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目的:建立灵敏、易操作的液相色谱(串联质谱法测定人血浆中普拉克索,并应用于临床药动学研究。方法:血浆样品经乙醚-二氯甲烷(3:2,v/v)液-液萃取后,以乙腈-10 mmol.L-1醋酸铵-甲酸(60:40:0.1,v/v/v)为流动相,Venusil ASB-C18柱(150 mm×4.6 mm,5μm)进行分离,采用电喷雾电离源,以选择反应监测(SRM)方式进行正离子检测,用于定量分析的离子反应分别为m/z212→m/z(111+126+153)(普拉克索)和m/z243→m/z210(石杉碱甲,内标)。结果:测定血浆中普拉克索的线性范围为5.92～740 pg.mL-1,定量下限为5.92 pg.mL-1,日内、日间精密度(RSD)均小于9.7%,准确度(RE)在-2.5%～0.6%之间。本法被成功应用于健康受试者单剂量口服0.125 mg和0.25 mg盐酸普拉克索片的药动学研究。结论:本方法同时选择3个主要碎片离子作为普拉克索定量产物离子,明显改进了分析方法的灵敏度,适用于人血浆样品中普拉克索的测定。
Objective: To establish a sensitive and easy-to-use liquid chromatography (tandem mass spectrometry) for the determination of pramipexole in human plasma.Methods: The plasma samples were extracted with 3: 2, v / v (150 mm × 4.6 mm, 5 μm) using a mobile phase of acetonitrile-10 mmol·L-1 ammonium acetate-formic acid (60:40: 0.1, v / v / v) ), And electrospray ionization was used to detect positive ions by selective reaction monitoring (SRM). The ion reactions for quantitative analysis were m / z 212 → m / z (111 + 126 + 153) (pramipexole ) And m / z243 → m / z210 (huperzine A, internal standard) .Results: The linear range of pramipexole in plasma was 5.92 ~ 740 pg.mL-1 and the lower limit of quantification was 5.92 pg.mL- Day and day precision was less than 9.7%, accuracy (RE) between -2.5% ~ 0.6% .This method has been successfully applied to healthy subjects a single oral dose of 0.125 mg and 0.25 mg Plump hydrochloride The pharmacokinetics of the films was studied.Conclusion: The method selected three major fragment ions as the quantitative product ions of pramipexole, which significantly improved the sensitivity of the analytical method and was suitable for the determination of pramipexole in human plasma samples.