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目的建立高效液相色谱法-质谱联用法测定人血中阿比朵尔的浓度。方法用乙腈直接沉淀蛋白法处理血浆,色谱柱:Thermo Biobasic-8色谱柱(2.1 mm×100 mm,5.0μm),流动相:乙腈(含1‰甲酸)-水(含1‰甲酸)=70∶30;流速:0.3 m L·min~(-1);进样量:10.0μL;柱温:室温。质谱用电喷雾离子源(ESI)正离子检测,多反应监测(MRM)模式。考察该方法的专属性、线性范围与定量下限、精密度与回收率、基质效应和稳定性。结果阿比朵尔血浆浓度在5.58~658.00 ng·m L~(-1)内线性关系良好,批内精密度相对标准偏差(RSD)<9.11%,批间精密度RSD<7.76%,提取回收率在70.20%~79.38%,基质效应在86.39%~98.64%。结论该法准确、灵敏度高、重现性好,可用于人体中阿比朵尔血浆浓度的测定。
Objective To establish a method for the determination of abidol in human blood by high performance liquid chromatography-mass spectrometry. Methods The plasma was precipitated by acetonitrile directly on a Thermo Biobasic-8 column (2.1 mm × 100 mm, 5.0 μm). The mobile phase consisted of acetonitrile (containing 1 ‰ formic acid) and water (containing 1 ‰ formic acid) : 30; flow rate: 0.3 m L · min -1; injection volume: 10.0 μL; column temperature: room temperature. Mass spectrometry Electrospray ionization (ESI) positive ion detection, multiple reaction monitoring (MRM) mode. The specificity, linearity and lower limit of quantitation, precision and recovery, matrix effect and stability of this method were investigated. Results The plasma concentration of abiraterol showed a good linearity within 5.58 ~ 658.00 ng · m L -1, with a relative standard deviation (RSD) of <9.11% within batch and RSD <7.76% between batches. The rates ranged from 70.20% to 79.38%, with matrix effects ranging from 86.39% to 98.64%. Conclusion The method is accurate, sensitive and reproducible. It can be used for the determination of abidol in human plasma.