色谱

色谱 ›› 2012, Vol. 30 ›› Issue (07): 647-653.DOI: 10.3724/SP.J.1123.2012.03013

• 研究论文 •    下一篇

仿真饰品中邻苯二甲酸酯类增塑剂的含量测定和迁移风险考察

赖莺*, 黄宗平, 葛秀秀, 林睿, 陈和秀   

  1. 厦门出入境检验检疫局技术中心, 福建 厦门 361026
  • 收稿日期:2012-03-06 修回日期:2012-05-18 出版日期:2012-07-28 发布日期:2012-07-19
  • 通讯作者: 赖莺,博士,高级工程师,主要从事进出口商品的色谱、质谱和光谱等方面的检验和科研工作. Tel: (0592)3269967.
  • 基金资助:

    国家质检总局科研计划项目(2009IK075, 2011IK048).

Determination of phthalic acid esters in imitation jewellery and investigation of their migration risk

LAI Ying*, HUANG Zongping, GE Xiuxiu, LIN Rui, CHEN Hexiu   

  1. Technology Center of Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China
  • Received:2012-03-06 Revised:2012-05-18 Online:2012-07-28 Published:2012-07-19
  • Contact: Ying Lai

PDF

540

被引次数

15

摘要： 建立了仿真饰品中14种邻苯二甲酸酯类增塑剂的含量和迁移量测定的气相色谱-质谱(GC-MS)检测方法。考察了微波萃取、超声波萃取、快速溶剂萃取和索氏提取4种前处理方法对增塑剂含量测定的影响。在模拟人体温度及汗液环境下,考察了0～168 h内塑料仿真饰品中邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)和邻苯二甲酸二辛酯(DOP)3种增塑剂的迁移风险。结果表明微波萃取法的提取效率优于其余3种方法。所建立方法的定量限为5 mg/kg (邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)为25 mg/kg),在0.1～50 mg/L(DINP、DIDP在0.5～250 mg/L)范围内,线性相关系数在0.99以上,在3个添加水平下的回收率在90.95%与98.67%之间。在模拟条件下,DEHP的迁移风险较高,浸泡72 h后约有0.75%溶出,而DBP和DOP的溶出风险较低。该法的灵敏度高、回收率高、选择性好,能满足实际工作的要求。

关键词: 仿真饰品, 邻苯二甲酸酯, 气相色谱-质谱法, 迁移风险, 微波萃取

Abstract: A reliable gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of 14 phthalic acid esters (PAEs) in imitation jewellery. The influences of sample pretreatment methods including microwave extraction, ultrasonic extraction, accelerated solvent extraction (ASE) and Soxhlet extraction on the determination of PAEs were investigated. The migration risk of dibutyl phthalate (DBP), bis(2-ethyl hexyl) phthalate (DEHP) and dioctyl phthalate (DOP) in plastic imitation jewellery was investigated under the simulated body temperature and sweat environment within 0 h to 168 h. The results showed that the target compounds can be effectively extracted with hexane-acetone (1:1, v/v) under microwave extraction for 35 min. The limit of quantification (LOQ) of the method was 5 mg/kg for 12 PAEs (25 mg/kg for diisononyl phthalate (DINP) and diisodecyl phthalate (DIDP)). The calibration curves were linear within 0.1~50 mg/L (0.5~250 mg/L for DINP and DIDP) with the correlation coefficients above 0.99. The recoveries ranged from 90.95% to 98.67% at three spiked levels. The migration risk of DEHP was higher than DBP and DOP with 0.75% dissolved after soaking for 72 h under the simulated conditions. The sensitivity, recovery and selectivity of the method can meet the requirements of the practical work.

Key words: imitation jewellery, microwave extraction, migration risk, phthalic acid esters (PAEs) , gas chromatography-mass spectrometry (GC-MS)

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