色谱

色谱 ›› 2011, Vol. 29 ›› Issue (05): 399-403.DOI: 10.3724/SP.J.1123.2011.00399

• 研究论文 • 上一篇    下一篇

单分散磁性亚微米粒子固相萃取-液相色谱-串联质谱法测定牛奶中的双酚A

吴新华2, 丁利1, 肖家勇1, 龙妍娇3, 许宙1, 李忠海2, 王利兵1*   

  1. 1. 湖南省检验检疫科学技术研究院, 湖南出入境检验检疫局技术中心, 食品安全科学技术湖南省重点实验室, 湖南 长沙 410004; 2. 中南林业科技大学食品科学与工程学院, 湖南 长沙 410004; 3. 广东出入境检验检疫局, 广东 广州 510623
  • 收稿日期:2010-12-08 修回日期:2011-02-26 出版日期:2011-05-28 发布日期:2011-05-28
  • 通讯作者: 王利兵,博士,研究员,研究方向为食品安全与检验检疫安全. Tel: (0731)85627689,

Determination of bisphenol A in milk by liquid chromatography-tandem mass spectrometry coupled with solid phase extraction of monodisperse magnetic submicron particles as adsorbent

WU Xinhua2, DING Li1, XIAO Jiayong1, LONG Yanjiao3, XU Zhou1, LI Zhonghai2, WANG Libing1*   

  1. 1. Hunan Academy of Inspection and Quarantine, Technology Center of Hunan Entry-Exit Inspection and Quarantine Bureau, Hunan Key Laboratory of Food Safety Science & Technology, Changsha 410004, China; 2. Faculty of Food Science & Engineering, Central South University of Forestry & Technology, Changsha 410004, China; 3. Guangzhou Entry-Exit Inspection and Quarantine Bureau, Guangzhou 510623, China
  • Received:2010-12-08 Revised:2011-02-26 Online:2011-05-28 Published:2011-05-28

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827

被引次数

44

摘要： 采用溶剂热还原法制备的单分散性Fe3O4磁性亚微米粒子(Fe3O4-magnetic submicron particles)进行固相萃取(SPE),结合高效液相色谱-串联质谱(HPLC-MS/MS)测定了牛奶中的双酚A(BPA)。对溶液的pH、磁性粒子用量、洗脱溶剂和体积等影响因素进行了优化,得到的最优萃取条件为: 溶液的pH 6,磁性粒子用量3.5 mg,用0.4 mL甲醇洗脱。以Agilent XDB C18柱为分析柱,流动相为乙腈-0.25 mmol/L氨水（80:20, v/v）溶液,在负离子模式下进行MS/MS测定。双酚A在1～100 μg/L范围内线性关系良好(r=0.9993);在3个添加水平下,回收率为85.3%～96.1%,相对标准偏差小于10%;通过不断稀释加标浓度确定方法的检出限(信噪比为3)为1.0 μg/L。该方法简单、准确,能用于牛奶中双酚A的快速测定。

关键词: 单分散性磁性亚微米粒子, 高效液相色谱-串联质谱, 固相萃取, 牛奶, 双酚A

Abstract: Monodisperse magnetic submicron particles were synthesized by a solvothermal reduction method. A solid phase extraction (SPE) based on the monodisperse magnetic submicron particles and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of bisphenol A (BPA) at trace level in milk has been established. The important parameters that affect the extraction efficiency such as the solution pH, dosage of magnetic submicron particles, nature of elution solution and its volume were optimized. The optimal extraction conditions were as follows: the pH 6.0, the dosage of 3.5 mg magnetic submicron particles and 0.4 mL methanol as elution solution. BPA was analyzed by HPLC-MS/MS in negative ion mode using an Agilent XDB C18 column as analytical column. Under the optimal conditions, the calibration curves showed a good linearity in the BPA concentration range of 1.0~100.0 μg/L. The correlation coefficient was 0.9993. The average recoveries of BPA at three spiked levels ranged from 85.3% to 96.1% with the relative standard deviations (RSDs) less than 10%. The detection limit of the method was 1.0 μg/L. The method is sensitive, simple, and suitable for the rapid determination of BPA in milk.

Key words: bisphenol A (BPA), high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), milk, monodisperse magnetic submicron particles, solid-phase extraction (SPE)