[关键词]
[摘要]
本文采用液液萃取方法,用3 mL葡萄酒样、7 mL水、4.5 g硫酸铵和60 μL 0.02% (V/V)的内标(4-甲基-2-戊醇)溶液混合,再加入0.5 mL二氯甲烷作为萃取溶剂,涡旋10 min后离心10 min,取下层提取物进行气相色谱分析,以ZB-WAX毛细柱(30 m×0.25 mm×0.25 μm)为分析用色谱柱,柱温40 ℃保持5 min后以3 ℃/min升温至190 ℃,保持10 min;载气为高纯氮气,流速1.5 mL/min;进样量0.5 μL;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。
[Key word]
[Abstract]
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 × 0.25 mm × 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 min. 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.
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[基金项目]
广州市科技项目基础研究专项(11C15380690)