固相萃取-高效液相色谱法同时测定饲料中的3种雌激素

Simultaneous Determination of Three Estrogens in Feed by Solid Phase Extraction-High Performance Liquid Chromatography

【目的】建立饲料中3种雌激素（17β-雌二醇、苯甲酸雌二醇和戊酸雌二醇）的固相萃取-高效液相色谱（SPE-HPLC）测定方法。【方法】饲料样品经甲醇＋水提取，固相萃取柱净化，采用Dionex C18色谱柱，以乙腈和水为流动相进行梯度洗脱，流速1.0 mL/min，检测波长230 nm，柱温30℃。【结果】3种雌激素的线性关系较好；检出限为0.5～1.0 mg/kg；平均回收率为89.3％～108.0％。【结论】SPE-HPLC法操作简便、线性范围宽、检出限低、准确度高，可同时测定饲料中3种雌激素的含量。

Obj ective Solid phase extraction-high performance liquid chromatography （SPE-HPLC）method was established to determine three estrogens （17β-estradiol,estradiol benzoate, estradiol valerate）in feed simultaneously.[Method]Three estrogens were extracted by metha-nol/water,cleaned by SPE,and finally determined by high performance liquid chromatography （HPLC）which was performed on a Dionex C18 column with a mobile phase gradient elution （ace-tonitrile and water as mobile phases）.The flow rate was 1. 0 mL/min,the detection wavelength was 230 nm,and the column temperature was 30 ℃.[Results]The results revealed good linear responses of three estrogens,limit of detections were 0. 5-1. 0 mg/kg,and the average recovery ratio were 89. 3%-108. 0%.[Conclusion]The method can simultaneously determine three estro-gens （17β-estradiol,estradiol benzoate,estradiol valerate）in feed with wide linear range,low de-tection limit and high accuracy.