摘要
本研究建立了玉米中有机氯农药、多氯联苯和多溴联苯醚等多种持久有机污染物的样品前处理方法和气相色谱-三重四极杆质谱分析方法。玉米样品水化后,用乙酸乙酯直接2次提取和44%酸性硅胶柱净化,采用气相色谱-三重四极杆质谱在动态多反应离子检测模式进行分析,内标法定量。有机氯农药、多氯联苯和多溴联苯醚的响应与质量浓度呈较好的线性关系,决定系数大于0.996,高取代溴联苯醚的响应与质量浓度为二次曲线关系;方法回收率在55.7%~122.8%之间,相对标准偏差(RSD)1.0%~16.1%;方法检出限在0.003~1.174 ng/g之间。建立的分析方法前处理操作简便,提取效率高,净化效果好,分析方法灵敏度高,准确性和精密度好,适用于玉米样品中持久性有机污染物的分析检测。
The present study established a method based on gas-chromatography-tandem mass spectrometry for analysis of polychlorinated biphenyls,organochlorine pesticides and polybrominated biphenyl ether in maize.By this method,the hydrated maize powder sample was extracted with ethyl acetate twice.The extraction was purified on 5 g acidic silica(44%)and was subsequently analyzed by gas chromatography-tandem mass spectrometry with mass spectrometer operated on a dynamic multiple reaction monitor(dMRM)acquisition mode.The quantitation was carried out with internal standard method.The results indicated that all target analytes had a good quantitative linear range with excellent regression factor(R 2>0.996),while highly brominated biphenyl ethers were with quadratic calibration curve.The method detection limits for all targets were between 0.003~1.174 ng/g whereas the highly brominated biphenyl ether gave relatively poor detection limits.The recovery of method was 55.7%~122.8%with relative standard deviations of 1.0%~16.1%.The pretreatment process of this method was simple to operate with good purification effect and good recovery.This method was sensitive,accurate and suitable for the analysis of trace persistent organic pollutants in maize.
作者
张炜
杨永坛
王松雪
李森
蔡娣
李丽
Zhang Wei;Yang Yongtan;Wang Songxue;Li Sen;Cai Di;Li Li(Academy of National Food and Strategic Reserves Administration,Beijing 100037)
出处
《中国粮油学报》
CAS
CSCD
北大核心
2022年第9期280-287,共8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(ZX1942)。
关键词
气相色谱-三重四极杆质谱法
酸化硅胶
玉米
多氯联苯
有机氯农药
多溴联苯醚
gas chromatography-tandem mass spectrometry
acidic silica
maize
polychlorinated biphenyl
organochlorine pesticides
polybrominated biphenyl ether
