分析与检测

静态顶空-气相色谱串接飞行时间质谱法测定绿茶中5种禁用香精

  • 马军 ,
  • 郝莉花
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  • (河南省产品质量监督检验院,河南 郑州,450000)
硕士,高级工程师(郝莉花高级工程师为通信作者,E-mail:522007712@qq.com)

收稿日期: 2022-06-07

  修回日期: 2022-07-06

  网络出版日期: 2022-12-02

基金资助

国家市场监督管理总局2020年技术保障专项项目(2020YJ019)

Determination of five prohibited flavorants in green tea by static headspace-gas chromatography tandem time of flight mass spectrometry

  • MA Jun ,
  • HAO Lihua
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  • (Henan Institute of Quality Supervision and Inspection, Zhengzhou 450000, China)

Received date: 2022-06-07

  Revised date: 2022-07-06

  Online published: 2022-12-02

摘要

建立了静态顶空气进样-气相色谱串接飞行时间质谱同时快速检测绿茶中5种禁用香精成分(樟脑、胡薄荷酮、胡椒酚甲醚、桉油精和反式茴香脑)的方法,对市售23批次绿茶进行5种禁用香精筛查。绿茶经粉碎过筛后称量于顶空瓶中,在顶空进样器中加热平衡,进入气相色谱系统,以DB-624UI(30 m×0.25 mm,1.4 μm)色谱柱分离,飞行时间质谱测定,基质曲线外标法定量。结果表明,5种禁用香精成分在0.5~10 μg/kg范围内线性关系良好,线性相关系数(r2)为0.998~0.999;5种禁用香精的检出限分别为:樟脑0.3 μg/kg、胡薄荷酮0.3 μg/kg、胡椒酚甲醚0.1 μg/kg、桉油精0.2 μg/kg、反式茴香脑0.2 μg/kg,相对标准偏差为0.88%~3.36%。23批次绿茶及茉莉花茶中,桉油精检出7批次,胡椒酚甲醚和樟脑各检出1批次。该方法处理简单、快速,检测灵敏度高,可用于绿茶中5种禁用香精成分的检测。

本文引用格式

马军 , 郝莉花 . 静态顶空-气相色谱串接飞行时间质谱法测定绿茶中5种禁用香精[J]. 食品与发酵工业, 2022 , 48(21) : 286 -291 . DOI: 10.13995/j.cnki.11-1802/ts.032523

Abstract

An analytical method for simultaneous rapid detection of five banned flavorants (camphor, pulegone, piperonyl methyl ether, eucalyptol and trans-anethole) in green tea was established by static headspace-gas chromatography tandem time-of-flight mass spectrometry. This method was used to examine five banned flavors of 23 species of commercial green tea. The green tea was crushed, screened, and weighed in a headspace flask, and then it was heated and balanced in a headspace sampler. The green tea was separated by a DB-624UI (30 m×0.25 mm, 1.4 μm) chromatographic column, determined by time-of-flight mass spectrometry mode and quantified by a matrix-matched external standard method. The results showed that the data had a good linear correlation between 0.5 and 10 μg/kg with the correlation coefficients r2 0.998-0.999. The detection limits of the five banned flavorants were 0.3 μg/kg for camphor, 0.3 μg/kg for pulegone, 0.1 μg/kg for piperonyl methyl ether, 0.2 μg/kg for eucalyptol, and 0.2 μg/kg for trans-anethole, respectively. The relative standard deviation of the method was 0.88%-3.36%. Among the 23 species of green tea and jasmine tea, 7 species of eucalyptol were detected, and 1 species of piperonyl methyl ether and camphor could be detected. The method is simple, rapid, and sensitive, that can be used for the simultaneous detection of five banned flavor components in green tea.

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