RESUMO
A method based on in situ formed ionic liquids microextraction-ultra performance liquid chromatography(ISFILM-UPLC) was established for the determination of vancomycin in human serum.The samples were pretreated by vortex and centrifugation.[C6MIM] [Br] and NaPF6 were applied as the extracting agent,and Metronidazole as the internal standard.Methanol was applied to redissolve the precipitate.The separation was carried out on a BEH C18 column,and the mobile phase consisted of methanol and 0.05 mol/L monopotassium phosphate solution.The flow rate was 0.2 mL/min,the injection volume was 5 μL,and the column temperature was 18 ℃.The key parameters of this method such as the specificity,accuracy and precision were validated.This method showed good correlation with the immunoassay.It shows great potential for the application in clinical practice.
RESUMO
@#A method based on direct protein precipitation-ultra performance liquid chromatography was established for the determination of trace 5-fluorouracil in serum. The samples were pretreated with 6% perchloric acid as the precipitant and 5-chlorouracil as the internal standard, and the supernatant separated after vortex mixing and high speed centrifugation was used as the test sample. The separation was carried out with an Acquity HSS T3 column and the mobile phase consisting of water and acetonitrile, and the flow rate was 0. 2 mL/min; the injection volume was 5 μL, and the column temperature was 20 °C. The key parameters of this method such as specificity, accuracy, precision and linearity, were validated. Compared with other methods, this method can complete the analysis with significantly reduced time and cost. The established method is useful for therapeutic drug monitoring of 5-fluorouracil plasma concentration and it has been successfully applied in clinical cases.