液相色谱-串联质谱联用法测定黄鳝血中5种雌激素残留研究

Simultaneous determination of five estrogens in eel blood by liquid chromatography-tandem mass spectrometry

目的:建立黄鳝全血中己烯雌酚、雌酮、17а-雌二醇、17β-雌二醇和雌三醇等5种雌激素残留的液相色谱-串联质谱检测方法。方法:样品经0.1%甲酸酸化甲醇提取后,用Waters OasisHLB小柱进行净化,在XBridgeTM C18(150 mm×2.1 mm,5μm)色谱柱上,用0.08%氨水/0.08%氨水乙腈进行梯度洗脱分离,采用电喷雾(ESI)电离负离子多反应监测模式(MRM)测定。结果:各待测物在0.1μg/L～50.0μg/L范围内具有良好的线性,相关系数>0.999,回收率在85.4%～113.0%范围,相对标准偏差(RSDs)在2.0%～6.8%之间,最低定量检出限在0.1μg/L～0.3μg/L范围。结论:建立的方法简便、干扰少、特异性强,适合于黄鳝全血中痕量雌激素残留的检测。

Objective：To establish a method for the simultaneous determination of five estrogens residues,such as diethystilbestrol,estrone,17-alpha-estradiol,17-beta-estradiol and estriol in eel blood by liquid chromatography coupled with tandem mass spectrometry（HPLC-MS/MS）.Methods： The blood was extracted by methanol acidified with 0.1% formic acid,cleaned and enriched by a Waters Oasis HLB solid-phase extraction（SPE） cartridge,the separation was performed on a XBridgeTM C18（150 mm×2.1 mm,5 μm） column by the mobile phase of acetonitrile and water both containing 0.08% ammonia（V/V） as a gradient eluent.Detection was carried out by HPLC-MS/MS using a negative electrospray ionization interface in the multi-reaction monitoring（MRM） mode.Results： Calibration curves were linear within the range of 0.1 μg/L～50.0 μg/L with the correlation coefficients more than 0.999,and the limits of quantification（LOQs）were between 0.1 μg/L～0.3 μg/L.The extraction recoveries were between 85.4%～113.0%,and the RSDs were between 2.0%～6.8%.Conclusion： The developed method is simple,accurate and high specific for the satisfactory determination of trace estrogens residues in eel blood.