食品研究与开发:2025,46(18):139-143
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静态顶空-气相色谱串接飞行时间质谱法测定芝麻油中四氯乙烯
马军,巩凡,李晓明,郝莉花 *,葛静静
(河南省产品质量检验技术研究院,河南 郑州 450001)
Determination of Tetrachloroethylene in Sesame Oil by Static Headspace-Gas Chromatography Tandem Time of Flight Mass Spectrometry
MA Jun,GONG Fan,LI Xiaoming,HAO Lihua *,GE Jingjing
(Henan Institute of Product Quality Inspection Technology,Zhengzhou 450000,Henan,China)
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投稿时间:2024-06-02    
中文摘要: 该文建立静态顶空气进样-气相色谱串接飞行时间质谱快速检测芝麻油中四氯乙烯的分析方法,并用该方法对市售197批次芝麻油进行四氯乙烯筛查。芝麻油经称量后于顶空瓶中加热平衡,进入气相色谱系统,以DB-624毛细管色谱柱(30 m×0.25 mm,1.4 μm)分离,飞行时间质谱测定,基质曲线外标法定量。结果表明,四氯乙烯在0.5~10 μg/kg线性范围内呈良好线性,线性相关系数R2为0.999 7;方法定量限为0.5 μg/kg,在标准曲线范围内进行加标回收试验,加标回收率为93.4%~112.2%,相对标准偏差(relative standard deviations,RSD)为1.2%~2.0%。对市售芝麻油197批次进行测定,未检出阳性样品。
Abstract:An analytical method for the rapid detection of tetrachloroethylene in sesame oil was developed based on static headspace-gas chromatography tandem time-of-flight mass spectrometry. This method was employed to examine tetrachloroethylene in 197 batches of commercially available sesame oil. Sesame oil was heated and equilibrated in a headspace vial,introduced into the gas chromatography system,separated by a DB-624 chromatographic column( 30 m×0.25 mm,1.4 μm),and quantified by time-of-flight mass spectrometry via a matrix curve external standard method. The results indicated that tetrachloroethylene exhibited good linearity within the range of 0.5 to 10 μg/kg,with R2 of 0.999 7. The limit of quantification was 0.5 μg/kg. Recovery experiments conducted within the standard curve range showed recovery rates ranging from 93.4% to 112.2%,with relative standard deviations (RSDs) between 1.2% and 2.0%. Among the 197 batches of commercially available sesame oil analyzed,no batch tested positive for tetrachloroethylene.
文章编号:202518018     中图分类号:    文献标志码:
基金项目:市场监督管理总局科技计划项目(2022MK081);河南省市场监督管理局科技计划项目(2022sj53)
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