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

摘要

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0.1～2.0 mg/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0.005～0.05 mg/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 dissolution-precipitation, 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.