色谱 ›› 2014, Vol. 32 ›› Issue (9): 988-991.DOI: 10.3724/SP.J.1123.2014.06008

• 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塑料包装矿泉水中11种双酚类化合物

勾新磊1, 高峡1,2, 胡光辉1, 池海涛1, 乐胜峰1, 王尉1, 刘伟丽1,2   

  1. 1. 北京市理化分析测试中心, 有机材料检测技术与质量评价北京市重点实验室, 北京 100089;
    2. 北京市食品安全分析测试工程技术研究中心, 北京 100089
  • 收稿日期:2014-06-05 修回日期:2014-07-15 出版日期:2014-09-08 发布日期:2014-08-30
  • 通讯作者: 高峡
  • 作者简介:高峡,gaoxia@iccas.ac.cn.
  • 基金资助:

    北京市自然科学基金项目(2122018);北京市科学技术研究院创新团队计划项目(IG200801N/C2).

Simultaneous determination of 11 bisphenols in plastic bottled drinking water by ultra performance liquid chromatography-tandem mass spectrometry

GOU Xinlei1, GAO Xia1,2, HU Guanghui1, CHI Haitao1, LE Shengfeng1, WANG Wei1, LIU Weili1,2   

  1. 1. Beijing Key Laboratory of Detection Technology and Quality Evaluation of Organic Material, Beijing Centre for Physical and Chemical Analysis, Beijing 100089, China;
    2. Beijing Engineering Research Center of Food Safety Analysis, Beijing 100089, China
  • Received:2014-06-05 Revised:2014-07-15 Online:2014-09-08 Published:2014-08-30

摘要:

建立了同时测定塑料包装矿泉水中11种双酚类化合物的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。以真空冷冻干燥的方法对样品进行前处理。使用Waters ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm)进行分离,以甲醇和0.1%(v/v)氨水为流动相对目标物进行梯度洗脱。在电喷雾负离子模式及多反应监测(MRM)模式下进行定性和定量分析。结果表明,11种双酚类化合物在线性范围内线性关系良好,线性相关系数(R2)均大于0.997;目标物的检出限为0.01~1.00 μg/L;3个加标水平下的回收率为75.3%~102.1%,相对标准偏差为1.5%~8.9%。本方法准确、简便、快速,可用于塑料包装矿泉水中双酚类化合物的实际检测。

关键词: 超高效液相色谱-串联质谱, 双酚类化合物, 塑料包装矿泉水

Abstract:

A sensitive method was developed for the simultaneous determination of 11 bisphenols in plastic bottled drinking water by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were freeze-dried under vacuum and then dissolved with methanol. The separation was performed on a UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) by using 0.1%(v/v) NH3·5H2O and methanol as mobile phases with gradient elution at a flow rate of 0.2 mL/min. The electrospray ionization (ESI) source in negative ion mode was used for the analysis of the 11 bisphenols in the multiple reaction monitoring (MRM) mode. The results verified that the standard curves for the 11 bisphenols were obtained with good correlation coefficients (R2)>0.997 in their concentration ranges. The limits of detection (LOD, S/N=3) for the 11 bisphenols were in the range of 0.01-1.00 μg/L. The mean recoveries for the 11 bisphenols at three spiked levels (low, middle, high) were 75.3%-102.1% with the relative standard deviations of 1.5%-8.9%. Seven plastic bottled drinking water samples were tested, and no bisphenol was found. The method is accurate, simple, rapid and feasible for the simultaneous determination of bisphenols in plastic bottled drinking water.

Key words: bisphenols, plastic bottled drinking water, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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