GC-MS法同时测定食品接触材料中4种对羟基苯甲酸酯的特定迁移量

Simultaneous Determination of Specific Migration of Four p-hydroxybenzoates in Food Simulants by GC-MS

建立了气相色谱/质谱法（GC-MS）同时测定3%乙酸、10%乙醇、20%乙醇、50%乙醇和植物油食品模拟物中对羟基苯甲酸甲酯（MPHB）、对羟基苯甲酸乙酯（EPHB）、对羟基苯甲酸异丙酯（IPPHB）和对羟基苯甲酸丙酯（PPHB）的特定迁移量。实验结果表明：4种对羟基苯甲酸酯在HP-5柱上12.5 min内达到基线分离,在0.05-10 mg/L或0.5-100 mg/kg范围内线性关系良好（r2〉0.999 6）,在5、40、100 mg/kg三水平的加标回收率为93.6%-106%,相对标准偏差为0.21%-6.21%;在五种食品模拟物中方法的定量限为0.2-0.5 mg/kg。所建立的检测方法用于对塑料类食品接触材料样品中4种对羟基苯甲酸酯特定迁移量的检测,结果令人满意。

A novel method for simultaneous determination of specific migration（SM） of methyl-phydroxybenzoate, ethyl-p-hydroxybenzoate, iso-propyl-p-hydroxybenzoate and propyl-p-hydroxybenzoate in food simulants（3% acetic acid, 10% ethanol, 20% ethanol, 50% ethanol and olive oil） was developed by gas chromatography mass spectrometry（GC-MS）. After the migration test, the soaking solution was cooled down, and vortexed. The olive oil food simulant sample was extracted with isopropanol ethanol solution, while one milliliter of other aqueous food simulant（3% acetic acid, 10% ethanol, 20% ethanol or 50% ethanol solution） sample was diluted to 10 milliliter with isopropanol. And the clear supernatant from olive oil food simulant sample and the diluted aqueous food simulant samples were dried with anhydrous sodium sulfate, and then filtered through a polytetrafluoroethylene filter with a disposable syringe before injection. The baseline separation of four p-hydroxybenzoates was achieved within 12.5 min on a HP-5 column. External standard method of calibration curve was adopted via mass spectrometer detector. The regression coefficient of linearity of the method was over 0.999 6 from 0.05 to 10 mg/L or 0.5 to 100 mg/kg. The recoveries of them were between 93.6% and 106%, and the corresponding the relative standard deviation were between 0.21% and 6.21% at 5, 40, 100 mg/kg. The limits of quantification were between 0.2-0.5 mg/kg. The method was applied to analyze the migration of four p-hydroxybenzoates from plastic packing samples with satisfactory results.