高效液相色谱法同时测定人尿液中布洛芬和吲哚美辛的浓度
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篇名: 高效液相色谱法同时测定人尿液中布洛芬和吲哚美辛的浓度
TITLE:
摘要: 目的:建立同时测定人尿液中布洛芬和吲哚美辛浓度的方法。方法:尿液样品经乙腈沉淀蛋白后,采用高效液相色谱法测定。色谱柱为Discovery C18,流动相为乙腈-20 mmol/L乙酸铵溶液(85 ∶ 15,V/V,用冰醋酸调节pH至3.5),紫外检测波长为220 nm,流速为1.0 mL/min,柱温为室温,进样量为80 μL。结果:布洛芬和吲哚美辛的尿药浓度均在0.1~50.0 μg/mL范围内线性关系良好(r分别为0.999 6、0.999 5,n=3),定量下限均为0.1 μg/mL,最低检测限均为0.03 μg/mL;日内、日间RSD均小于10%(n=5),准确度为94.7%~97.2%;布洛芬和吲哚美辛的提取回收率分别为89.5%~91.8%、90.2%~92.4%(RSD均小于10%,n=15)。结论:该方法简便、快速,且选择性、精密度、准确度良好,适用于人尿液中布洛芬和吲哚美辛浓度的同时测定。
ABSTRACT: OBJECTIVE: To establish a method for simultaneous determination of ibuprofen and indomethacin concentration in human urine. METHODS: The urine samples were precipitated by acetonitrile. HPLC method was adopted. The determination was performed on Discovery C18 column with mobile phase consisted of acetonitrile-20 mmol/L ammonium acetate solution (85 ∶ 15,V/V, pH value adjusted to 3.5 with glacial acetic acid) at the flow rate of 1.0 mL/min. UV detection wavelength was set at 220 nm. The column temperature was room temperature, and sample size was 80 μL. RESULTS: The linear range of ibuprofen and indomethacin were both 0.1-50.0 μg/mL (r=0.999 6, 0.999 5,n=3). The limits of quantitation were both 0.1 μg/mL, and the limits of detection were both 0.03 μg/mL. RSDs of inter-day and intra-day were all lower than 10% (n=5), and accuracy ranged 94.7%-97.2%. The extraction recoveries of ibuprofen and indomethacin were 89.5%-91.8% and 90.2%-92.4% (all RSDs<10%,n=15), respectively. CONCLUSIONS: The method is simple and rapid with high selectivity, sensitivity and accuracy. It is suitable for simultaneous determination of ibuprofen and indomethacin concentration in human urine.
期刊: 2017年第28卷第26期
作者: 刘丰,周辉,袁泰先
AUTHORS: LIU Feng,ZHOU Hui,YUAN Taixian
关键字: 高效液相色谱法;布洛芬;吲哚美辛;尿药浓度
KEYWORDS: HPLC; Ibuprofen; Indomethacin;Urine concentration
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