色谱

色谱

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超高效液相色谱串联质谱法测定鱼组织中6种抗雌激素药物

肖甚圣1, 杨奕2, 张晶2, 吴永宁1,3*, 邵兵2   

  1. 1. 武汉工业学院食品科学与工程学院, 湖北 武汉 430023; 2. 北京市疾病预防控制中心, 食物中毒诊断溯源技术北京市重点实验室, 北京 100013; 3. 中国疾病预防控制中心营养与食品安全所, 北京 100025
  • 收稿日期:2011-06-20 修回日期:2011-08-03 出版日期:2011-11-28 发布日期:2011-12-25
  • 通讯作者: 吴永宁,研究员,博士生导师,研究方向为化学污染监测
  • 基金资助:

    国家自然科学基金重点项目(No. 20837003)和北京市卫生系统高层次卫生技术人才培养计划项目.

Determination of 6 antiestrogens in fish tissues by ultra performance liquid chromatography-tandem mass spectrometry

XIAO Shensheng1, YANG Yi2, ZHANG Jing2, WU Yongning1,3*, SHAO Bing2   

  1. 1. College of Food Science and Engineering, Wuhan Polytechnic University, Wuhan 430023, China; 2. Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Prevention and Control, Beijing 100013, China; 3. Institute of Nutrition and Food Safety, Chinese Center for Disease Prevention and Control, Beijing 100025, China
  • Received:2011-06-20 Revised:2011-08-03 Online:2011-11-28 Published:2011-12-25

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摘要： 采用超高效液相色谱-串联质谱(UPLC-MS/MS)在多反应监测(MRM)模式下建立了鱼肉、鱼肝中6种抗雌激素类药物(托瑞米芬、氯米芬、他莫昔芬、雷洛昔芬、阿那曲唑、来曲唑)的检测方法。样品采用乙腈超声提取,上清液中加入适量水稀释提取液,经混合型阳离子交换(MCX)固相萃取柱富集、净化后进行UPLC-MS/MS分析。UPLC分离在ACQUITY UPLCTM BEH C18柱(100 mm×2.1 mm, 1.7 μm)上进行,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱。6种抗雌激素药物的定量限(以信噪比为10计)为0.1～0.3 μg/kg; 4个加标水平的平均回收率为84.9%～112.2%,相对标准偏差为0.9%～14.3%。该方法可用于鱼肉、鱼肝中6种抗雌激素药物的痕量分析。

关键词: 超高效液相色谱-串联质谱, 固相萃取, 抗雌激素药物, 鱼肝, 鱼肉

Abstract: A comprehensive analytical method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed for the simultaneous determination of 6 antiestrogens (toremifene, clomiphene, tamoxifen, raloxifene, anastrozole and letrozole) in fish muscle and liver. The multi-reaction monitoring mode was employed for the determination. The homogeneous fish tissue samples were ultrasonically extracted with acetonitrile, and then the supernatants were diluted by water. The target compounds were concentrated and purified by a mixed-mode cationic-exchanger (MCX) cartridge, and then separated on an ACQUITY UPLCTM BEH C18 column (100 mm×2.1 mm, 1.7 μm) using a binary mobile phase gradient with water containing 0.1% formic acid and acetonitrile. The limits of quantification (LOQ, S/N=10) of the 6 antiestrogens were 0.1~0.3 μg/kg in muscle and liver samples. The average recoveries of target compounds (spiked at four concentration levels) based on internal standard calibration were in the range of 84.9%~112.2% with the relative standard deviations of 0.9%~14.3%. This method can be applied to the trace analysis of target drugs in fish muscle and liver samples.

Key words: antiestrogens, fish liver, fish muscle, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), solid phase extraction (SPE)