固相萃取tipLC法同时测定畜禽肉中5种雌激素的研究

Simultaneous Determination of % Kinds of Estrogens in Meat of Livestock and Poultry by Solid-phase Extraction and-Liquid Chromatography

目的研究建立固相萃取高效液相色谱法同时测定畜禽肉中5种雌激素(雌二醇、雌三醇、雌酮、炔雌醇和己烯雌酚)的快速而准确的方法。方法优化固相萃取实验条件,研究样品的提取和净化方法,以提高方法的灵敏度和精确度。固相萃取小柱为Oasis HLB 6 cc/200 mg;洗脱液为乙腈;色谱柱为Eclipse XDB--C18 5μm 4.6 mm×l50 mm柱;二极管阵列检测器,检测波长为210 nm。结果 5种雌激素分离效果好,标准曲线线性良好,相关系数r>0.999 3,方法的检出限为19.2～24.2 ng/g,有较好的准确度和精密度,回收率为79%～95%,相对标准偏差小于5%。结论该法操作简便,灵敏、准确、无杂质干扰,适合畜禽肉中激素的日常检测。

[Objective]To research and establish a rapid and sensitive Solid-phase extraction（SPE） high performance liquid chromatographic method for the determination of 5 estrogens（estradiol,estriol,estrone,ethynylestradiol,and diethylstilbestrol） in meat of livestock and poultry. [Methods]The SPE experimental conditions were optimized and the method of extraction and purification was studied to improve the sensitivity and accuracy.The SPE column was Oasis HLB 6 cc/200 mg.The elutropic liquid was acetonitrile.Chromatographic column was Eclipse XDB-C18 5 μm 4.6 mm×150 mm,Diode array detector detecting wavelength was 245 nm. [Results]Good separation was achieved in the 5 kinds of estrogens and the standard curve showing a direct ratio between the concentration and the peak area were obtained,correlation coefficient r0.999 3.Detection limits were in the range of 19.2~24.2 ng/g.The method precision and accuracy were satisfactory with recovery percentages ranging from 79% to 95% and relative standard deviations lower than 5%. [Conclusion]The method is proved to be satisfactory in precision,accuracy and sensitivity and adapt to the daily detection of livestock and poultry meat hormone.