溶剂辅助蒸馏-气相色谱-串联质谱法分析酿酒葡萄中的游离态萜烯类化合物

Analysis of Free Terpenoids in Four Vitis vinifera Varieties Using Solvent Assisted Flavour Evaporation and Gas Chromatography-Tadem Mass Spectrometry

应用气相色谱-串联质谱联用技术(GC-MS/MS)和溶剂辅助蒸馏技术(SAFE)对4种酿酒葡萄中的游离态萜烯类化合物进行了研究。采用恒温振荡法浸提葡萄中的成分,溶剂辅助蒸馏法除去不挥发性成分,提取液经氮吹浓缩后进行GC-MS/MS分析。实验中优化了SAFE条件(循环水浴温度、样品流量)。通过NIST05a谱库检索、标准品的保留指数(RI值)对比及参考文献的RI值对比分析,在4种葡萄中共鉴定出30种萜烯类化合物,其中包括10种单萜烯类化合物、18种倍半萜烯类化合物、1种二萜烯类化合物以及1种三萜烯类化合物。在蛇龙珠葡萄中检出了28种萜烯类化合物,在梅鹿辄、赤霞珠和品丽珠葡萄中分别检出了16,17和16种萜烯类化合物。在蛇龙珠葡萄中检出了17种倍半萜烯类化合物,远多于其他3种酿酒葡萄。通过半定量分析,发现在赤霞珠葡萄中单萜烯类化合物含量较高,在蛇龙珠葡萄中倍半萜烯化合物含量较高。实验结果表明,该方法适用于酿酒葡萄中游离态萜烯类成分的定性和定量分析。

The free terpenoids in four Vitis vinifera varieties were studied by solvent assisted flavour evaporation （SAFE） and gas chromatography-tadem mass spectrometry （GC-MS/MS）. The compounds of the grapes were extracted with vibrating extraction at constant temperature, and then the non-volatiles were removed by SAFE. The volatile compounds were concentrated with a stream of nitrogen and analyzed by GC-MS/MS. The temperature of cycle water and flow rate of the sample were optimized in SAFE procedure. In the four varieties of grapes, a total of 30 terpenoids were identified by mass spectral data from NIST05a and Kovats retention indices of the standards （RIS ） or from the literature （RIL） , including 10 monoterpenoids, 18 sesquiterpenoids, 1 diterpenoid, and 1 triterpenoid. Twenty-eight terpenoids were detected in Cabernet Gernischt, and 16, 17, and 16 in Merlot, Cabernet Sauvignon, and Cabernet Fanc, respectively. A total of 17 sesquiterpenoids were identified in Cabernet Gernischt, and it was the richest among the four grapes. According to semi-quantitative method, the concentration of monoterpenoids in Cabernet Sauvignon was the highest among the four grapes, whereas the concentration of sesquiterpenoids in Cabernet Gernischt was the highest. The results showed that this method can be used to identify and quantify the free terpenoids in grapes.