柱前衍生,LC-MS/MS同时测定血浆中的孕二烯酮、依托孕烯和炔雌醇

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建立LC-MS/MS同时测定血浆中孕二烯酮、依托孕烯和炔雌醇的方法。血浆样品经液-液萃取、柱前衍生处理后,采用ESI离子源,多反应离子监测(MRM),正离子扫描进行测定。以炔诺孕酮为内标,采用C18(100mm×2.1mm,5μm)柱,梯度流动相,梯度流速测定血浆中孕二烯酮、依托孕烯和炔雌醇。结果表明,孕二烯酮、依托孕烯分别在0.1~20ng·mL-1、炔雌醇在0.01~2ng·mL-1时线性关系良好,精密度小于10.0%、方法回收率在93.6%~110.9%。对复方孕二烯酮和复方依托孕烯透皮给药制剂进行了家兔的药动学研究。本方法灵敏度高(孕二烯酮、依托孕烯达到100pg·mL-1,炔雌醇达到10pg·mL-1)、重现性好,适合药动学研究。 To establish a simultaneous LC-MS / MS method for the determination of gestodene, etoposide and ethinyl estradiol in plasma. Plasma samples were subjected to liquid-liquid extraction and precolumn derivatization. ESI-MS, MRM and positive-ion scanning were used to determine plasma samples. Taking norgestrel as internal standard, gestodene, etoposide and ethinylestradiol were measured in plasma using C18 (100mm × 2.1mm, 5μm) column, gradient mobile phase and gradient flow rate. The results showed that gestodene and epostrenol at 0.1 ~ 20ng · mL-1, ethinyl estradiol at 0.01 ~ 2ng · mL-1 linearity was good, the precision was less than 10.0%, the recovery rate was 93.6% 110.9%. Rabbits pharmacokinetics studies were carried out on the compound gestrinone and the compound transdermal delivery formulation of gesthenone. The method has high sensitivity (gestodene, 100 mg · mL-1 for gestodene, and 10 pg · mL-1 for ethinylestradiol), and has good reproducibility and is suitable for pharmacokinetic studies.
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