色谱

色谱 ›› 2012, Vol. 30 ›› Issue (10): 1017-1020.DOI: 10.3724/SP.J.1123.2012.08015

• 专栏 • 上一篇    下一篇

衍生化气相色谱-质谱法测定玩具和食品接触材料中双酚A

高永刚1*, 张艳艳2, 高建国1, 张慧玲1, 郑丽莎1, 陈静1   

  1. 1. 山东出入境检验检疫局技术中心, 山东 青岛 266003; 2. 青岛市产品质量检验技术研究所, 山东 青岛 266022
  • 收稿日期:2012-08-14 修回日期:2012-08-29 出版日期:2012-10-28 发布日期:2012-10-17
  • 通讯作者: 高永刚,硕士,工程师,主要从事消费品安全检测技术研究. Tel: (0532)80885759, E-mail: 147059027@qq.com.
  • 基金资助:

    山东省自然科学基金项目(ZR2010EM025).

Determination of bisphenol A from toys and food contact materials by derivatization and gas chromatography-mass spectrometry

GAO Yonggang1*, ZHANG Yanyan2, GAO Jianguo1, ZHANG Huiling1, ZHENG Lisha1, CHEN Jing1   

  1. 1. Shandong Exit-Entry Inspection ＆ Quarantine Bureau, Qingdao 266003, China; 2. Qingdao Testing Research Institute of Product Quality, Qingdao 266022, China
  • Received:2012-08-14 Revised:2012-08-29 Online:2012-10-28 Published:2012-10-17

PDF

593

被引次数

29

摘要： 建立了玩具和与食品接触的材料中双酚A的衍生化气相色谱-质谱(GC-MS)检测方法。通过索氏萃取富集样品中的双酚A,与乙酸酐反应,终产物用GC-MS进行测定。优化了衍生化时间、衍生化试剂用量等衍生化条件。在最佳条件下,双酚A衍生物稳定且峰形良好,在0.05～50 mg/L范围内,相关系数(r2)在0.999以上。在0.05、1.00、10.00 mg/kg 3个添加水平下,双酚A的加标回收率为80%～93%,相对标准偏差(RSD)均小于3.7%;检出限(以信噪比(S/N)=3计)为10 μg/kg。该方法精密度好、回收率高,可用于玩具和食品接触材料中双酚A的定量检测。

关键词: 气相色谱-质谱法, 食品接触材料, 双酚A, 玩具, 乙酸酐, 柱前衍生化

Abstract: A method was developed for the determination of bisphenol A (BPA) in toys and food contact materials. The BPA was extracted with Soxhlet extraction method from the sample and reacted with acetic anhydride. The final product was determined by gas chromatography-mass spectrometry (GC-MS). To achieve the optimum derivatization performance, the derivatization time and dosage of derivatization reagent etc. were investigated. Under the optimized experimental conditions, the final product was stable and the peak shape was good. The linearity of the derivative was good in the range of 0.05 to 50 mg/L with the correlation coefficient (r2) above 0.999. The recoveries ranged from 80% to 93% at the spiked levels of 0.05, 1.00, 10.00 mg/kg with the relative standard deviations (RSDs) less than 3.7%. The limit of detection (S/N=3) was 10 μg/kg. The method is accurate and has high recovery. The method is suitable for the inspection of bisphenol A in toys and food contact materials.

Key words: acetic anhydride, bisphenol A, food contact materials, gas chromatography-mass spectrometry (GC-MS), toys, pre-column derivatization