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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 OasisHLB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 liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of 5 estrogenic residues of diethylstilbestrol, estrone, 17α-estradiol, 17β-estradiol and estriol in whole blood of eel. Methods: After the sample was extracted with 0.1% formic acid and extracted with methanol, the column was purified on a Waters Oasis HLB cartridge and eluted with a gradient of 0.08% aqueous ammonia / 0.08% aqueous ammonia on a XBridge C18 (150 mm × 2.1 mm, 5 μm) column Detachment was performed using electrospray ionization (ESI) ionization negative ion multiple reaction monitoring mode (MRM). Results: The calibration curves of all the analytes showed good linearity in the range of 0.1μg / L ~ 50.0μg / L with the correlation coefficient> 0.999, the recoveries ranged from 85.4% to 113.0%, and the relative standard deviations (RSDs) ranged from 2.0% to 6.8% Between the minimum detection limit of 0.1μg / L ~ 0.3μg / L range. Conclusion: The established method is simple, less interference and strong specificity, suitable for the detection of trace estrogen residues in the whole blood of eel.