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建立高效液相测定水产品中15种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,15种雌激素得到很好的分离,并得到浓度与峰面积呈正比的线性关系,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0.75μg/g、雌二醇0.45μg/g、炔雌醇0.45μg/g、雌酮0.45μg/g、炔诺酮0.60μg/g、己烯雌酚0.45μg/g、炔诺孕酮0.75μg/g、醋酸氯地孕酮0.75μg/g、醋酸甲地孕酮0.75μg/g、醋酸甲羟孕酮0.45μg/g、黄体酮0.45μg/g、苯甲酸雌二醇0.60μg/g、戊酸雌二醇0.75μg/g、已酸羟孕酮0.60μg/g、庚酸炔诺酮0.75μg/g;加标回收率均在80%~120%之间。证明该方法用于检测水产品中的激素具有快速、简便、灵敏、准确且样品处理简单等优点。
Establishment of high performance liquid chromatography determination of aquatic products in 15 kinds of hormones and determination of content. Aquatic products by ultrasonic extraction of methanol, 0.45μm membrane filtration, high performance liquid chromatography analysis. The results showed that the 15 estrogens were well separated and the linear relationship between concentration and peak area was obtained. The correlation coefficient R ~ 2> 0.999; the relative standard deviation of repeatability (N = 6) were within 5% Limit: estriol 0.75μg / g, estradiol 0.45μg / g, ethinyl estradiol 0.45μg / g, estrone 0.45μg / g, norethisterone 0.60μg / g, diethylstilbestrol 0.45μg / g, Ketone 0.75 μg / g, chlormadinone 0.75 μg / g, megestrol acetate 0.75 μg / g, medroxyprogesterone acetate 0.45 μg / g, progesterone 0.45 μg / g, estradiol benzoate 0.60 μg / g, estradiol valerate 0.75μg / g, oxycodone 0.60μg / g, norethisterone 0.75μg / g; recoveries were 80% to 120%. It is proved that the method is rapid, simple, sensitive, accurate and simple in sample processing for the detection of hormones in aquatic products.