HPLC-MS/MS法测定新生儿血浆中奥美拉唑的浓度

Determination of omeprazole concentration in neonates plasma by HPLC-MS/MS

目的建立一种测定新生儿血浆中奥美拉唑浓度的HPLC-MS/MS法。方法新生儿血浆样品用乙腈沉降蛋白后,以兰索拉唑为内标,色谱柱为C18(4. 6 mm×150. 0 mm,3. 5μm),流动相为乙腈-水(0. 1%甲酸)=85∶15,流速为0. 3 m L·min^(-1),柱温为35℃,进样量为10μL。用电喷雾离子化源,正离子方式,多反应监测(MRM)扫描方式进行监测。考察该方法的专属性、标准曲线与定量下限、精密度与回收率,以及稳定性。结果血浆中奥美拉唑的浓度在5～4000 ng·m L^(-1)内线性关系良好,标准曲线为y=1. 20×10^(-3)x+2. 06×10^(-2)(r=0. 998 7),定量下限为5 ng·m L^(-1)。批内、批间RSD均小于15%,相对偏差为-7. 36%～3. 62%,提取回收率为77. 94%～93. 12%,无明显的基质效应。结论该方法简便快速,灵敏度好,准确度高,专属性强,适用于新生儿血浆中奥美拉唑浓度的测定。

Objective To establish a method for the determination of omeprazole in neonates plasma by HPLC-MS /MS.Methods After precipitated by acetonitrile,the plasma was separated by C18 column(4.6 mm×150.0 mm,3.5 μm) with mobile phase consisted of acetonitrile - water(containing 0.1% formic acid) (85 ∶ 15) at a flow rate of 0.3 mL·min^-1,column temperature was kept at 35 ℃ and lansoprazole was used as the internal standard.The ion transitions were performed under electron spray ionization in positive multiple reaction monitoring (MRM) model.The specificity,standard curve and lower limitation of quantitation, precision and recovery rate and stability were investigated.Results Calibration curves of omeprazole were obtained in range of 5-4000 ng·mL^-1 with good linearities,the standard curve was y = 1.20×10^-3x + 2.06×10^-2 (r = 0.998 7) ,and the lowest limitation of quantification was 5 ng·mL^-1 ; the intra-and inter-batch RSDs were no more than 15%,the relative errors were in range of-7.36%-3.62%,the recovery rate was 77.94%-93.12%,and there was no obvious matrix effect.Conclusion The method has good sensitivity and precision, suitable for the determination of omeprazoLe in neonates plasma.