超高效液相色谱-串联质谱法测定人血浆中罗匹尼罗浓度

Determination of Ropinirole in Human Plasma by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 建立了超高效液相色谱串联质谱(UPLC-MS/MS)测定人血浆中罗匹尼罗浓度的方法,采用向血浆样品中加入氘代内标后,以甲基叔丁基醚进行萃取。色谱柱为Acquity UPLC BEH C18柱(2.1 mm×50 mm×1.7 μm),流动相为甲醇10 mmol/L乙酸铵(含0.2%氨水)(80∶20,V/V),流速为0.4 mL/min。采用多反应监测(MRM)扫描模式,以电喷雾离子源(ESI)正离子方式检测。结果显示,方法的线性范围为0.02~5 μg/L,最低定量限为0.02 μg/L,日内、日间精密度均小于15%,准确度在85%~115%之间,萃取回收率为85%。该方法快速、灵敏、专属性强,不受血浆基质的影响,不同条件下的稳定性考察结果良好,适用于罗匹尼罗的人体药代动力学研究。

     

    Abstract: A method of ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of ropinirole in human plasma. The plasma samples were extracted with methyl tert-butyl ether after the addition of deuterated internal standard. The analytical column was Acuity UPLC BEH C18 column (2.1 mm×50 mm×1.7 μm), and the mobile phase was composed of methanol 10 mmol/L ammonium formate in 0.2% ammonium solution (80∶20, V/V). The flow rate was 0.4 mL/min. Detection was performed with multiple reactions monitoring (MRM) using positive electrospray ionization(ESI). The results show that the calibration curve is linear over the concentration range of 0.02-5 μg/L. The lower limit of quantification is 0.02 μg/L. Inter-day and intra-day precision are less than 15%, and the accuracy is within 85%-115%. Extraction recoveries are around 85% and the determination is independent of plasma matrix. In addition, the analyte is proved to be stable under various storage and processing conditions. Therefore, this method proves to be rapid, sensitive and specific, and suitable for the pharmacokinetic study of ropinirole in humans.

     

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