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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 establish a rapid and accurate method for the simultaneous determination of five estrogens (estradiol, estriol, estrone, ethinylestradiol and diethylstilbestrol) in livestock and poultry meat by solid-phase extraction and high performance liquid chromatography. Methods The experimental conditions of solid phase extraction (SPE) were optimized and the methods of extraction and purification of samples were studied to improve the sensitivity and accuracy of the method. The solid phase extraction cartridge was Oasis HLB 6 cc / 200 mg; the eluent was acetonitrile; the column was an Eclipse XDB - C18 5 μm 4.6 mm × 150 mm column; the diode array detector was used at a detection wavelength of 210 nm. Results The results showed that the five estrogens had good separation performance and the standard curve was linear with the correlation coefficient r> 0.999 3. The detection limit of the method was 19.2-24.2 ng / g with good accuracy and precision and the recovery was 79% 95%, relative standard deviation less than 5%. Conclusion The method is simple, sensitive, accurate, no impurity interference, suitable for daily testing of hormones in livestock and poultry meat.