HPLC法同时测定人血浆和尿液中三氟柳及其活性代谢物HTB

目的:采用HPLC法测定三氟柳(TFL)及其活性代谢产物HTB的血药浓度、尿药浓度。方法:采用岛津公司2010型HPLC仪,紫外检测波长为234 nm,萘普生作内标。色谱柱为YMC C₁₈(150 mm×4.6 mm,5μm),流动相为甲醇-水-甲酸(75∶25∶0.1),流速0.78 mL·min^-1,柱温30℃。血浆和尿液样本酸化后200~5μg·mL^-1,尿液标准曲线范围分别为200~5、40~1μg·mL^-1,其线性、准确度、精密度、定量下限、提取回收率、特异性、稳定性等指标均符合NMPA的指导原则要求。12例受试者单次口服TFL胶囊(含TFL 600mg)后,用所建方法检测了经时血药浓度和尿药浓度,结果可靠。结论:本法稳定可靠,可用于TFL、HTB的血药、尿药浓度测定和体内药代动力学研究。

Simultaneous determination of triflusal and its active metabolite HTB in human plasma and urine by HPLC

Objective:To establish an HPLC method for determination of triflusal(TFL)and its major active metabolite 2-hydroxy-4-trifluoromethyl benzoic acid(HTB)in human plasma and urine.Methods:Shimadzu 2010 series HPLC was used and the UV detector wavelength was set at 234 nm.Naproxen was used as an internal standard(IS).Urine and plasma samples were extracted by dichloromethane after acidized.The extraction solution was dried,re-dissolved and separated on a YMC C₁₈ column(150 mm×4.6 mm,5μm).Mobile phase was methanol-water-formic acid(75∶25∶0.1)and the flow rate was 0.78 mL·min^-1.The column oven was set at 30℃.Results:In plasma,the calibration curves for TFL was in the range of 20-0.5μg·mL^-1,for HTB was in the range of 200-5μg·mL^-1.In urine,the calibration curves for TFL was in the range of 200-5μg·mL^-1,for HTB was in the range of 40-1μg·mL^-1.The linear,accuracy,precision,limit of quantitation(LOQ),extraction recovery,specificity,stability of our method meets the requirements by National medical products administration(NMPA).After a single oral administration of TFL capsule(containing TFL 600 mg)in 12 subjects,the method was used to detect the plasma and urine concentrations,and the results were reliable.Conclusion:The method was suitable for the determination of Triflusal and its major active metabolite HTB in human plasma and urine.