高效液相色谱串联质谱法测定大鼠血浆及组织中卡巴拉汀含量

 目的 建立准确、灵敏、可靠的高效液相色谱-串联质谱法 (HPLC-MS/MS)检测大鼠血浆及组织中卡巴拉汀的含量。方法 采用Agilent C₁₈ (4.6 mm×100 mm，3.5 μm) 色谱柱，以水-甲醇 (20∶80) 为流动相，流速0.3 mL·min^-1。质谱采用电喷雾电离源正离子模式 (ESI⁺)，多重反应检测 (MRM) 方式进行离子监测，药物卡巴拉汀和内标安替比林用于定量的特征反应分别是251.3→206.1和189.1→106.1。体内所有生物样品采用醋酸乙酯萃取法处理。结果 卡巴拉汀在各自测定的浓度范围内线性均良好，r > 0.999 0，相对提取回收率>60%，中、高浓度精密度RSD

Quantitative Determination of Rivastigmine in Rat Plasma and Tissues by HPLC-MS/MS Method

OBJECTIVE To establish a highly accurate,sensitive and credible high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method for the determination of rivastigmine in rat plasma and tissues.METHODS All biological samples were extracted with ethyl acetate.Chromatographic separation was performed on an Agilent C18 column(4.6 mm×100 mm,3.5 μm) using water-methanol(20∶80) as mobile phase at a flow rate of 0.3 mL·min-1.The MS analysis was performed by multiple reaction monitoring(MRM) with electronic spray ionization source(ESI+) for quantitative response of rivastigmine(251.3→206) and the internal standard,antipyrine(189.1→106.1) respectively.RESULTS The calibration curves of rivastigmine in plasma and tissues showed satisfactory linearity,and the relative extraction recovery of three concentrations in plasma and all tissues were over 60% except some individuals and all RSDs met the requirements.The limit of quantification of rivastigmine in plasma and tissues were 0.1 and 0.2 ng·mL-1 respectively.CONCLUSION The method is rapid,accurate,highly selective and sensitive,and is suitable for the quantitative analysis of rivastigmine in biological sample of rats.