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 ～ 20 μg· mL-1,最低定量浓度0.01 μg· 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.c
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