色谱

色谱 ›› 2014, Vol. 32 ›› Issue (11): 1209-1213.DOI: 10.3724/SP.J.1123.2014.07039

• 研究论文 • 上一篇    下一篇

固相萃取-超高效液相色谱-串联质谱法同时测定饲料中的3种雌激素

肖全伟1, 吴文林1, 杨万林2, 梁润1, 李绍波1, 刘玲利3   

  1. 1. 成都市产品质量监督检验院食品中心, 四川 成都 610100;
    2. 中国空军第34师西郊场站医院, 北京 100195;
    3. 成都理工大学材料与化学化工学院, 四川 成都 610059
  • 收稿日期:2014-07-23 出版日期:2014-11-08 发布日期:2014-10-31
  • 通讯作者: 肖全伟,E-mail:xqw66666@163.com.
  • 基金资助:

    四川省科技基础条件平台建设专项;成都市科技计划项目(12RKYB174ZF-001).

Simultaneous determination of three estrogens in feed by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

XIAO Quanwei1, WU Wenlin1, YANG Wanlin2, LIANG Run1, LI Shaobo1, LIU Lingli3   

  1. 1. Testing Center of Food, Chengdu Product Quality Supervision and Inspection Institute, Chengdu 610100, China;
    2. Xijiao Hospital, Chinese Air Force 34th Transport Division, Beijing 100195, China;
    3. College of Material and Chemistry & Chemical Engineering, Chengdu University of Technology, Chengdu 610059, China
  • Received:2014-07-23 Online:2014-11-08 Published:2014-10-31

PDF

119

被引次数

17

摘要：

建立了固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)同时测定饲料(预混合、配合和浓缩饲料)中3种雌激素(17β-雌二醇、苯甲酸雌二醇和戊酸雌二醇)的检测方法。饲料样品经乙腈提取,Heaion C18固相萃取柱净化后,用ACQUITY UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7 μm)分离,乙腈和0.1%氨水溶液作为流动相进行梯度洗脱,多反应监测(MRM)模式检测,内标法定量。结果表明,17β-雌二醇和戊酸雌二醇在10~200 μg/L、苯甲酸雌二醇在5~200 μg/L范围内具有良好线性,相关系数(r)≥0.996。17β-雌二醇、苯甲酸雌二醇和戊酸雌二醇的检出限分别为7、5和7 μg/kg。样品的平均加标回收率为96.5%~102.0%。该法前处理操作简便、分析速度快、检出限低、准确度高,可用于饲料中3种雌激素的同时检测。

关键词: 17β-雌二醇, 苯甲酸雌二醇, 超高效液相色谱-串联质谱, 固相萃取, 饲料, 戊酸雌二醇

Abstract:

A method was developed for the simultaneous determination of three estrogens (17β-estradiol, estradiol benzoate, estradiol valerate) in feed by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). After the sample was extracted by acetonitrile and cleaned-up on a Heaion C18 solid phase extraction (SPE) column, the three estrogens were separated by an ACQUITY UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) with gradient elution using acetonitrile and 0.1% ammonia solution as mobile phases and finally confirmed and quantified in multiple reaction monitoring (MRM) mode. The internal standard calibration curves were used for the quantification. The results showed that all the estrogens were determined with excellent linear relationships from 10 μg/L to 200 μg/L for 17β-estradiol and estradiol valerate, and from 5 μg/L to 200 μg/L for estradiol benzoate. The correlation coefficients (r) of the three estrogens were not lower than 0.996. The limits of detection for 17β-estradiol, estradiol benzoate and estradiol valerate were 7 μg/kg, 5 μg/kg and 7 μg/kg, respectively. The average recoveries were 96.5%-102.0%. The results demonstrated that the developed method can simultaneously determine the three estrogens in feed with advantages of simple pretreatment, rapid analysis, low limit of detection and high accuracy.

Key words: 17β-estradiol, estradiol benzoate, estradiol valerate, feed, solid phase extraction (SPE), ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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