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标题：Determination of volatile alkylpyrazines in microbial samples using gas chromatography-mass spectrometry coupled with head space-solid phase microextraction
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作者：So Hyeon Jeon ; So Hyeon Jeon ; Jeoung Hwa Shin 等
期刊名称：Journal of Analytical Science and Technology
电子版ISSN：2093-3371
出版年度：2016
卷号：7
期号：1
页码：1-8
DOI：10.1186/s40543-016-0096-3
语种：English
出版社：Korea Basic Science Institute
摘要：Abstract Background Determination of volatile alkylpyrazines (VAPs) in microbial samples is needed for the understanding of microbial metabolism. An analytical method for screening and quantification of six volatile alkylpyrazines was developed and successfully applied to the real microbial samples. Methods Headspace-solid phase microextraction (HS-SPME) which is a simple extraction simultaneously carrying out clean-up and pre-concentration of VAPs in microbial samples was adopted. GC-TOF/MS with CombiPal SPME autosampler was used for fast screening of microbial samples and the optimization of HS-SPME condition. Separation and quantification of six VAPs that have the potential to be detected in microbial samples using quadrupole GC/MS in chemical ionization (CI) mode were carried out. Results The optimal extraction conditions for HS-SPME at 50 °C and 50 min were investigated. To eliminate matrix effects, DB-WAX column was more appropriate to separate each alkylpyrazines from the interferences than DB-5MS column. Chemical ionization provided enhanced confirmation from adduct ions ([M + 29]+ and [M + 41]+) of methane reagent gas as well as increasing signal intensity of molecular ions for quantitative analysis. Linear calibration curves of six alkylpyrazines were obtained within a range between 1 and 50 ng/g. Conclusions This proposed method was successfully applied to the microbial samples. 2-Methylpyrazine and 2,5-dimethylpyrazine were determined in the level of 6.0~34.0 ng/g.
关键词：Volatile alkylpyrazines (VAPs);Microbial samples;Gas chromatography/mass spectrometry (GC/MS);Head space-solid phase microextraction (HS-SPME);Chemical ionization (CI)