气相色谱-质谱法测定聚氯乙烯包装材料和食品模拟物中的46种增塑剂

Determination of 46 plasticizers in food contact polyvinyl chloride packaging materials and their migration into food simulants by gas chromatography-mass spectrometry

建立了46种增塑剂在聚氯乙烯（PVC）食品包装材料中的含量及其在水、3%乙酸、10%乙醇和橄榄油4种食品模拟物中迁移量的气相色谱-质谱（GC-MS）测定方法。食品包装材料、水质模拟物和橄榄油中增塑剂分别采用溶解-沉淀法、正己烷液-液萃取和凝胶渗透色谱（GPC）法提取。采用GC-MS法,在选择离子监测模式（SIM）下对46种增塑剂进行定性,采用外标法进行定量测定。各种增塑剂在0.1-2.0mg/L质量浓度范围内呈线性,相关系数为0.991 0-0.999 9,各组分检出限均在0.005-0.05mg/kg之间。在2种食品模拟物中,3个浓度添加水平下46种增塑剂的加标回收率在69.51%-107.21%之间,精密度（RSD,n=6）为3.53%-18.95%。该方法可满足PVC食品接触制品及4种不同性质的食品模拟物中多种类增塑剂的快速筛查和准确定性、定量测定要求。

A gas chromatography-mass spectrometry（GC-MS） method was developed for the determination of 46 plasticizers in food contact polyvinyl chloride（PVC） packaging materials and their migration into food simulants,i.e.water,3% acetic acid, 10% ethanol and olive oil.Plasticizers in the PVC packaging materials,aqueous food simulants and olive oil food simulants were extracted by the dissolutionprecipitation,liquid-liquid extraction and gel permeation chromatography（GPC） approaches,respectively.The extracts were analyzed by GC-MS in selective ion monitoring（SIM） mode and quantified using the external standard method.The calibration curves were linear in the ranges of 0.1-2.0 mg/L with the correlation coefficients of 0.991 0-0.999 9.The limits of detection were from 0.005 mg/kg to 0.05 mg/kg（S/N=5）.The recoveries at 3 spiked levels were 69.51%-107.21% and the relative standard deviations（RSDs, n=6） ranged from 3.53% to 18.95%.These results show that this method is fast,sensitive and accurate for the qualitative and quantitative determination of plasticizers in food contact plastic products and 4 types of food simulants.