GC_MS法同时测定_安哥诺_李果实非挥发性风味物质衍生化条件研究.pdfVIP

186 2010, Vol. 31, No. 14 食品科学 ※分析检测 GC-MS法同时测定 “安哥诺”李果实非挥发性 风味物质衍生化条件研究 胡 玲，王友升* ，李丽萍 (北京工商大学化学与环境工程学院，植物资源研究开发北京市重点实验室，北京 10004 8) 摘 要：对气相色谱与质谱联用(GC-M S)法同时测定 “安哥诺”李果实中的非挥发性风味物质的衍生化条件进行 研究。通过正交试验得到较优条件：取200 μL 李果实的甲醇提取液，蒸干后加入250 μL 衍生化试剂( 甲氧胺盐酸盐 的吡啶溶液，2 0 m g/ m L ) ，3 0 ℃条件下衍生反应2 ～2 .5h ；然后再加入2 5 0 μL N - 甲基三甲基硅基三氟乙酰胺 (MSTFA) ，于37 ℃条件下衍生化30min ；将完成衍生化的样品存放24h 后进样GC-MS 分析。采用此方法可快速地 对李果实中的有机酸、糖类和氨基酸等非挥发性风味物质进行同时检测，方法稳定性好。 关键词：G C - M S ；衍生化；有机酸；糖类；氨基酸 Optimization of Precolumn Derivatization for Simultaneous Gas Chromatography-Mass Spectrometric Analysis of Non-volatile Flavor Compounds in ,, Angeleno,, Plum Fruit HU Ling ，WANG You-sheng* ，LI Li-ping (Beij ing Key Laboratory for Plant Resources Research and Development, School of Chemical and Environmental Engineering, Beij ing Technology and Business University, Beij ing 100048, China) Abstract ：This paper reports the orthogonal array optimization of some condition s for precolumn derivatization of non- volatile flavor compounds from ,,Angeleno,, plum fruit prior to gas chromatography-mass spectrometric (GC-MS) analy sis. An optimal derivatization was achieved by allowing 200 μL of methanol extract of ,,Angeleno,, plum fruit to react with 250 μL of pyridine containing 20 mg/mL of methoxyamine hydrochloride for 2 －2.5 h at 30 ℃, followed by addition of 250 μL of MSTFA for reaction at 37 ℃for another 30 min . Storage for 24 h was carried out before GC-MS analysis. This method can allow the rapid simultaneous determination of organic acids, sugars and amino acids in plum fruit with good reproducibility. Key words ：GC-M S ；sily lation ；organic acid s ；su gars ；amin o acids