液相色谱-串联质谱法测定兔血浆阿霉素浓度

LC-MS/MS determination of adriamycin in rabbit plasma

目的：建立测定兔血浆中阿霉素浓度的液相色谱-串联质谱（LC/MS/MS）法。方法：以柔红霉素为内标。血浆样品经液-液萃取法处理后，采用RESTEK Pinnacle ⅡC18 柱（150 mm×2.1 mm，5 μm）进行色谱分离，流动相为乙腈-10 mmol·L-1乙酸铵-乙酸（70：30：1），流速220 μL·min-1。用电喷雾离子化和正离子多离子反应监测方式检测阿霉素，检测离子为m/z 544.2→397.2（阿霉素）和m/z 528.2→321.3（内标）。结果：阿霉素在1.54- 1025 ng·mL^-1范围内线性关系良好，定量限为1.54 ng·mL^-1；方法回收率为99.9 % - 101.3 %,日内、日间RSD均小于14.5%。结论：本法特异、灵敏、快速、准确，适用于兔血浆中阿霉素浓度的测定。

Objective： To develop a liquid chromatography-tandem mass spectrometry （LC/MS/MS） method for the determination of adriamycin in rabbit plasma. Methods： Daunorubicin was used as the internal standard. The plasma samples were pretreated by a simple liquid-liquid extraction. The analyte was separated on a RESTEK Pinnacle ⅡC18 （150 mm×2.1 mm,5 μm） column by isocratic elution with acetonitrile-10mmol·L-1 ammonium acetate- （70：30：1） at a flow rate of 220 μL·min-1, and analyzed by mass spectrometry in the positive ion multiple reaction monitoring （MRM） mode. The precursor-to-product ion transitions of m/z 544.2→397.2 and m/z 528.2→321.3 were used to measure and quantify adriamycin and daunorubicin, respectively. Results： Good linearity was achieved over the range of 1.54-1025 ng·mL-1, the limit of quantification was 1.54 ng·mL-1. The relative recovery was 99.9 %-101.3 %, and the intra- and inter-day precisions were less than 14.5 %. Conclusion： The assay method is specific, sensitive, rapid, accurate, and suitable for the determination of adriamycin in rabbit plasma.