Chinese Journal of Chromatography ›› 2016, Vol. 34 ›› Issue (9): 868-879.DOI: 10.3724/SP.J.1123.2016.05008

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Determination of 31 phthalate esters in baked foods and plastic packaging materials by high performance chromatography-tandem mass spectrometry

BO Yanna1,2,3, LI Rong3, ZHANG Pengjie3, LIN Qinbao1, ZHANG Xianchen3, CHEN Lisi3, HU Yiguang3, HUANG Zhiqiang2   

  1. 1. Key Laboratory of Product Packaging and Logistics of Guangdong Higher Education Institutes, Institute of Packaging Engineering, Jinan University, Zhuhai 519070, China;
    2. Hunan Academy of Inspection and Quarantine, Hunan Key Laboratory of Food Safety Science & Technology, Changsha 410004, China;
    3. Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528400, China
  • Received:2016-05-11 Online:2016-09-08 Published:2016-08-26
  • Supported by:

    National Key Technology R&D Program (No. 2012BAK08B01); Science and Technology Planning Project of Guangdong Province of China (No. 2014A040401011); Science and Technology Planning Project of AQSIQ of China (No. 2015IK260); Social Public Welfare Major Project of Zhongshan City (No. 2015B2295).

Abstract:

A high performance liquid chromatography-tandem mass spectrometric method for the analysis of 31 phthalate acid esters (PAEs) in baked foods and plastic packaging materials was developed. The food samples were extracted with ethyl acetate. Then, the extracts were frozen at -18℃, cleaned up at low temperature and high speed centrifuge before analyzed by HPLC-MS/MS. While for plastic packaging materials, after cut into small pieces, mixed solvent of methyl alcohol-acetone-n-hexane (1:1:1, v/v/v) was applied to ultra-sonic extraction of the target PAEs. The separation was performed on an MGⅢC18 capillary column (2.0 mm×100 mm, 5 μm), and determined by MS/MS in selected reaction monitoring (SRM) mode. The results indicated that the method had good linear relationships with r2 not less than 0.9958. The average recoveries (n=6) of the 31 PAEs were in the range of 80.1%-113.0% except for bis-dodecyl ester (DLP), whose average recoveries were 70.9%-109.7%, and the relative standard deviations were in the range of 1.0%-13.7%. The limits of detection (LODs) were 0.02-8.15 μg/kg, and the limits of quantification (LOQs) were 0.07-27.17 μg/kg. The method was successfully applied to determine the 31 PAEs in four kinds of baked foods (bread, biscuits, pastry and filling) and their plastic packaging. The method is suitable for the determination of the 31 PAEs in baked foods and packaging with easy operation, high accuracy and precision.

Key words: baked foods, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), phthalate acid esters (PAEs), plastic packaging

CLC Number: