摘要
建立吸附法进行香气提取、气相色谱-质谱法测定不同酒龄黄酒中挥发性香气物质的方法。对比分析固相微萃取和搅拌棒吸附萃取对黄酒香气提取的效果,获得优化的香气提取方法。结果表明:采用搅拌棒吸附萃取-气相色谱-质谱法测定黄酒挥发性香气物质的平均相对标准偏差为11.47%,回收率为88.6%~92.3%,说明所建方法稳定;采用搅拌棒吸附萃取-气相色谱-质谱法共测得60种挥发性香气物质,其中15种醇类物质、25种酯类、6种醛类和5种酸类物质;随酒龄增加,乙醇含量逐渐减少,而11种酯类、1种醇类、1种酮类和1种醛类含量逐渐增加,随陈酿时间增加,部分醇、醛类物质被催化氧化成有机酸,酸的增加促进了酯化反应。搅拌棒吸附萃取-气相色谱-质谱法具有前处理简单快捷、重复性好等优点,可为黄酒香气分析提供准确可靠的数据。
A method was developed for the determination of volatiles in Chinese rice wine with different aging times by gas chromatography-mass spectrometry(GC-MS) with sorptive extraction.Solid phase microextraction(SPME) and stir bar sorptive extraction(SBSE) were compared to select the best extraction method among the two.Compared with SPME,SBSE resulted in a higher-fold enrichment and a lower limit of detection.The average relative standard deviation(RSD) of the developed SBSE/GC-MS method(6 parallel determinations) was 11.47% and the recoveries for isobutyl alcohol,furfural and ethyl acetate were in the range of 88.6%-92.3%,suggesting its good stability.Sixty volatiles were identified and quantified,including 15 alcohols,25 esters,6 aldehydes and 5 acids,and others.With increasing aging time,ethanol concentration showed a gradual decrease,while the concentrations of 11 esters,1 alcohol,1 ketone and 1 aldehyde gradually increased.These changes may be caused by the oxidation of alcohols and aldehydes into acids followed by the esterification of acids and alcohols during storage.In conclusion,SBSE/GC-MS is a reliable method allowing the determination of volatiles in Chinese rice wine.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2011年第22期179-183,共5页
Food Science
基金
教育部高等学校全国优秀博士论文作者资助专项(201059)
上海市自然科学基金项目(10ZR1429600)
关键词
黄酒
搅拌棒吸附萃取
固相微萃取
气相色谱-质谱法
Chinese rice wine
stir bar sorptive extraction(SBSE)
solid phase microextraction(SPME)
gas chromatography-mass spectrometry(GC-MS)