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建立了人血浆中麦考酚酸浓度的毛细管区带电泳测定法。200μL的血浆样品经400μL的乙腈沉淀蛋白后,紧接一段水柱进样,进样量为:0.5 psi×10 s。分离采用内径75μm,有效长度50 cm的未涂层熔硅弹性石英毛细管柱。通过均匀设计实验,选定pH为8.60的硼酸缓冲液(硼酸初始浓度为200 mmol/L)为背景缓冲液。结果显示,测定方法的标准曲线在0.625～30.0μg/mL的范围内,r平均值大于0.9997;检测下限为0.200μg/mL;日内、日间精密度均小于4.45%。应用本方法和高效液相色谱-串联质谱法,对14份接受麦考酚酸酯治疗的肾移植术后患者的血样进行分析,表明本方法准确、精密、经济,对于麦考酚酸的临床定量极具价值。
A capillary zone electrophoresis method was established for the determination of mycophenolic acid in human plasma. A 200 μL sample of plasma was precipitated with 400 μL of acetonitrile and immediately injected into a column of water at 0.5 psi × 10 s. Uncoated fused silica capillary columns with an internal diameter of 75 μm and an effective length of 50 cm were separated. Through a uniform design experiment, selected borate buffer pH 8.6 (boric acid initial concentration of 200 mmol / L) as the background buffer. The results showed that the standard curve of the determination method was in the range of 0.625-30.0μg / mL, the average value of r was greater than 0.9997, and the detection limit was 0.200μg / mL. The intra- and inter-day precision was less than 4.45%. Using this method and high performance liquid chromatography-tandem mass spectrometry, analysis of blood samples from 14 patients who underwent mycophenolate mofecoxib treatment after kidney transplantation showed that this method is accurate, precise and economical and is clinically applicable to mycophenolic acid Quantitative great value.