顶空固相微萃取-气质联用法测定奶茶中的香兰素和乙基香兰素

徐幸; 彭飞进; 舒平; 狄家卫; 赵浩军; 王坤

doi:10.13386/j.issn1002-0306.2016.16.007

顶空固相微萃取-气质联用法测定奶茶中的香兰素和乙基香兰素

大理州质量技术监督综合检测中心
云南华测检测认证有限公司

基金项目:

云南省卫生厅制修订食品安全地方标准项目(云卫[2014]DB003)；

详细信息

作者简介:
徐幸(1983-),女,博士,工程师,研究方向:食品质量安全检测,E-mail:xuxing1983@163.com。;

中图分类号: TS207.3
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出版历程
- 收稿日期: 2016-02-18

Determination of vanillin and ethyl vanillin in milky tea by HS-SPME-GC/MS

Dali Comprehensive Inspection Centre of Quality and Technical Supervision
Centre Testing International Co.,Ltd.

摘要

摘要: 采用顶空固相微萃取（HS-SPME）和气相色谱质谱联用技术（GC/MS）,建立了测定奶茶中香兰素和乙基香兰素的分析方法。选取了75μm carboxen/聚二甲基硅氧烷（CAR/PDMS）萃取纤维,考察了萃取温度、萃取时间和盐浓度等因素对萃取效率的影响。采用3,4-亚甲二氧苯乙酮作为内标,对香兰素和乙基香兰素进行定量。结果表明,在检测范围0.5²5.0μg内,该方法对香兰素（R2=0.9974）和乙基香兰素（R2=0.9987）具有良好的线性关系,固体样品中香兰素和乙基香兰素的检出限分别为0.5 mg/kg和0.3 mg/kg,液体样品中检出限分别为0.05 mg/kg和0.03 mg/kg,香兰素的平均回收率为88.99%¹05.15%,相对标准偏差（RSDs）为2.40%⁹.26%,乙基香兰素的平均回收率为91.57%¹05.13%,相对标准偏差为2.35%⁸.49%。该方法操作简便、准确可靠,适合于奶茶中香兰素和乙基香兰素的分析要求。
- 香兰素 /
- 乙基香兰素 /
- 顶空固相微萃取-气质联用法（HS-SPME-GC/MS） /
- 奶茶
Abstract: A method for headspace solid phase micro extraction( HS- SPME) and gas chromatography mass spectrometry( GC / MS) was developed for the determination of vanillin and ethyl vanillin in milky tea. 75 μm carboxen / polydimethylsiloxane( CAR / PDMS) fiber was selected for extraction in this study. The parameters affecting extraction efficiency such as extraction temperature,extraction time and salt concentration were investigated.3',4'-( methylenedioxy) acetophenone was used as an internal standard for quantifying vanillin and ethyl vanillin.The results showed that the linear relationships between ratio of peak area and concentration of vanillin( R2= 0.9974) and ethyl vanillin( R2= 0.9987) were good enough from 0.5 to 25.0 μg.The limits of detection for vanillin and ethyl vanillin were 0.5 mg / kg and 0.3 mg / kg in solid samples,and they were 0.05 mg / kg and 0.03 mg / kg in liquid samples,respectively. The average recoveries of vanillin were 88.99% ~ 105.15%,and the relative standard deviations( RSDs) were 2.40% ~ 9.26%. The average recoveries of ethyl vanillin were 91.57% ~ 105.13%,and the RSDs were 2.35% ~8.49%.This method is convenient and reliable,and it is suitable for the determination of vanillin and ethyl vanillin in milky tea.
- vanillin /
- ethyl vanillin /
- headspace solid phase micro extraction and gas chromatography mass spectrometry(HS-SPME-GC/MS) /
- milky tea

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