摘要
目的建立气相色谱内标法测定白酒中甲醇含量的方法。方法选择色谱柱为HP-INNOWAX石英毛细管柱,载气为氮气,流速为2.0 mL/min。检测器为火焰离子化检测仪(flame ionization detector,FID),温度为250℃;进样口温度为200℃;分流比为5:1;采用液体直接进样,溶剂为40%(V/V)乙醇,内标物质为叔戊醇。结果被测物甲醇和内标物质叔戊醇均能得到很好的分离,空白溶剂无干扰;在线性范围100.9~1008.6 mg/L内,方法线性方程为Y=0.002155X+0.012511,相关系数为0.9999;方法检出限为5.0 mg/L、定量限为16.7 mg/L;平均回收率分别为96.8%~99.6%,相对标准偏差(relative standard deviation,RSD)不超过0.45%结论方法操作简单,进样时间短,数据准确,重复性好,适用于白酒中甲醇含量的检测。
Objective To develop a method for determination of methanol in liquor by internal standard method of gas chromatography.Methods HP-INNOWAX quartz capillary column was chosen as the chromatographic column,and the carrier gas was nitrogen,with the 2.0 mL/min flow rate.The detector was flame ionization detector(FID)and the temperature was 250℃;The inlet temperature was 200℃and the split ratio was 5:1.The sample was directly injected by liquid,the solvent was 40%(V/V)ethanol,and the internal standard material was tert-amyl alcohol.Results Both the test substance methanol and the internal standard substance tert-amyl alcohol were well separated without the interference from blank control.In the linear range of 100.9-1008.6 mg/L,the linear equation of the method was Y=0.002155 X+0.012511,with a correlation coefficient 0.9999.The detection limit was 5.0 mg/L and the quantitative limit was 16.7 mg/L.The average recoveries were 96.8%-99.6%,and the relative standard deviation(RSD)no more than 0.45%.Conclusion The method has the advantages of simple operation,short injection time,accurate data,and good repeatability and can be used for the determination of methanol content in liquor.
作者
冯俊富
朱飞如
FENG Jun-Fu;ZHU Fei-Ru(Beihai food and Drug Inspection Institute,Beihai 536000,China)
出处
《食品安全质量检测学报》
CAS
2020年第13期4521-4525,共5页
Journal of Food Safety and Quality
关键词
气相色谱法
内标法
白酒
甲醇
gas chromatography
internal standard method
liquor
methanol
