摘要
本文采用液液萃取方法，用3mL葡萄酒样、7mL水、4．5g硫酸铵和60μL0．02％（嘲的内标（4．甲基．2．戊醇）溶液混合，再加入0．5mL二氯甲烷作为萃取溶剂，涡旋10min后离心10min，取下层提取物进行气相色谱分析，以ZB—WAX毛细柱（30m×0．25mm×0．25μm）为分析用色谱柱，柱温40℃保持5vain后以3℃／min升温至190℃，保持10min；载气为高纯氮气，流速1．5mL／min；进样量0．5μL；进样口200℃；不分流模式进样，以FID为检测器。该方法能良好分离出葡萄酒中63种化合物，其中用标准物质定性了30种香气成分，包括9种醇类，11种酯类，8种酸类，2种醛酮类。所定性香气成分定量结果重复性良好，有28种成分RSD％小于10％；采用内标法进行定量分析，定量准确性高，有28种成分回收率在85～120％之间。本方法操作简便，污染小，前处理时间短，且重复性良好，定量准确度高，符合进一步作葡萄酒指纹分析的技术要求。
In this paper, 3 mL wine was diluted with water （7 mL） and internal standard solution （60 μL 0.02% （V/V） 4-Methyl-2-pentanol）, salted with 4.5 g ammonium sulfate and then extracted with 0.5 mL dichloromethane. After scrolled for 10 min and centrifuged for 10 min, the extract was injected in a GC system. ZB-WAX capillary column （30 m ×0.25mm×0.25 μm） used with the temperature program was as follows： 40 ℃ for 5 min, then raised at 3 ℃/min up to 190℃ for 10 rnin. N2 was used as carrier gas with flow rate of 1.5 mL/min, injection volume and input temperature were 0.5 mL and 200 ℃, and the injection mode was splitless. The results were detected by FID. The method could isolate 63 compounds from wine, and 30 of them were analyzed qualitatively. They included nine alcohols, eleven esters, eight organic acids, two aldoketones. Repeatability of 28 of them was less than 10% （as RSD） with the recoveries from 85% to 120%. The quantitative analysis by using internal standard solution was accurate. This method has the advantages of simple operation, little pollution, short time of pretreatment and good repeatability and accuracy, which satisfies the further demand of wine fingerprinting analysis technology.
出处
《现代食品科技》
EI
CAS
北大核心
2014年第6期281-288,共8页
Modern Food Science and Technology
基金
广州市科技项目基础研究专项(11C15380690)
关键词
液液萃取
气相色谱法
葡萄酒
挥发性成分
定量分析
内标法
liquid-liquid extraction
gas chromatography
wine
volatile compounds
quantitative analysis
internal standard method
