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目的:建立高效液相色谱-质谱联用测定右酮洛芬人体血(尿)药浓度的方法,考察右酮洛芬的血药浓度及经尿排泄特征。方法:色谱柱为Inspire-C_(18)(150 mm×2.1 mm,5μm),以甲醇-水(5 mmo1.L~(-1)醋酸铵和0.05%乙酸)(68:32,v/v)为流动相。质谱采用电喷雾离子源四级杆质谱,以选择性离子监测方式进行负离子检测。12名健康受试者单次静脉滴注右酮洛芬氨丁三醇注射液25 mg后,采集血浆并定时收集尿液。采用甲醇直接沉淀法处理样品后,评价右酮洛芬的血药浓度及尿排泄特征。结果:右酮洛芬在0.01～20.66μg·ml~(-1)浓度范围内线性关系良好,精密度(RSD)为4.3%～7.2%,准确度(RE)为0.7%～5.3%,绝对回收率为98.9%～102.2%。静滴右酮洛芬氨丁三醇注射液25 mg后,C_(max)(3.53±0.57)μg·ml~(-1),AUC_(0-t)(7.98±0.90)μg·h·ml~(-1),t_(1/2)(2.0±0.6)h,t_(max)(0.5±0.03)h。24 h内累积排泄率为(1.2±0.23)%。结论:该方法简单,符合生物样品分析要求;右酮洛芬氨丁三醇在体内以右酮洛芬形式经尿排泄较少,12 h内基本排泄完全。
OBJECTIVE: To establish a method for the determination of dexketoprofen human blood (urinary) drug concentration by high performance liquid chromatography-mass spectrometry (HPLC-MS) and to investigate the dexketoprofen blood concentration and urine excretion characteristics. METHODS: The column was Inspire-C 18 (150 mm × 2.1 mm, 5 μm) with methanol-water (5 mmo1.L -1 ammonium acetate and 0.05% acetic acid) ) As mobile phase. Mass spectrometry using electrospray ionization quadrupole mass spectrometry, selective ion monitoring of negative ion detection. Twelve healthy subjects received a single intravenous infusion of 25 mg of dexketoprofen trometamol injection, and plasma was collected and urine collected regularly. After the sample was treated by methanol precipitation method, the blood concentration and urinary excretion of dexketoprofen were evaluated. Results: Dexketoprofen showed good linearity in the concentration range of 0.01-20.66μg · ml -1 with RSD of 4.3% -7.2% and accuracy of RE of 0.7% -5.3% The recovery rate was 98.9% ~ 102.2%. After intravenous injection of dexketoprofen trometamol 25 mg, C max 3.53 ± 0.57 μg · ml -1, AUC 0-t 7.98 ± 0.90 μg · h · ml ~ (-1), t 1/2 (2.0 ± 0.6) h, t max (0.5 ± 0.03) h. The cumulative excretion rate within 24 h was (1.2 ± 0.23)%. Conclusion: The method is simple and meets the requirements of biological sample analysis. Dexketoprofen trometamol is less excreted in the body in the form of dexketoprofen and excretes completely within 12 h.