UPLC-MS/MS法同时测定人血浆中普拉克索和金刚烷胺浓度

目的:建立利用UPLC-MS/MS法同时测定人血浆中普拉克索和金刚烷胺的分析方法。方法:在碱性条件下,血浆样品经乙酸乙酯萃取。采用Acquity UPLC BEH C₁₈ (2.1 mm×50 mm,1.7 μm)色谱柱,甲醇(A)-0.01%甲酸水(B)为流动相,梯度洗脱,流速0.2 mL·min^-1,柱温为30 ℃;采用电喷雾离子源、正离子方式、多反应监测(RRM),普拉克索离子反应为m/z 212→153,金刚烷胺为m/z 152→135,内标伪麻黄碱为m/z 166→148。结果:普拉克索血浆质量浓度在10~1 200 pg·mL^-1,金刚烷胺在0.7~700 ng·mL^-1内线性关系良好,两者日内、日间RSD均小于9.8%,方法回收率均在100.3%~106.0%之间。所测30例帕金森患者中,普拉克索平均谷浓度为(643.61±243.19) pg·mL^-1,金刚烷胺平均谷浓度为(551.67±81.14) ng·mL^-1。 结论:建立的检测方法可用于同时测定人体血浆中普拉克索和金刚烷胺的浓度。

Objective:To develop a sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of pramipexole and amantadine in human plasma.Methods:The plasma sample was first extracted with acetic ether in alkaline conditions.UPLC-MS/MS was performed on an Acquity UPLC BEH C₁₈ (2.1 mm×50 mm,1.7 μm) column with the mobile phase consisting of methanol (A) and 0.01% aqueous formic acid (B) in gradient elution.The flow rate was controlled at 0.2 mL·min^-1,and the column temperature was set at 30 ℃.A mass spectrometer equipped with electrospray ionization source was used as detector operate in the positive ion mode.Multiple reaction monitoring (RRM) mode was performed using the transition of m/z 212→153,m/z 152→135 and m/z 166→148 to quantify pramipexole,amantadine and internal standard of pseudoephedrine,respectively.Results:In human plasma,the standard curves of pramipexole and amantadine were linear from 10-1 200 pg·mL^-1 and 0.7~700 ng·mL^-1,the overall relative recoveries ranged from 100.3%-106.0% with the intra- and inter-day RSDs both below 9.8%.In 30 cases of Parkinson's patients,the average trough concentration of pramepexole and amantadine was (643.61± 243.19) pg·mL^-1 and (551.67±81.14) ng·mL^-1,respectively.Conclusion:The established method can be used to simultaneously determine pramipexole and amantadine.

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