PMID- 18377916 OWN - NLM STAT- MEDLINE DCOM- 20080813 LR - 20090115 IS - 0021-9673 (Print) IS - 0021-9673 (Linking) VI - 1190 IP - 1-2 DP - 2008 May 9 TI - Quantitative analysis of 3-alkyl-2-methoxypyrazines in juice and wine using stable isotope labelled internal standard assay. PG - 294-301 LID - 10.1016/j.chroma.2008.02.088 [doi] AB - A solid phase microextraction (HS-SPME)-GC-MS methodology was established for the analysis of 3-alkyl-2-methoxypyrazines (MPs) in wine using a stable isotope dilution assay. The compounds analysed were 3-isobutyl-2-methoxypyrazine (IBMP), 3-sec-butyl-2-methoxypyrazine (SBMP), and 3-isopropyl-2-methoxypyrazine (IPMP) using their respective deuterated analogues ([2H3]-IBMP, [2H3]-SBMP, [2H3]-IPMP) as internal standards, synthesised during this work. A divinylbenzene/carboxene/polydimethylsiloxane (DVB/CAR/PDMS) fibre was selected for isolation of MPs and the effects of matrix parameters such as pH and ethanol concentration were examined in the development of the method. Best results were obtained at a pH of approximately 6 and with a wine dilution factor of 1:2.5, resulting in an ethanol concentration of approximately 5% (v/v). Relative standard deviations (RSDs) of replicate samples were 5.6-7% for all MPs at 5 ng L(-1) and <5% for 15 and 30 ng L(-1) samples. The limit of detection was <0.5 ng L(-1) in juice and 1-2 ng L(-1) in wine. The recovery efficiencies for spiked wine samples were between 99 and 102% for all three MPs. Using this method, we investigated the impact of the Multicoloured Asian Lady Beetle (MALB) on MPs in wine. In red wine fermented with live MALB, IPMP is the most prevalent MP detected, although SBMP concentrations are also increased and IBMP is unchanged from background levels. MALB that have been dead for 1 day before addition to juice can still contribute to elevated SBMP concentrations in wine, but not if they have been dead for 3 days or longer. Clarifying juice prior to fermentation leads to substantially lower IPMP concentration in the subsequent wine when compared with unclarified juice. FAU - Kotseridis, Y S AU - Kotseridis YS AD - Department of Food Science & Technology, Agricultural University of Athens, Athens, Greece. ykotseridis@aua.gr FAU - Spink, M AU - Spink M FAU - Brindle, I D AU - Brindle ID FAU - Blake, A J AU - Blake AJ FAU - Sears, M AU - Sears M FAU - Chen, X AU - Chen X FAU - Soleas, G AU - Soleas G FAU - Inglis, D AU - Inglis D FAU - Pickering, G J AU - Pickering GJ LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20080302 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Isotopes) RN - 0 (Pyrazines) SB - IM MH - Beverages/*analysis MH - Calibration MH - Isotopes MH - Magnetic Resonance Spectroscopy MH - Pyrazines/*analysis MH - Reference Standards MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Wine/*analysis EDAT- 2008/04/02 09:00 MHDA- 2008/08/14 09:00 CRDT- 2008/04/02 09:00 PHST- 2007/12/28 00:00 [received] PHST- 2008/02/20 00:00 [revised] PHST- 2008/02/25 00:00 [accepted] PHST- 2008/04/02 09:00 [pubmed] PHST- 2008/08/14 09:00 [medline] PHST- 2008/04/02 09:00 [entrez] AID - S0021-9673(08)00396-8 [pii] AID - 10.1016/j.chroma.2008.02.088 [doi] PST - ppublish SO - J Chromatogr A. 2008 May 9;1190(1-2):294-301. doi: 10.1016/j.chroma.2008.02.088. Epub 2008 Mar 2.