气相色谱-质谱法测定食用油中3-氯丙醇酯

Determination of 3-chloropropanol-1,2-diol(3-MCPD)Esters in Edible Oil by Gas Chromatography and Mass Spectrometry

采用碱水解方式,基于苯基硼酸 （PBA）衍生化方法并结合气相色谱/质谱 （GC/MS） 联用仪测定了植物油中3-氯丙醇 （3-MCPD） 酯的含量。水解时间是碱水解样品前处理方法的关键因素,经优化,大豆油等不同品类的食用油的最佳水解时间为 1-6 min。另外,以大豆油为基质,考察了基于碱水解方式的分离分析方法的回收率、重复性以及检出限。其中,在 150-1500 μg/kg范围内进行3水平重复加标回收实验,回收率为 94%-105%、RSD为3.7%-10.8%、检出限为 15 μg/kg,定量限为 50 μg/kg。本方法能够满足日常样品中3-氯丙醇 （3-MCPD） 酯的检测。

3-chloropropanol-1,2-diol（3-MCPD）Sesters inSedible oilSwas determined by gas chromatography/mass spectrometry （GC/MS） after alkaline hydrolysis and derivatization with phenylboronic acidS（PBA） sequentially. The hydrolysisStime is a critical factor inSsampleSpretreatment procedures. The optimum hydrolysisStime of differentSedible oilsSranged from 1min to 6 min. The recovery,Srepeatability and detection limit were evaluated with soybeanSoils as the research model. Based on the threeSlevels spike in the rangeSof 150-1500Sμg/kg, the recovery was between 94% and 105%, while the relative standard deviation ranged from 3.7%~10.8%. In addition, the limit of detection （LOD） and the limit of quantification were 15 μg/kg and 50 μg/kg, respectively. This method could meet with requirements of the routine detection of 3-chloropropanol-1,2-diol（3-MCPD）Sesters in edible oil.