提出了蒸馏法-液液萃取-气相色谱-串联质谱法(GC-MS/MS)测定葡萄酒中挥发性酚类物质含量的方法。取100 mL葡萄酒样品(液温20 ℃)于500 mL蒸馏瓶中,连接冷凝管进行蒸馏,收集馏出液100 mL。取馏出液20 mL于50 mL离心管中,加入20 μL内标溶液(25.0 mg·L^-1 3,4-二甲基苯酚的乙醇溶液),涡旋振荡5 min,混匀。加入氯化钠使之饱和(氯化钠质量浓度为360 g·L^-1),用10 mL二氯甲烷进行萃取(5 mL/次×2次),每次萃取振荡5 min,超声10 min,离心5 min。合并的有机相用3.0 g无水硫酸钠除水后,于35 ℃氮吹至1 mL。采用GC-MS/MS测定所得溶液中14种挥发性酚类物质的含量。结果表明,14种挥发性酚类物质的质量浓度与内标质量浓度的比值在一定范围内跟对应的峰面积比值呈线性关系,检出限(3S/N)为0.5~9.2 μg·L^-1。按照标准加入法进行回收试验,回收率为87.3%~107%,测定值的相对标准偏差(n=6)为0.70%~5.6%。

A method for determination of volatile phenols in wine by gas chromatography tandem mass spectrometry (GC-MS/MS) with distillation and liquid-liquid extraction was proposed. 100 mL of wine sample (liquid temperature of 20 ℃) was taken and put into a 500 mL-distillation bottle, connecting the condenser tube for distillation. 100 mL of distillate was collected, 20 mL of which was taken and put into a 50 mL-centrifuge tube. 20 μL of internal standard solution (ethanol solution containing 25.0 mg·L^-1 3,4-dimethylphenol) was added, and the mixture was oscillated by vortex for 5 min and mixed well. Sodium chloride was added to reach saturation (sodium chloride mass concentration of 360 g·L^-1). The solution was extracted with 10 mL of dichloromethane (5 mL/time×2 times, oscillation for 5 min, ultrasound for 10 min and centrifugation for 5 min for each extraction), and the combined organic phase was dehydrated with 3.0 g of anhydrous sodium sulfate and blown to 1 mL by nitrogen at 35 ℃. 14 volatile phenols in the obtained solution were determined by GC-MS/MS. As shown by the results, linear relationships between the mass concentration ratios of 14 volatile phenols to internal standard and the corresponding peak area ratios were found in definite ranges, with detection limits (3S/N) in the range of 0.5-9.2 μg·L^-1. Test for recovery was carried out according to the standard addition method, giving results in the range of 87.3%-107%, with RSDs (n=6) of the determined values in the range of 0.70%-5.6%.