油学报》2023年第9期190-196,共7页Journal of the Chinese Cereals and Oils Association

基　　金：中央级公益性基本科研业务费专项资金项目(ZX2012)。

摘　　要：建立气相色谱-电子捕获检测器法测定小麦和稻米中11种代表性多溴联苯醚的分析方法。全麦粉或糙米粉经水化后,采用乙酸乙酯提取和5 g酸性硅胶(44%,m:m)固相净化柱净化,使用气相色谱-电子捕获检测器进行检测,外标法定量。小麦和稻米中,11种多溴联苯醚的定量线性范围分别为0.1~50 ng/g、0.2~50、0.5~50 ng/g,线性相关系数R^(2)均大于0.998;方法检出限在0.03~0.15 ng/g之间,定量限为0.1~0.5 ng/g之间;方法回收率为67.6%~99.7%,相对标准偏差为0.4%~17.8%。本方法的样品前处理简单,对仪器要求低,准确度和精密度较好,适用于小麦和稻米中多溴联苯醚的检测分析。To establish and validate an analytical method for detection 11 kinds of polybrominated biphenyl ethers in wheat and rice based on gas chromatography-electron capture detector,hydrated powders of wheat or rice were extracted with ethyl acetate and purified solid phase column packed with 5 g acid silica gel(44%,m:m).The samples were subsequently analyzed with gas chromatography-electron capture detector,and quantified by external standard method.Eleven kinds of targeted polybrominated diphenyl ethers had good linear ranges in the range of 0.1~50,0.2~50 ng/g and 0.5~50 ng/g with the regression coefficients greater than 0.998.The limits of detection were 0.3 to 0.15 ng/g for all PBDEs.The recoveries were 67.6%~99.7% and the relative standard deviations were 0.4%~17.8%.This method had the advantages of simple sample pretreatment,good recovery,satisfying analytical accuracy and precision,suitable for the screening of polybrominated biphenyl ether in wheat and rice matrix.

关 键 词：多溴联苯醚 气相色谱-电子捕获检测器法 小麦 稻米 

分 类 号：O657.7[理学—分析化学]