Determination of Volatile Phenols in Wine by Gas Chromatography Tandem Mass Spectrometry with Distillation and Liquid-Liquid Extraction
摘 要
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%。
Abstract
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%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202306011
所属栏目 工作简报
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收稿日期 2022/10/9
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备注王焕琦,工程师,研究方向为食品质量与安全
引用该论文: WANG Huanqi,NIE Siping,WANG Zhengqiang. Determination of Volatile Phenols in Wine by Gas Chromatography Tandem Mass Spectrometry with Distillation and Liquid-Liquid Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(6): 683~689
王焕琦,聂四平,王正强. 蒸馏法-液液萃取-气相色谱-串联质谱法测定葡萄酒中挥发性酚类物质的含量[J]. 理化检验-化学分册, 2023, 59(6): 683~689
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参考文献
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【2】RAPP A. Volatile flavour of wine: Correlation between instrumental analysis and sensory perception[J]. Die Nahrung, 1998,42(6):351-363.
【3】ROBINSON A L, BOSS P K, SOLOMON P S, et al. Origins of grape and wine aroma. Part 1. Chemical components and viticultural impacts[J]. American Journal of Enology and Viticulture, 2014,65(1):1-24.
【4】STYGER G, PRIOR B, BAUER F F. Wine flavor and aroma[J]. Journal of Industrial Microbiology & Biotechnology, 2011,38(9):1145-1159.
【5】VAN BEEK S, PRIEST F G. Decarboxylation of substituted cinnamic acids by lactic acid bacteria isolated during malt whisky fermentation[J]. Applied and Environmental Microbiology, 2000,66(12):5322-5328.
【6】BALTES W, WITTKOWSKI R, SÖCHTIG I, et al. Ingredients of smoke and smoke flavor preparations[M]//The Quality of Foods and Beverages. Amsterdam:Elsevier, 1981:1-19.
【7】KENNISON K R, GIBBERD M R, POLLNITZ A P, et al. Smoke-derived taint in wine: The release of smoke-derived volatile phenols during fermentation of Merlot juice following grapevine exposure to smoke[J]. Journal of Agricultural and Food Chemistry, 2008,56(16):7379-7383.
【8】DÍEZ J. Optimisation of stir bar sorptive extraction for the analysis of volatile phenols in wines[J]. Journal of Chromatography A, 2004,1025(2):263-267.
【9】VANBENEDEN N, DELVAUX F, DELVAUX F R. Determination of hydroxycinnamic acids and volatile phenols in wort and beer by isocratic high-performance liquid chromatography using electrochemical detection[J]. Journal of Chromatography A, 2006,1136(2):237-242.
【10】TEMPōRE S, CUZANGE E, SCHAAPER M H, et al. “Brett character” in wine: Is there a consensus among professional assessors? A perceptual and conceptual approach[J]. Food Quality and Preference, 2014,34:29-36.
【11】轻工业部食品发酵研究所发酵室,酒分析小组.气相色谱法分析白酒的挥发性酚元化合物[J]. 食品与发酵工业, 1980(6):10-15.
【12】庄名扬.酱香型白酒中微量成分的生理活性[J].酿酒, 2006,33(6):109-110.
【13】徐岩,范文来,葛向阳,等.科学认识中国白酒中的生物活性成分[J].酿酒科技, 2013(9):1-6.
【14】寻思颖,董睿,彭黔荣,等.高效液相色谱法测定酱香型白酒中挥发性酚类物质[J].食品科学, 2012,33(24):239-243.
【15】赵雅敏,林琳,王和玉,等.液-液微萃取结合气相色谱-质谱联用技术快速测定饮料酒中挥发性酚类化合物[J].分析科学学报, 2018,34(6):789-794.
【16】CARRILLO J D, TENA M T. Determination of ethylphenols in wine by in situ derivatisation and headspace solid-phase microextraction-gas chromatography-mass spectrometry[J]. Analytical and Bioanalytical Chemistry, 2007,387(7):2547-2558.
【17】朱燕,范文来,徐岩.应用DI-SPME和GC-MS分析白酒中游离挥发性酚类化合物[J].食品与发酵工业, 2010,36(10):138-143.
【18】ZHOU Q, QIAN Y P, QIAN M C. Analysis of volatile phenols in alcoholic beverage by ethylene glycol-polydimethylsiloxane based stir bar sorptive extraction and gas chromatography-mass spectrometry[J]. Journal of Chromatography A, 2015,1390:22-27.
【19】傅玉书,胡国栋,龚书宝.气相色谱法分析白酒的非挥发性酚类化合物[J].色谱, 1985(增刊1):111-115.
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