HPLC-/MS/MS法测定健康人血浆中普拉克索浓度

Determination of pramipexole hydrochloride sustained-release tablets in healthy human plasma by HPLC-MS/MS

目的建立高效液相串联质谱法测定人血浆中普拉克索浓度的方法。方法在碱性条件下,用乙酸乙酯提取浓缩后,进样用LC-MS/MS,固定相为AQ-C18柱(4.6 mm×150 mm,10μm),流动相为乙腈-20 mmol.L-1醋酸铵水溶液=60∶40,质谱条件为电喷雾离子源、正离子方式、多级离子反应监测,离子反应分别为m/z:212.2→152.9(普拉克索)和m/z 273.2→109.6(吡西卡尼)。结果普拉克索的血浆浓度在5～1000 pg.mL-1内线性关系良好,Y=1.33×103X+0.05(r=0.9979),定量下限可达5 pg.mL-1。结论建立的检测方法准确、稳定,可满足血浆中普拉克索含量测定。

Objective To establish an HPLC -MS/MS method for the determination of pramipexole in healthy human plasma. Methods The plasma sample was extracted with acetic ether after evaporation of the organic layer and separated on a AQ - C18 column（4. 6 mm × 150 mm, 10 μm）. The mobile phase consisted of acetonitrile and 20 mmol · L^-1 ammonium acetate （60： 40）. A mass spectrometer equipped with electrosprayionization source was used as detector operate in the positive ion mode . Multiple reaction monitoring mode using the transition of m/z： 212.2- 152.9 and m/z： 273.2 -109.6 were used to quantify pramipexole and internal standard （IS）, respectively. Results In human plasma, the standard curve was linear from 5 - 1000 pg · mL^-1 , Y = 1.33×10^-3X ＋0. 05 （r =0. 9979）. The lower limit of quantification of faropenem was 5 pg·mL^-1. Conclusion The method had a good selectivity and reproducibility and can be used for the investigation of pramipexole in human plasma.