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HPLC-MS/MS联用技术定量测定人血浆中伊伐布雷定及其代谢产物

Quantitative Determination of Ivabradine and N-Desmethylivabradine in Human Plasma by HPLC-MS/MS

    摘要
  • 摘要: 为了定量测定人血浆中伊伐布雷定和去甲伊伐布雷定浓度，建立了HPLC-MS/MS联用方法以地西泮为内标，V（甲醇）∶V水(5 mM醋酸铵+1%甲酸)=80∶20的混合溶液为流动相，Diamosil C18（150 mm×4.6 mm，5 μm）色谱柱为分析柱，通过电喷雾离子源(ESI)，以正离子多反应监测(MRM)方式检测。用于定量分析的离子对分别为m/z 469.2→177.1（伊伐布雷定），m/z 455.2→177.1（去甲伊伐布雷定），m/z 285.1→193.1（地西泮）。伊伐布雷定的标准曲线线性范围为0.101 3～101.3 μg/L，定量下限为0.101 3 μg/L；去甲伊伐布雷定的标准曲线线性范围为0.085～25.5 μg/L，定量下限为0.085 μg/L。日内、日间精密度的RSD<15%，平均回收率>75%。

     

    Abstract: Ivabradine and N-desmethylivabradine in human plasma was determined by high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS)．Diazepam was used as internal standard．Ivabradine and N-desmethylivabradine was separated on a Diamosil C18 column (150 mm×4.6 mm×5 μm)．Electrospray ionization(ESI) source was applied，and multiple reaction monitoring(MRM) mode was operated in the positive mode with the monitor ions at m/z 469.2→177.1 for ivabradine, m/z 455.2→177.1 for N-desmethylivabradine and m/z 285.1→193.1 for the interna1 standard, respectively. The linear calibration curve are obtained over the concentration range of 0.101 3—101.3 μg/L for ivabradine and 0.085—25.5 μg/L for N-desmethylivabradine．The limit of quantitation are 0.101 3 μg/L and 0.085 μg/L for ivabradine and N-desmethylivabradine, respectively. The inter-day and intra-day precision (RSD) is less than 15%. The average recoveries are above 75%.

     

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