LC-MS法检测人血浆中右酮洛芬的浓度

Determination of dexketoprofen in human plasma by LC-MS

目的:建立LC-MS测定人血浆中右酮洛芬浓度的方法。方法:待测血浆样品经甲醇沉淀后,用LC-MS法进行检测,以非布司他为内标。色谱柱为Inspire C18(150 mm×2.1 mm,5μm),流动相为5 mmol.L-1醋酸铵溶液(0.05%乙酸)-甲醇(32∶68),流速为0.35 mL.min-1;质谱采用电喷雾离子化(ESI)方式和选择性离子检测(SIM)模式,检测离子为负离子。结果:本方法线性范围为0.01～20μg.mL-1,最低定量浓度0.01μg.mL-1,准确度、精密度以及稳定性均符合有关要求。结论:该方法简便、准确,灵敏度高,专属性强,适用于人血浆中右酮洛芬浓度的测定。

Objective： To establish a liquid chromatography-mass spectrometry（LC-MS） method for determination of dexketoprofen in human plasma.Methods： The plasma samples were precipitated by methanol.The drug and an internal standard（febuxostat） were separated on a Inspire C18（150 mm×2.1 mm,5 μm） column by Agilent LC-MS with 5 mmol·L-1 ammonium acetate（0.05% acetic acid）-methanol（32∶68） as the mobile phase at a flow rate of 0.35 mL·min-1.The detection was carried out by means of electrospray ionization mass spectrometry in negative ion mode.Selective ion（SIM） mode was used.Results： The assay had the calibration range from 0.01 to 20 μg·mL-1 and the lower limit of quantification（LLOQ） was 0.01 μg·mL-1 for dexketoprofen.The accuracy,precision（intra-day and inter-day）,sensitivity,specificity and stability（ambient temperature,freeze/thaw,freeze storage） of the method fulfilled the analytical validation criteria of the guideline.Conclusion： The method is simple,accurate,sensitive and specific for determination of dexketoprofen in human plasma.