Headspace Solid-Phase Microextraction Gas Chromatography–Mass Spectrometry Analysis of Volatiles in Orujo Spirits from a Defined Geographical Origin
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- 作者：Rosa M. Peñ ; a ; Julia Barciela ; Carlos Herrero ; Sagrario Garcí ; a-Martí ; n
- 刊名：Journal of Agricultural and Food Chemistry
- 出版年：2008
- 出版时间：April 23, 2008
- 年：2008
- 卷：56
- 期：8
- 页码：2788 - 2794
- 全文大小：259K
- 年卷期：v.56,no.8(April 23, 2008)
- ISSN：1520-5118
文摘
A headspace solid-phase microextraction (HS-SPME) and gas chromatography−selective ion monitoring/mass spectrometry (GC−SIM/MS) method was optimized for analysis of 22 volatile compounds in orujo spirit samples from the Geographic Denomination “Orujo de Galicia/Augardente de Galicia”. HS-SPME experimental conditions, such as fiber coating, extraction temperature, extraction and pre-equilibrium time, sample volume, and the presence of salt, were studied to improve the extraction process. The best results were obtained using a 65 µm Carbowax-divinylbenzene fiber during a headspace extraction at 40 °C with constant magnetic stirring for 15 min and after a 5 min period of pre-equilibrium time. The sample volume was 6 mL of orujo containing 25% of NaCl, placed in 12 mL glass vials equipped with a screw cap and PTFE/silicone septum. Desorption was performed directly in the gas chromatograph injector port for 5 min at 250 °C using the splitless mode. The proposed method is sensible (with detection limits between 0.0045 and 0.2399 mg/L), precise (with coefficients of variation in the range 0.99–8.18%), and linear over more than 1 order of magnitude. The developed method presented recoveries comprised between 76.0 and 112.4%. The applicability of the new method was demonstrated by determining the considered 22 volatile compounds in nine orujo commercial samples with quality and origin brands.