热分离进样/气相色谱-质谱法测定橄榄油中脂肪酸乙酯

建立了热分离进样/气相色谱-质谱快速测定橄榄油中4种脂肪酸乙酯(棕榈酸乙酯、硬脂酸乙酯、油酸乙酯、亚油酸乙酯)的分析方法。采用热分离进样技术进样,以DB-5MS色谱柱分离,选择离子监测模式检测。结果显示,4种脂肪酸乙酯在0.01~0.20 mg/L范围内线性良好(r^2>0.999),方法的检出限(LOD)和定量下限(LOQ)分别为0.3 mg/kg和1.0 mg/kg,在低、中、高3个加标水平(1.0、2.0、10 mg/kg)下的回收率为82.4%~109%,相对标准偏差(RSD)为0.68%~6.8%。该方法灵敏度高,准确度和重现性好,可用于橄榄油中4种脂肪酸乙酯的快速检测。

Determination of Fatty Acid Ethyl Esters in Olive Oil by Gas Chromatography-Mass Spectrometry with Thermal Separation Injection

A gas chromatography-mass spectrometric method with thermal separation injection was developed for the rapid detection of 4 fatty acid ethyl esters,i.e.palmitic acid ethyl ester,linoleic acid ethyl ester,oleic acid ethyl ester and stearic acid ethyl ester in olive oil.The target compounds were volatilized at appropriate inlet temperature,separated on a DB-5MS column,and detected in selected-ion monitoring mode.Results showed that the standard curves for 4 analytes were linear over the concentration range of 0.01-0.20 mg/L,with correlation coefficients(r2) greater than 0.999.The limits of detection(LODs) and limits of quantitation(LOQs) of the method were 0.3 mg/kg and 1.0 mg/kg,respectively.Recoveries at three levels of 1.0,2.0 and 10 mg/kg ranged from 82.4% to 109%,with relative standard deviations of 0.68%-6.8%.The method is sensitive,accurate and stable,and is suitable for the rapid detection of 4 fatty acid ethyl esters in olive oil.