RESUMO
Objective: To establish an HPLC-fluoremetry method for determination of the plasma concentration of mycophenolic acid ( MPA) in renal transplantation patients. Methods:The sample was subjected to precipitate proteins using acetonitrile, and the supernatant (20 μl) was used for the sample injection and determination on a Hypersil BDS C18 (250 mm × 4. 6 mm, 5 μm) column with temperature at 25℃. The mobile phase consisted of acetonitrile-methanol-0. 2 mol·L-1 dipotassium hydrogen phosphate buffer (pH=9. 0)( 18∶2∶80)with the flow rate of 1. 0 ml·min-1. The excitation wavelength (Ex) was 342 nm and the emission wave-length ( Em) was 425 nm. Results:The endogenous plasma impurities and drug combinations had no interference with the determina-tion. The calibration curve was linear over the range of 0. 25-50. 00 mg·L-1(r=0. 999 7), and the lower limit of quantification was 0. 25 mg·L-1 . The mean methodological recovery was 99. 12% and the mean extraction recovery was 93. 27%, the intra-day RSD was less than 2% and the inter-day RSD was less than 6%. Totally 10 cases of renal transplantation patients were with mycophenolate mofetil at the dose of 0. 5-1. 75 g·d-1 , and MPA in plasma was within the range of 0. 43-21. 58 mg·L-1 . Conclusion:The method is rapid, sensitive, accurate and convenient, which can be used in the quantitative determination of plasma concentration of MPA in re-nal transplantation patients.
RESUMO
OBJECTIVE:To establish a method for content determination of the principal agent in bumetanide tablets by HPLC-fluoremetry.METHODS:HPLC-fluoremetry was carried out using a Kromasil C 18 column and a mobile phase con?sisting of acetonitrile-water(50∶50),the fluorescence detector of228nm for excitation and418nm for emission was used,the internal standard was dixiben,the flow rate was0.6ml/min,the sample size was20?l,the column temperature was the same as room temperature.RESULTS:The concentration of bumetanide was linear in the range of16.75～335.00?g/ml(r=0.9997),the average recovery was99.26%(RSD=0.49%,n=3).CONCLUSION:The present method is convenient and reliable,whi_ ch can be used for content determination of the principal agent in bumetanide tablets.
RESUMO
OBJECTIVE:To determine the plasma concentration of mycophenolic acid (MPA) in renal transplantation patients by HPLC-Fluoremetry. METHODS: The sample was subjected to precipitation of proteins using 5% Zinc Sulfate methanol saturated solution,and the supernatant (20 ?L) was taken for sample injection and determination on Zorbax Eclipse XDB C18 with mobile phase consisted of acetonitrile-methanol-0.2 mol?L-1 glycine buffer(18∶2∶80,pH=9.0) at a flow rate of 1.0 mL?min-1. The column temperature was of 25℃;the excitation wavelength(EX) was 342 nm and the emission wavelength(EM) was 425 nm. RESULTS: The linear range of MPA was 0.5～40 mg?L-1,with its lowest limit of quantitation at 0.5 mg?L-1. The methodology recovery was 98.23%～101.00%;the extraction recovery of MPA was 91.56%～94.46%;the intra-day RSD was 0.64%～3.22% and the inter-day RSD was 5.12%～6.10%. CONCLUSION: The method is sensitive,rapid,accurate,convenient,and applicable for the quantitative determination of plasma concentration of MPA in renal transplantation patients.