色谱

色谱 ›› 2013, Vol. 31 ›› Issue (1): 38-45.DOI: 10.3724/SP.J.1123.2012.10028

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法快速测定水基食品模拟物中28种受限芳香族伯胺的迁移量

肖晓峰, 王建玲*, 杨娟娟, 刘艇飞, 陈彤, 何军, 邓弘毅, 高启燕   

  1. 台州出入境检验检疫局, 浙江 台州 318000
  • 收稿日期:2012-10-31 修回日期:2012-11-30 出版日期:2013-01-28 发布日期:2013-01-21
  • 通讯作者: 王建玲
  • 基金资助:

    国家质检总局科技计划项目(2005IK173).

Rapid analysis of 28 primary aromatic amines in aqueous food simulants by high performance liquid chromatography-tandem mass spectrometry

XIAO Xiaofeng, WANG Jianling*, YANG Juanjuan, LIU Tingfei, CHEN Tong, HE Jun, DENG Hongyi, GAO Qiyan   

  1. Taizhou Entry-Exit Inspection and Quarantine Bureau, Taizhou 318000, China
  • Received:2012-10-31 Revised:2012-11-30 Online:2013-01-28 Published:2013-01-21
  • Contact: WANG JIANLING

PDF

265

被引次数

5

摘要： 建立了高效液相色谱-串联质谱(HPLC-MS/MS)联用方法用于快速测定水基食品模拟物(10%乙醇、30 g/L乙酸和20%乙醇)中28种芳香族伯胺的迁移量。用水基食品模拟物浸泡待测样品中一定时间(在100 ℃条件下)后,冷却至室温并混匀,所得浸泡液经亲水性聚四氟乙烯针头式过滤器过滤后,直接进行HPLC-MS/MS测定。采用Agilent Zorbax SB-Phenyl柱,以水和0.1%甲酸-25%乙腈-甲醇溶液为流动相进行梯度洗脱分离;质谱具电喷雾离子源,在正离子和分段式多反应监测(MRM)模式下检测。结果表明,方法定量限为0.002～10 μg/L,在5～100 μg/L或10～100 μg/L范围内线性关系良好(r2＞0.995);在10、20、40 μg/L水平的加标回收率为76.6%～114%,相对标准偏差为1.53%～8.97%。该方法样品前处理简单快速,色谱分离效果和线性关系好,检出限较低、回收率和准确度高,且完全满足欧盟(EU)No 10/2011法规中对芳香族伯胺特定迁移量的限量要求。该方法已成功应用于30批次出口欧盟的食品接触材料相关制品中芳香族伯胺特定迁移量的检测。

关键词: 芳香族伯胺, 迁移量, 食品接触材料, 水基食品模拟物, 液相色谱-串联质谱

Abstract: A novel method for rapid analysis of the migration amounts of 28 primary aromatic amines (PAAs) in aqueous food simulants (10% ethanol, 30 g/L acetic acid and 20% ethanol aqueous solution) was developed using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). After the migration test, the soaking solution was cooled down from 100 ℃, vortexed, filtered through a hydrophilic polytetrafluoroethylene filter with a disposable syringe, and then the filtrate was analyzed by HPLC-MS/MS. A Zorbax SB-Phenyl column (250 mm×4.6 mm, 5 μm) was selected for chromatography. The mobile phase consisted of water and 0.1% formic acid-25% acetonitrile-methanol solution with gradient elution. The 28 PAAs in aqueous food simulants were detected by tandem mass spectrometer operated in positive electrospray ionization (ESI+)and multiple reaction monitoring (MRM) mode. The limits of quantification for the 28 PAAs were between 0.002 μg/L and 10 μg/L. The linearity of the method was good with correlation coefficients (r2) greater than 0.995 over the concentration range from 5 μg/L or 10 μg/L to 100 μg/L. The average recoveries of the 28 PAAs were between 76.6% and 114% with the relative standard deviations between 1.53% and 8.97% at the levels of 10, 20, and 40 μg/L. The method shows rapid pretreatment, the lower limits of quantification, good recoveries and accuracies, and meets the requirement of European Union (EU)No 10/2011 regulation for the specific migration of PAAs. The method has been applied to analyze the 28 PAAs in different aqueous food simulants from the migration test of 30 batches of food contact material samples exported to EU.

Key words: aqueous food simulants, food contact material, migration amount, primary aromatic amines, liquid chromatography-tandem mass spectrometry (LC-MS/MS)

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