高效液相色谱-串联质谱法测定肉类食品和饲料中雌二醇和雌三醇  

DETERMINATION OF ESTRADIOL AND ESTRIOL IN FOODS AND FEEDS BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY -TANDEM MASS SPECTROMETRY

作　　者：尹江伟[1] 刘红河[2] 刘祖强[1] 肖惠贞[1] 

机构地区：[1]深圳市宝安区疾病预防控制中心,深圳518101 [2]深圳市疾病预防控制中心

出　　处：《现代预防医学》2010年第10期1928-1930,1933,共4页Modern Preventive Medicine

基　　金：深圳市科技计划项目(200602172);深圳市宝安区科技计划立项项目(2006005)

摘　　要：[目的]建立液相色谱-串联质谱联用同时测定饲料和肉类食品中雌二醇和雌三醇的方法,调查这几种雌激素在肉类食品和饲料中的污染情况。[方法]样品加乙酸缓冲溶液均质,加酶溶液酶解后。再加甲醇超声提取。用叔丁基甲醚液-液萃取2次,萃取液浓缩后,以乙腈-水为流动相,经C18柱分离后进行LC/MS/MS分析,采用负离子扫描,离子源为ESI(-),定量检测方式为多反应监测(MRM)方式,利用保留时间和碎片信号比值判断定性结果。并用建立的方法分析实际样品。[结果]3种雌激素线性相关系数r﹥0.998,相对标准偏差在1.1%～5.8%之间,高、中、低不同水平的加标回收率在80.9%～113.3%之间。[结论]该方法简便快速,精密度较高,可应用于肉和饲料中雌二醇和雌三醇的同时测定。调查结果显示,食品中雌二醇、雌三醇均有检出。[Objective] To establish a method for determination of estradiol and estriol simultaneously, and to study the pollution in foods and feeds. [Methods] Samples were homogenized in acetate buffer, and then extracted with methanol ultrasonically, finally extracted with tert-butyl methyl ether, dried up with nitrogen gas, and redissolved with acetonitrile-water. The samples were liquid-liquid extracted by tert-butyl methyl ether for two times, and the extraction liquid concentrated and the acetonitrile-water was used as flow motion, and was performed by LC/MS/MS analysis after separating by C18 columns. Then the samples were scanned by negative ion. and ion source was ESI （-）. The quantitative detection way was multi-reaction monitoring way. The qualitative results were determined by retained time and fragment signal. The samples were analyzed by established method. [ Results ] The correlation coefficients were above 0.998, the relative standard deviation （RSD） were ranged from 1.1% to 5.8% and the recoveries of high, moderate and low levels were at the range of 80.9 and 113.3%. [Conclusion] The method was simple, effective, and accurate. It can be applied to the determination of estradiol and estriol in foods and feeds.

关 键 词：雌二醇 雌三醇 高效液相色谱-串联质谱 食品分析 

分 类 号：R155.55[医药卫生—营养与食品卫生学]