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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(5mM醋酸铵+1%甲酸)=80∶20的混合溶液为流动相,Diamosil C18(150mm×4.6mm,5μm)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/z469.2→177.1(伊伐布雷定),m/z455.2→177.1(去甲伊伐布雷定),m/z285.1→193.1(地西泮)。伊伐布雷定的标准曲线线性范围为0.101 3～101.3μg/L,定量下限为0.101 3μg/L;去甲伊伐布雷定的标准曲线线性范围为0.085～25.5μg/L,定量下限为0.085μg/L。日内、日间精密度的RSD<15%,平均回收率>75%。
In order to quantitatively determine the concentrations of ivabradine and noradrepradine in human plasma, an HPLC-MS / MS method was established using diazepam as internal standard, V (methanol): V water (5 mM ammonium acetate + % Formic acid) = 80:20 was used as the mobile phase. Diamosil C18 column (150 mm × 4.6 mm, 5 μm) was used as the analytical column and detected by positive ion MRM (Electron Spray Ionization Source) . The ion pairs used for the quantitative analysis were m / z 469.2 → 177.1 (ivabradine), m / z 455.2 → 177.1 (demyivirdenib), m / z 285.1 → 193.1 (diazepam ). The standard curve of ivabradine linear range of 0.101 3 ~ 101.3μg / L, the lower limit of quantification of 0.101 3μg / L; standard curve of demyavirbine linear range of 0.085 ~ 25.5μg / L, the lower limit of quantification of 0.085μg / L. Intraday and interday precision RSD <15%, the average recovery rate of> 75%.