色谱 ›› 2016, Vol. 34 ›› Issue (7): 673-680.DOI: 10.3724/SP.J.1123.2016.03001

• 特别策划:出入境检验检疫系统专栏(2016) • 上一篇    下一篇

前吸附技术-超高压液相色谱-串联质谱法同时测定酒中24种邻苯二甲酸酯

吴敏1, 郑向华1, 张志刚1, 陈燕1, 林立毅1, 黄志强2   

  1. 1. 厦门出入境检验检疫局, 福建 厦门 361026;
    2. 湖南省检验检疫科学技术研究院, 湖南 长沙 410004
  • 收稿日期:2016-03-03 出版日期:2016-07-08 发布日期:2013-02-05
  • 通讯作者: 郑向华
  • 基金资助:

    "十二五"国家科技支撑计划项目(2012BAK08B01);福建省自然科学基金项目(2014J01057).

Simultaneous determination of 24 phthalates in liquors using front adsorption technology and ultra performance liquid chromatography-tandem mass spectrometry

WU Min1, ZHENG Xianghua1, ZHANG Zhigang1, CHEN Yan1, LIN Liyi1, HUANG Zhiqiang2   

  1. 1. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China;
    2. Hunan Inspection and Quarantine Technology Academy, Changsha 410004, China
  • Received:2016-03-03 Online:2016-07-08 Published:2013-02-05
  • Supported by:

    National Key Technology R&D Program during the Twelfth Five-year Plan Period (No. 2012BAK08B01);Natural Science Foundation of Fujian Province (No. 2014J01057).

摘要:

建立了前吸附技术-超高压液相色谱-串联质谱测定酒中24种邻苯二甲酸酯含量的方法。酒类样品经稀释、净化后采用前吸附技术排除仪器管路中的本底干扰,经超高压液相色谱-串联质谱仪进行测定。采用多反应监测模式、电喷雾电离源正离子(ESI+)模式进行检测,外标法定量。24种邻苯二甲酸酯在0.005~2.00 mg/L范围内线性关系良好,相关系数(r)均大于0.99,检出限(S/N=3)为0.003~0.05 mg/kg。以不含增塑剂的酒类样品作为空白样品进行加标回收率试验,各种邻苯二甲酸酯化合物的回收率为75.4%~118.2%,相对标准偏差(RSD)为4.0%~11.2%。该法不但可以有效排除管路中邻苯二甲酸酯本底的干扰,而且简单、灵敏、稳定。

关键词: 超高压液相色谱-串联质谱, 酒, 邻苯二甲酸酯, 前吸附技术

Abstract:

A method for the simultaneous determination of 24 phthalates in liquors was developed by using front adsorption technology and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were diluted and cleaned-up by an HLB solid phase extraction cartridge. The front adsorption technology was used to suppress the interferences which came from plastic pipes in the UPLC-MS/MS. And then the targets were analyzed by UPLC-MS/MS under the positive ion mode using multiple reaction monitoring (MRM) mode. The calibration curves showed a good linearity in the range of 0.005-2.00 mg/L with r>0.99. The limits of detections (S/N=3) were 0.003-0.05 mg/kg. The average recoveries of the spiked samples were between 75.4% and 118.2% with the relative standard deviations (RSDs) of 4.0%-11.2%. The method could be used to simultaneously confirm the multi-residue of the 24 phthalates in liquors. And the method is simple, sensitive and stable.

Key words: front adsorbing technology, liquors, phthalates, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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