色谱

色谱 ›› 2013, Vol. 31 ›› Issue (9): 908-913.DOI: 10.3724/SP.J.1123.2013.02033

• 技术与应用 • 上一篇    下一篇

高效液相色谱-串联质谱法测定饲料和卧床土中的环境雌激素

李雪1,2, 牟光庆1, 陈历俊1,2, 姜铁民2   

  1. 1. 大连工业大学食品学院, 辽宁 大连 116034;
    2. 北京三元食品股份有限公司, 北京 100076
  • 收稿日期:2013-02-27 修回日期:2013-04-24 出版日期:2013-09-28 发布日期:2013-09-02
  • 通讯作者: 陈历俊
  • 基金资助:

    国家"863"计划项目(2011AA100903);奶牛产业技术体系北京市创新团队建设项目.

Determination of environmental estrogens in cow feed and soil by high performance liquid chromatography-tandem mass spectrometry

LI Xue1,2, MU Guangqing1, CHEN Lijun1,2, JIANG Tiemin2   

  1. 1. College of Food Science and Technology, Dalian Polytechnic University, Dalian 116034, China;
    2. Beijing Sanyuan Foods Co., Ltd., Beijing 100076, China
  • Received:2013-02-27 Revised:2013-04-24 Online:2013-09-28 Published:2013-09-02

PDF

233

被引次数

14

摘要：

建立了饲料和卧床土中雌三醇、雌二醇、雌酮、双酚A和己烯雌酚5种环境雌激素的固相萃取结合高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。对色谱流动相、质谱条件、固相萃取柱等影响因素进行了优化,得到的最优化条件为:样品经乙腈提取后,用固相萃取柱(NH2-SPE)进行富集,采用Acquity UPLCTM HSS T3色谱柱分离,以乙腈-甲醇(4:1, v/v)与0.01%氨水为流动相,采用梯度洗脱,在负离子模式下进行MS/MS测定。在该优化条件下,5种环境雌激素的检出限(以信噪比为3计)为0.06~0.22 μg/kg,回收率为81.70%~102.20%,相对标准偏差小于10.00%。该方法用于饲料和卧床土中的5种环境雌激素残留量的测定具有简便、快速、灵敏的特点。

关键词: 高效液相色谱-串联质谱, 环境雌激素, 饲料, 卧床土

Abstract:

An analytical method was developed for the determination of the residues of five environmental estrogens, including estriol, estradiol, estrone, bisphenol A and diethylstilbestrol, in the cow feed and soil by solid phase extraction (SPE) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The important parameters which affect the determination efficiency such as the mobile phase, the condition of mass spectrometry and solid phase extraction column were optimized. The optimal determination conditions were as follows: the sample was extracted with acetonitrile at first, then cleaned-up with an NH2-SPE column, and an Acquity UPLCTM HSS T3 column was selected to separate the analytes. Acetonitrile-methanol (4:1, v/v) and 0.01% ammonia aqueous solution were used as the mobile phase by gradient elution in the negative mode. The limits of detection (LOD, S/N=3) were 0.06-0.22 μg/kg. The overall recoveries varied from 81.70% to 102.20%, and the relative standard deviations (RSDs) were all less than 10.00%. This method is simple, sensitive and accurate, and suitable for the determination of environmental estrogens in cow feed and soil.

Key words: cow feed, environmental estrogens, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), soil

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