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

Optimization of Precolumn Derivatization for Simultaneous Gas Chromatography-Mass Spectrometric Analysis of Non-volatile Flavor Compounds in "Angeleno" Plum Fruit

对气相色谱与质谱联用(GC-MS)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200μL李果实的甲醇提取液,蒸干后加入250μL衍生化试剂(甲氧胺盐酸盐的吡啶溶液,20mg/mL),30℃条件下衍生反应2～2.5h;然后再加入250μLN-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。

This paper reports the orthogonal array optimization of some conditions for precolumn derivatization of non-volatile flavor compounds from ＂Angeleno＂plum fruit prior to gas chromatography-mass spectrometric （GC-MS） analysis.An optimal derivatization was achieved by allowing 200μ L of methanol extract of ＂Angeleno＂ plum fruit to react with 250μL 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.