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目的建立快速、灵敏的液相色谱-串联质谱法(HPLC-MS/MS)测定大鼠血浆中活性寡肽RX31的浓度。方法血浆样品经甲醇蛋白沉淀后,以0.1%甲酸-甲醇为流动相梯度洗脱,CapcellMGⅢCl8柱分离。采用电喷雾电离源,以多反应监测(MRM)方式进行正离子检测,用于定量分析的离子反应分别为m/z640.3→m/z623.3(RX31)和m/z596.1→m/z287.1(内标,RX20)。结果在本实验条件下,血浆中RX31的线性范围为3.91～500ng/ml,定量下限为3.91ng/ml,日内、日间精密度(相对标准差,RSD)均小于12%,准确度(相对误差,RE)在-11%～5%。结论该法快速、灵敏、准确,可用于RX31的药代动力学研究。
OBJECTIVE To establish a rapid and sensitive liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) for the determination of RX31 in rat plasma. Methods Plasma samples were precipitated with methanolic protein and eluted with 0.1% formic acid-methanol as mobile phase. CapsllMGⅢCl8 column was used for the separation. The electrospray ionization source was used to conduct positive ion detection by multi-reaction monitoring (MRM). The ion reactions for quantitative analysis were m / z 640.3 → m / z 623.3 (RX31) and m / z 596.1 → m /z287.1 (internal standard, RX20). Results Under the experimental conditions, the linear range of RX31 in plasma was 3.91 ~ 500ng / ml and the lower limit of quantification was 3.91ng / ml. The intra-day and inter-day precision (RSD) was less than 12%, and the accuracy Error, RE) at -11% ~ 5%. Conclusion The method is rapid, sensitive and accurate and can be used to study the pharmacokinetics of RX31.