气相色谱-质谱法测定白酒中邻苯二甲酸酯

Determination of Phthalic Acid Esters in Liquor by Gas Chromatography-Mass Spectrometry

建立了白酒中15种邻苯二甲酸酯类化合物（PAEs）残留量的气相色谱-电子轰击离子源质谱（GC-EI/MS）测定方法。样品通过旋转蒸发除乙醇,正己烷超声提取,LC-Si SPE小柱净化,氮吹浓缩后进行气相色谱-质谱法分析。结果表明：该方法具有良好的线性关系,相关系数（r^2）大于0.998,平均加标回收率为85.3%-103.1%,相对标准偏差为3.8%-8.8%,15种邻苯二甲酸酯（PAEs）的方法检出限（MDL）为0.011-0.041mg/L。该方法具有简单、快速、灵敏度高和定性定量准确等优点,满足各类白酒样品的分析要求。

A gas chromatography-mass spectrometry（GC-MS）method was developed for the determination of 15 PAEs residues in liquor samples.The samples were extracted by ultrasonic extraction with n-hexane and purified with LC-Si solid phase extraction column,and then were concentrated and analyzed by GC-MS.The results showed that the calibration curves were in good linearity between the peak area and the concentration of 0.05-8.0μg·mL-1 for 15 PAEs with correlation coefficients not less than 0.998,the average spiked recoveries ranged from 85.3% to 103.1%,the relative standard deviations ranged from3.8%-8.8%,and the detection limits of the method（MDL）were less than 0.041mg/L.The proposed method was simple,rapid,sensetive and accutate,and could meet the requirements of the analysis of various liquor samples.