[关键词]
[摘要]
本文对炉温、保温时间、气液相比和盐析试验4个方面对测定葡萄酒中甲醇的顶空—毛细柱气相色谱法进行摸索,确定最优的顶空气相色谱分析条件为:以ZB-WAX毛细柱为分析用色谱柱,分流进样(分流比20:1、2 mm分流衬管);载气流速2.0 mL/min;炉温70 ℃;保温时间15 min;测定液5 mL;不加盐析剂,FID为检测器。方法在甲醇浓度范围10.2~407.6 mg/L之间线性良好,r=0.9997;平均回收率99.2%,样品重现性RSD为1.4%,检出限为8.5 mg/L,本方法与国标GB/T 15038-2006方法相比简便、高效,测定结果可靠。
[Key word]
[Abstract]
In this paper, through four factors such as temperature, time, the ratio of gas-liquid phase and salting out, the determination of methanol in wine by head space GC with capillary column was studied and the optimal conditions were found as following: using a Phenomenex ZB-WAX chromatographic column and a FID detector. The split ratio was 20 with split liner tube (2mm I.D) and the flow rate of carrier gas was 2.0 mL/min. The heated temperature was 70℃ with head space sampling used and vial equilibration time was 15 min and sample volume was 5 mL in a 20mL vial. The linear of this method was satisfied when the concentration of methanol was at the range of 10.2~407.6 mg/L (r=0.9997). The lowest method detection limit was 8.5 mg/L and the average recovery rate was 99.2%. RSD of Repeat was 1.4%. It was shown that this method is more simple and efficient than GC method in GB/T15038-2006, and the result was reliable.
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[基金项目]
广州市科技项目基础研究专项(11C15380690)