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建立高效液相配备二极管阵列检测器同时测定虾中雌三醇、雌二醇、己烯雌酚、雌酮、尼尔雌醇、苯甲酸雌二醇、戊酸雌二醇和炔雌醇,8种雌激素的鉴别及含量测定方法。水产品经甲醇超声提取,0.45μm滤膜过滤,经高效液相色谱分析。试验证明,8种雌激素得到很好的分离,并得到质量浓度与峰面积呈正比的线性关系(雌二醇、雌三醇、炔雌醇、雌酮、己烯雌酚、苯甲酸雌二醇、尼尔雌醇线性范围为0.16~9.00μg/mL,戊酸雌二醇线性范围为0.32~18.00μg/mL),相关系数R~2>0.999;重复性(N=6)相对标准偏差均在5%以内;定量限:雌三醇为0.15μg/mL、雌二醇为0.09μg/mL、己烯雌酚为0.09μg/mL、雌酮为0.15μg/mL、尼尔雌醇为0.09μg/mL、苯甲酸雌二醇为0.12μg/mL、戊酸雌二醇为0.15μg/mL、炔雌醇为0.15μg/mL;加标回收率均在80%~120%之间。证明该方法用于检测虾中的雌激素具有快速、简便、灵敏、准确且样品处理简单等优点。
A high-performance liquid-phase diode array detector was developed for the simultaneous determination of estriol, estradiol, diethylstilbestrol, estrone, nylestriol, estradiol benzoate, estradiol valerate and ethinylestradiol in shrimp, 8 estrogens Identification and determination of content. Aquatic products by ultrasonic extraction of methanol, 0.45μm membrane filtration, high performance liquid chromatography analysis. The test proves that the eight estrogens are well separated and the linear relationship between mass concentration and peak area is obtained (estradiol, estriol, ethinyl estradiol, estrone, diethylstilbestrol, estradiol benzoate, The linear range of estradiol was 0.16-9.00μg / mL, and the linear range of estradiol valerate was 0.32-18.00μg / mL), the correlation coefficient was R ~ 2> 0.999. The relative standard deviation of repeatability (N = 6) %; The limit of quantification: estriol 0.15μg / mL, estradiol 0.09μg / mL, diethylstilbestrol 0.09μg / mL, estrone 0.15μg / mL, nilestriol 0.09μg / mL, benzene Estradiol formate was 0.12μg / mL, estradiol valerate was 0.15μg / mL, ethinyl estradiol was 0.15μg / mL, and the recoveries were both between 80% and 120%. This method is proved to be rapid, simple, sensitive, accurate and simple in sample processing for the detection of estrogen in shrimp.