基于DSPE-LC-MS/MS法的畜禽产品中雌激素的测定

Detection of estrogens in animal products by DSPE- LC- MS / MS

摘要: 本研究建立了畜禽产品中雌酮（estrone,E1）、雌二醇（estradiol,E2）、雌三醇（estriol,E3）以及己烯雌酚（diethylstilbestrol,DES）残留量的分散固相萃取（DSPE）-液相色谱-质谱联用（LC-MS/MS）分析测定方法。样品经乙腈沉淀蛋白质,无水Mg SO4去除水分后,以N-丙基乙二胺（PSA）极性吸附剂分散固相萃取净化,最后通过液相色谱质谱联用测定。在畜禽产品中添加不同浓度的雌激素后用该方法的回收率最高可达到96.63%,4种雌激素的检出限（S/N=3）为1.32¹6.52μg/kg。该方法为畜禽产品中雌激素残留的检测提供了可靠的参考依据。

Abstract: A method was developed for determining 4 estrogens ( estrone, estradiol, estriol and diethylstilbestrol) in animal products such as egg, chicken, beef and pork by dispersive solid phase extraction ( DSPE) as clean up step and liquid chromatography- tandem quadrupole mass spectrometry ( LC- MS / MS) as detection step. Acetonitrile was added into sample to precipitate the protein and anhydrous Mg SO4 was used for the removal of residual water, and then sample was cleaned up by DSPE using primary secondary amine ( PSA) dipolar adsorbent.Estrogens were detected by LC- MS / MS. The average recovery of 4 estrogens from the samples at three spiked levels could reach 96.63%.The limit of detection ( S / N = 3) ranged from 1.32μg / kg to 16.52μg / kg.