液相色谱-四极杆静电场轨道阱高分辨质谱检测血浆中门冬胰岛素

Determination of insulin aspart in plasma by liquid chromatography-quadrupole electrostatic field orbitrap high-resolution mass spectrometry

利用液相色谱-四极杆静电场轨道阱高分辨质谱仪建立一种人体血浆中门冬胰岛素的快速检测方法。使用甲醇-乙腈-乙酸溶液(49∶49∶2,V/V/V)沉淀蛋白;Agilent Eclipse Plus C18色谱柱(50 mm×2.1 mm,3.5μm)分离,以0.1%甲酸水和0.1%甲酸-乙腈作为流动相进行梯度洗脱;质谱分析采用选择离子监测(SIM)扫描模式。结果表明,人体血浆中门冬胰岛素在0.1~10μg/mL范围内线性关系良好(R^(2)=0.9938),定量限为0.1μg/mL,检出限为0.05μg/mL;提取回收率范围在71.6%~106.2%;日内及日间相对标准偏差(RSD)均小于15%。该方法能够满足公安机关对实际案件的检验需求。

A rapid detection method for insulin aspart in human plasma was established by using liquid chromatography-quadrupole electrostatic field orbitrap high-resolution mass spectrometry.Samples were pretreated with a precipitant of methanol-acetonitrile-acetic acid solution(49∶49∶2,V/V/V),an Agilent Eclipse Plus C18 column(50 mm×2.1 mm,3.5μm)was selected,with 0.1%aqueous formic acid and 0.1%formic acidacetonitrile as mobile phases for gradient elution,and mass spectrometry was performed in selected ions monitoring(SIM)scan mode.The experimental results showed that the linear relationship of insulin aspart in human plasma was good in the range of 0.1-10μg/mL(R^(2)=0.9938),with the limit of quantification of 0.1μg/mL,and the limit of detection of 0.05μg/mL.The recoveries ranged from 71.6%to 106.2%,and the relative standard deviations(RSDs)of the intra-day and inter-day were both less than 15%.The method can meet the inspection needs of actual cases.