色谱

色谱 ›› 2014, Vol. 32 ›› Issue (1): 81-88.DOI: 10.3724/SP.J.1123.2013.08032

• 研究论文 • 上一篇    下一篇

固相萃取-气相色谱-串联质谱法测定乳胶儿童用品中15种N-亚硝胺及其前体物的迁移量

李丕1, 白桦1, 李海玉1, 陈明2, 吕庆1, 张庆1   

  1. 1. 中国检验检疫科学研究院, 北京 100123;
    2. 江苏出入境检验检疫局轻工产品与儿童用品检测中心, 江苏 扬州 225009
  • 收稿日期:2013-08-19 修回日期:2013-09-18 出版日期:2014-01-08 发布日期:2013-12-26
  • 通讯作者: 张庆
  • 基金资助:

    国家质检总局科研项目(2011IK114，2012104018)；国家质检总局科技支撑课题(2013BAK04B03).

Determination of migration of 15 N-nitrosamines and N-nitrosatable substances from children’s latex articles by gas chromatography-tandem mass spectrometry using solid phase extraction

LI Pi1, BAI Hua1, LI Haiyu1, CHEN Ming2, LÜ Qing1, ZHANG Qing1   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100123, China;
    2. Inspection Center of Light Industry Products and the Children's Products, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Yangzhou 225009, China
  • Received:2013-08-19 Revised:2013-09-18 Online:2014-01-08 Published:2013-12-26

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摘要：

建立了同时测定乳胶儿童用品中15种N-亚硝胺及其前体物迁移量的固相萃取-气相色谱-串联质谱(SPE-GC-MS/MS)分析方法。以人工唾液作为迁移模拟物，以Chromabond Easy固相萃取柱(填料的主要成分是极性修饰的聚乙烯-二乙烯基苯共聚物)对迁移液中的N-亚硝胺分析物进行净化，采用HP-5MS UI色谱柱分离，MS/MS在多反应监测模式下进行定性及定量分析。15种N-亚硝胺在5~2000 μg/L范围内呈良好的线性关系，相关系数均大于0.998；方法定量限(S/N=10)为0.625~12.50 μg/kg，低于欧盟2009/48/EC指令的限量要求。在低、中、高3个添加水平的回收率为53.8%~116.2%、52.7%~105.1%和49.5%~102.9%；日内精密度分别为1.3%~14.0%(n=6)，日间精密度为1.6%~7.6%(n=4)。采用本方法对婴儿奶嘴样品和气球样品进行了测定，其中4件奶嘴和7件气球样品中检出亚硝胺及其前体物，奶嘴和气球中N-亚硝胺的总检出含量分别为0.0499~0.126 mg/kg和0.515~41.2 mg/kg；N-亚硝胺前体物总检出量分别为0.0264~0.0300 mg/kg和0.187~12.5 mg/kg。

关键词: N-亚硝胺, 固相萃取, 气相色谱-串联质谱, 乳胶儿童用品

Abstract:

A method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) using solid phase extraction (SPE) has been developed for the determination of 15 N-nitrosamines from children's latex articles. Artificial saliva was used as the migration solution to extract N-nitrosamines in children's latex articles. And then a polar modified polystyrene-divinylbenzene copolymer (Chromabond Easy) was used for the selective SPE of the analytes in the migration solution. The analytes were then separated on an HP-5MS UI GC column and determined by MS/MS in multiple reaction monitoring mode for qualitative and quantitative analysis. Good linearity ranged from 5 μg/L to 2000 μg/L was observed for all the compounds (R2 >0.998) and the limits of quantification for the 15 N-nitrosamines were 0.625-12.50 μg/kg (S/N=10), which were lower than the limits required by the EU 2009/48/EC Directive. The average recoveries of the target analytes at low, medium, and high spiked levels were in the ranges of 53.8%-116.2%, 52.7%-105.1% and 49.5%-102.9%, respectively. The average within-day and between-day RSDs were from 1.3% to 14.0% (n=6) and from 1.6% to 7.6% (n=4), respectively. The proposed method was used to monitor N-nitrosamines in baby nipples and balloons, and N-nitrosamines were found in some samples. The total contents of the 15 N-nitrosamines in the analyzed nipples and balloons samples ranged from 0.0499 mg/kg to 41.2 mg/kg. And the total contents of the N-nitrosatable substances in the analyzed samples ranged from 0.0264 mg/kg to 12.5 mg/kg.

Key words: N-nitrosamines, children’s latex articles, gas chromatography-tandem mass spectrometry (GC-MS/MS), solid phase extraction (SPE)

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