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建立了同时测定血浆中吲哚美辛和布洛芬两种非甾体抗炎药的HPLC测定方法。样品采用乙腈沉淀蛋白提取后离心,上清液用氮气吹干流动相复溶,以乙腈:20 mmol/L乙酸铵水溶液(甲酸调节p H为3.5)=85:15(V/V)进行洗脱,在ZORBAX SB-C18(4.6 mm×250 mm,5μm)色谱柱上分离,流速为1 m L/min,检测波长220 nm,采用内标法定量,吲哚美辛和布洛芬互为内标。结果表明吲哚美辛和布洛芬在0.1~50μg/m L范围内呈良好的线性关系,吲哚美辛和布洛芬的检出限(S/N=3)分别为1.3 ng和2.0 ng。回收率在86.3%~102.0%之间,日内精密度RSD3.4%。经方法学验证,该方法适用于血浆样品中吲哚美辛和布洛芬的测定,且方法专属性好、简便快捷。
A HPLC method for simultaneous determination of indometacin and ibuprofen in plasma was established. The sample was extracted with acetonitrile precipitation and centrifuged. The supernatant was reconstituted with a nitrogen-cooled mobile phase and washed with acetonitrile: 20 mmol / L ammonium acetate aqueous solution (pH 3.6 for formic acid) = 85: 15 (V / V) Off and separated on a ZORBAX SB-C18 (4.6 mm × 250 mm, 5 μm) column at a flow rate of 1 mL / min with a detection wavelength of 220 nm and quantified using an internal standard method with indomethacin and ibuprofen Standard. The results showed that there was a good linear relationship between indomethacin and ibuprofen in the range of 0.1 ~ 50μg / mL. The detection limits (S / N = 3) of indomethacin and ibuprofen were 1.3 ng and 2.0 ng, respectively. The recovery rate was between 86.3% and 102.0%, and the intraday RSD accuracy was 3.4%. The method validation, the method is suitable for the determination of indomethacin and ibuprofen in plasma samples, and the method specificity is good, simple and quick.