Millán Silvia, Sampedro M Carmen, Unceta Nora, Goicolea M Aranzazu, Barrio Ramón J
Department of Analytical Chemistry, Faculty of Pharmacy, University of Basque Country, Spain.
Anal Chim Acta. 2007 Feb 12;584(1):145-52. doi: 10.1016/j.aca.2006.10.042. Epub 2006 Nov 7.
A rapid liquid chromatographic-electrospray ionisation ion trap mass spectrometry (LC-ESI-ITMS) method has been developed for the routine analysis of eight of the most oenologically important biogenic amines in wine without any sample pre-treatment. The method involves addition of heptylamine as an internal standard (IS) and the direct injection of filtered wine samples previously diluted with ultra high purity (UHP) water. The full-scan MS-MS spectra and the identical retention times to those of reference standards were used for unequivocal identification of the analytes. For most amines, the most abundant ions were derived from the loss of an ammonia group, while in the case of spermine and the I.S. the major product ions arose from the loss of 1,3-propyldiamine and the production of adduct with water, respectively. Detection was achieved in positive ionisation with an ion trap mass spectrometer operating in multiple-reaction monitoring (MRM) mode. The method allowed accurate determination of the analytes in the range 0.5-40 ng mL(-1). Within-day and between-day relative standard deviation percentages were <8% and <12%, respectively. The overall process was successfully applied to identify and quantify biogenic amines in Rioja red wines. The new method is sensitive, rapid, cheap and less labour intensive.
已开发出一种快速液相色谱 - 电喷雾电离离子阱质谱法(LC - ESI - ITMS),用于在无需任何样品预处理的情况下对葡萄酒中八种最重要的葡萄酒酿造生物胺进行常规分析。该方法包括加入庚胺作为内标(IS),并直接进样预先用超纯水(UHP)稀释过的经过滤的葡萄酒样品。通过全扫描MS - MS谱图以及与参考标准品相同的保留时间来明确鉴定分析物。对于大多数胺类,最丰富的离子源自氨基团的丢失,而对于精胺和内标,主要产物离子分别源自1,3 - 丙二胺的丢失和与水加合物的产生。使用在多反应监测(MRM)模式下运行的离子阱质谱仪在正离子模式下进行检测。该方法能够准确测定浓度范围为0.5 - 40 ng mL⁻¹的分析物。日内和日间相对标准偏差百分比分别<8%和<12%。整个过程已成功应用于里奥哈红葡萄酒中生物胺的鉴定和定量。新方法灵敏、快速、成本低且劳动强度小。