色谱

色谱 ›› 2011, Vol. 29 ›› Issue (01): 42-48.DOI: 10.3724/SP.J.1123.2011.00042

• 研究论文 • 上一篇    下一篇

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

郭春海, 薄海波*, 段文仲, 贾海涛, 陈瑞春, 马育松, 艾连峰   

  1. 河北出入境检验检疫局, 河北 石家庄 050051
  • 收稿日期:2010-09-26 修回日期:2010-11-30 出版日期:2011-01-28 发布日期:2011-01-28
  • 通讯作者: 薄海波,博士,高级工程师,主要研究方向为食品安全与质量分析研究. E-mail: bohb1212@163.com.
  • 基金资助:

    国家质监总局科研计划项目(No. 2008IK116).

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

GUO Chunhai, BO Haibo*, DUAN Wenzhong, JIA Haitao, CHEN Ruichun, MA Yusong, AI Lianfeng   

  1. Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang 050051, China
  • Received:2010-09-26 Revised:2010-11-30 Online:2011-01-28 Published:2011-01-28
  • Contact: BO Hai-Bo

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被引次数

76

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0.9910～0.9999,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。

关键词: 气相色谱-质谱, 迁移量, 食品模拟物, 塑料食品包装, 增塑剂

Abstract: 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 0.9910~0.9999. 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.

Key words: food contact packaging materials, food simulants, migration, plasticizers, gas chromatography-mass spectrometry (GC-MS)