色谱

色谱 ›› 2015, Vol. 33 ›› Issue (3): 267-274.DOI: 10.3724/SP.J.1123.2014.11025

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定食品级聚苯乙烯和聚乙烯色母粒中33种初级芳香胺

满正印1,2, 王全林2, 李和生1, 张爱芝2, 沈坚2   

  1. 1. 宁波大学海洋学院, 浙江 宁波 315211;
    2. 宁波市产品质量监督检验研究院, 浙江 宁波 315048
  • 收稿日期:2014-11-19 修回日期:2014-12-25 出版日期:2015-03-08 发布日期:2015-02-12
  • 通讯作者: 王全林
  • 基金资助:

    浙江省质监科研计划项目(20140322);浙江省科技服务业示范项目(2013F10019).

Simultaneous determination of 33 primary aromatic amines in polystyrene and polyethylene masterbatches for foods by ultra-performance liquid chromatography- tandem mass spectrometry

MAN Zhengyin1,2, WANG Quanlin2, LI Hesheng1, ZHANG Aizhi2, SHEN Jian2   

  1. 1. School of Marine Sciences, Ningbo University, Ningbo 315211, China;
    2. Ningbo Academy of Product Quality Supervision and Inspection, Ningbo 315048, China
  • Received:2014-11-19 Revised:2014-12-25 Online:2015-03-08 Published:2015-02-12

PDF

257

被引次数

5

摘要：

建立了超高效液相色谱-三重四极杆质谱(UPLC-MS/MS)同时测定食品级聚苯乙烯(PS)和聚乙烯(PE)色母粒中33种初级芳香胺(PAAs)的检测方法。PS色母粒用二氯甲烷溶解,超声提取后加入甲醇沉淀,并将提取液过石墨化碳固相萃取柱净化;PE色母粒用二氯甲烷超声溶胀提取;将PS色母粒过柱液和PE色母粒提取液浓缩,浓缩液用甲醇-水(1:9, v/v)定容至2 mL, 0.22 μm膜过滤后上机检测。采用BEH Phenyl色谱柱(100 mm×2.1 mm, 1.7 μm),以0.07%(v/v)甲酸甲醇溶液-水(1:9, v/v)为流动相,梯度洗脱分离,UPLC-MS/MS多反应监测(MRM)模式检测,同位素内标法定量。优化了色谱分离条件、质谱碎裂电压、碰撞能量等,并考察了提取时间、提取溶剂、浓缩方式等对回收率的影响。33种PAAs的方法检出限为6~10 μg/kg,定量限为20~30 μg/kg, 2种不同基质样品在20、100、200 μg/kg等3个添加水平的平均回收率为61.3%~119.8%,相对标准偏差(RSD)为1.4%~14.8%。本方法操作简便、快速、准确、灵敏度高,能满足相关测定要求。

关键词: 超高效液相色谱-三重四极杆质谱法, 初级芳香胺, 内标法, 食品级色母粒

Abstract:

A comprehensive analytical method based on ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS) has been developed for the simultaneous determination of 33 primary aromatic amines (PAAs) in polystyrene (PS) and polyethylene (PE) masterbatches for foods. The PS masterbatches were dissolved with dichloromethane, and methanol was added to precipitate after extraction by ultrasound extraction. Then the extract was purified by passing through a carbon graphite solid phase extraction column. The PE masterbatches were swelled and extracted with dichloromethane by ultrasound. The purified PS solution and PE extract were concentrated, and diluted to 2 mL with methanol-water (1:9, v/v), and filtered through the membranes of 0.22 μm before UPLC-MS/MS analysis. The analytes were separated on a BEH Phenyl column (100 mm×2.1 mm, 1.7 μm), eluted by gradient with 0.07% (v/v) formic acid in methanol-water (1:9, v/v). The PAAs were detected by UPLC-MS/MS under multiple reaction monitoring (MRM) mode and quantified by the internal standard method. The separation conditions, fragment voltages and collision energies were optimized. The impacts of extraction times, extraction solvents and concentration methods on recoveries were studied. The limits of detection for the 33 primary aromatic amines were 6-10 μg/kg, and the limits of quantitation were 20-30 μg/kg. The mean recoveries of the two different masterbatch products at three spiked levels of 20, 100, 200 μg/kg were 61.3%-119.8%, and the relative standard deviations were 1.4%-14.8%. The experimental results indicated that the method is simple, rapid, sensitive, accurate, and can meet the related requirements for determination.

Key words: internal standard method, masterbatches for foods, primary aromatic amines (PAAs), ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS)

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