Centre de Formation et de la Recherche en Œnologie, UMR 1083 «SPO», Faculté de Pharmacie, Université Montpellier I, 15 Avenue Charles Flahault, F-34093 Montpellier, France.
J Chromatogr A. 2010 Nov 19;1217(47):7385-92. doi: 10.1016/j.chroma.2010.09.047. Epub 2010 Sep 22.
This paper reports a new, simple, rapid and economical method for routine determination of 24 amino acids and biogenic amines in grapes and wine. No sample clean-up is required and total run time including column re-equilibration is less than 40min. Following automated in-loop automated pre-column derivatisation with an o-phthaldialdehyde, N-acetyl-l-cysteine reagent, compounds were separated on a 3mm×25cm C(18) column using a binary mobile phase. The method was validated in the range 0.25-10mg/l; repeatability was less than 3% RSD and the intermediate precision ranged from 2 to 7% RSD. The method was shown to be linear by the 'lack of fit' test and the accuracy was between 97 and 101%. The LLOQ varied between 10μg/l for aspartic and glutamic acids, ethanolamine and GABA, and 100μg/l for tyrosine, phenylalanine, putrescine and cadaverine. The method was applied to grapes, white wine, red wine, honey and three species of physalis fruit. Grapes and physalis fruit were crushed, sieved, centrifuged and diluted 1/20 and 1/100, respectively, for analysis; wines and honeys were simply diluted 10-fold. It was shown using this method that the amino acid content of grapes was strongly correlated with berry volume, moderately correlated with sugar concentration and inversely correlated with total acidity.
本文报道了一种新的、简单、快速且经济的方法，用于常规测定葡萄和葡萄酒中的 24 种氨基酸和生物胺。无需样品净化，总运行时间（包括柱再平衡）小于 40 分钟。在自动在线柱预衍生后，用邻苯二醛和 N-乙酰-L-半胱氨酸试剂衍生，化合物在 3mm×25cm C(18)柱上用二元流动相分离。该方法在 0.25-10mg/l 范围内进行了验证；重复性小于 3%RSD，中间精密度范围为 2-7%RSD。通过“缺乏拟合”检验证明该方法具有线性，准确度在 97%至 101%之间。LLOQ 变化范围为 10μg/l 用于天冬氨酸和谷氨酸、乙醇胺和 GABA，100μg/l 用于酪氨酸、苯丙氨酸、腐胺和尸胺。该方法应用于葡萄、白葡萄酒、红葡萄酒、蜂蜜和三种酸浆属水果。葡萄和酸浆属水果经粉碎、过筛、离心后，分别稀释 1/20 和 1/100 进行分析；葡萄酒和蜂蜜简单稀释 10 倍。使用该方法表明，葡萄中的氨基酸含量与浆果体积密切相关，与糖浓度中度相关，与总酸度成反比。
