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顶空固相微萃取-气相色谱-离子阱质谱法分析食品中的呋喃

Analysis of furan in foods by headspace solid-phase microextraction-gas chromatography-ion trap mass spectrometry.

作者信息

Altaki M S, Santos F J, Galceran M T

机构信息

Departament de Química Analítica, Universitat de Barcelona, Diagonal 647, 08028 Barcelona, Spain.

出版信息

J Chromatogr A. 2007 Mar 30;1146(1):103-9. doi: 10.1016/j.chroma.2007.01.104. Epub 2007 Feb 1.

Abstract

A headspace-solid-phase microextraction (HS-SPME) coupled to gas chromatography-ion trap mass spectrometry (GC-IT-MS) method is proposed for the analysis of furan in different heat-treated carbohydrate-rich food samples. The extraction efficiency of six commercially available fibres was evaluated and it was found that a 75mum carboxen/polydimethylsiloxane coating was the most suitable for the extraction of the furan. Parameters affecting the efficiency of HS-SPME procedure such as extraction temperature and time, ionic strength, headspace and aqueous volume ratio (V(h)/V(w)), desorption temperature and time, were optimized. Quality parameters were established using spiked water and food samples. Linearity ranged between 0.02 and 0.5ngg(-1) and run-to-run and day-to-day precisions for food samples were lower than 6% and 10%, respectively. The limit of detection (LOD) of the method is sample dependent and ranged from 8 to 70pgg(-1), while the limit of quantification is from 30 to 250pgg(-1). Isotope dilution using furan-d(4) is proposed for furan determination providing similar results to those obtained by standard addition with internal standard (US Food and Drug Administration method). The developed HS-SPME-GC-IT-MS method was applied to the analysis of furan in different Spanish food samples from a local market, and concentrations ranging from 0.17 to 2279ngg(-1) were found.

摘要

本文提出了一种顶空-固相微萃取(HS-SPME)结合气相色谱-离子阱质谱(GC-IT-MS)的方法,用于分析不同热处理富含碳水化合物食品样品中的呋喃。评估了六种市售纤维的萃取效率,发现75μm碳分子筛/聚二甲基硅氧烷涂层最适合用于呋喃的萃取。优化了影响HS-SPME程序效率的参数,如萃取温度和时间、离子强度、顶空与水相体积比(V(h)/V(w))、解吸温度和时间。使用加标水和食品样品建立了质量参数。线性范围在0.02至0.5ng g(-1)之间,食品样品的批内和批间精密度分别低于6%和10%。该方法的检测限(LOD)取决于样品,范围为8至70pg g(-1),定量限为30至250pg g(-1)。建议使用呋喃-d(4)进行同位素稀释测定呋喃,其结果与通过内标标准加入法(美国食品药品监督管理局方法)获得的结果相似。所开发的HS-SPME-GC-IT-MS方法应用于分析当地市场上不同西班牙食品样品中的呋喃,发现浓度范围为0.17至2279ng g(-1)。

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