Aim To develop and validate a liquid chromatographic/tandem mass spectrometric (LC/MS/MS) method for the simultaneous quantitation of pseudoephedrine and diphenhydramine in human plasma after oral administration of co...Aim To develop and validate a liquid chromatographic/tandem mass spectrometric (LC/MS/MS) method for the simultaneous quantitation of pseudoephedrine and diphenhydramine in human plasma after oral administration of compound preparation. Methods Samples spiked with the analytes and the internal standard, chlorphenamine, were processed using liquid-liquid extraction. The extract was chromatographed on a Diamonsil C 18 column. The mobile phase consisted of methanol-water-formic acid (70∶30∶1), at a flow rate of 0.65 mL·min -1 . A Finnigan TSQ tandem mass spectrometer equipped with atmospheric pressure chemical ionization source was used as detector and was operated in the positive ion mode. Selected reaction monitoring (SRM) using the precursor/product ion combinations of m/z 166→148 and m/z 256→167 were used to quantify pseudoephedrine and diphenhydramine, respectively. Results The linear concentration ranges of the calibration curves for pseudoephedrine and diphenhydramine were both 2.0-400.0 μg·L -1 . The lower limit of quantification of both analytes was 2.0 ng·mL -1 . Each sample was chromatographed within 3.9 min. Conclusion The method was successfully used in simultaneous determination of pseudoephedrine and diphenhydramine in human plasma after oral administration of a compound preparation containing 60 mg pseudoephedrine chloride and 50 mg diphenhydramine chloride. The method was shown to be suitable for clinical investigation of pseudoephedrine and diphenhydramine pharmacokinetics.展开更多
In pH 4.5 Britton-Robinson(BR)buffer solution,erythrosin(ET)can react with diphenhydramine(DP)to form a 1:1 ion-association complex,which not only results in the change of the absorption spectra,but also results in th...In pH 4.5 Britton-Robinson(BR)buffer solution,erythrosin(ET)can react with diphenhydramine(DP)to form a 1:1 ion-association complex,which not only results in the change of the absorption spectra,but also results in the great enhancement of resonance Rayleigh scattering(RRS)and the quenching of fluorescence.Furthermore,a new RRS spectrum will appear,and the maximum RRS wavelength was located at about 580 nm.In this work,the spectral characteristics of the absorption,fluorescence and RRS,the optimum conditions of the reaction and the properties of an analytical chemistry were inves- tigated.A sensitive,simple and new method for the determination of DP by using erythrosin as a probe has been developed.The detection limits for DP were 0.0020μg/mL for RRS method,0.088μg/mL for absorption method and 0.094μg/mL for fluorophotometry.There was a linear relationship between the absorbance,RRS and fluorescence intensities and the drug concentration in the range of 0.0067-2.0, 0.29-6.4 and 0.31-3.2μg/mL,respectively.The effects of the interaction of diphenhydramine and erythrosin on the absorption,fluorescence and resonance Rayleigh scattering spectra were discussed. In light polarization experiment,the polarization of RRS at maximum wavelength was measured to be P =0.9779,and it revealed that the RRS spectrum of DP-ET complex consists mostly of resonance scat- tering and few resonance fluorescence.In this study,enthalpy of formation and mean polarizability were calculated by AM1 quantum chemistry method.In addition,the reaction mechanism and the rea- sons for the enhancement of scattering spectra and the energy transfer between absorption,fluores- cence and RRS were discussed.展开更多
文摘Aim To develop and validate a liquid chromatographic/tandem mass spectrometric (LC/MS/MS) method for the simultaneous quantitation of pseudoephedrine and diphenhydramine in human plasma after oral administration of compound preparation. Methods Samples spiked with the analytes and the internal standard, chlorphenamine, were processed using liquid-liquid extraction. The extract was chromatographed on a Diamonsil C 18 column. The mobile phase consisted of methanol-water-formic acid (70∶30∶1), at a flow rate of 0.65 mL·min -1 . A Finnigan TSQ tandem mass spectrometer equipped with atmospheric pressure chemical ionization source was used as detector and was operated in the positive ion mode. Selected reaction monitoring (SRM) using the precursor/product ion combinations of m/z 166→148 and m/z 256→167 were used to quantify pseudoephedrine and diphenhydramine, respectively. Results The linear concentration ranges of the calibration curves for pseudoephedrine and diphenhydramine were both 2.0-400.0 μg·L -1 . The lower limit of quantification of both analytes was 2.0 ng·mL -1 . Each sample was chromatographed within 3.9 min. Conclusion The method was successfully used in simultaneous determination of pseudoephedrine and diphenhydramine in human plasma after oral administration of a compound preparation containing 60 mg pseudoephedrine chloride and 50 mg diphenhydramine chloride. The method was shown to be suitable for clinical investigation of pseudoephedrine and diphenhydramine pharmacokinetics.
基金the National Natural Science Foundation of China(Grant No.20475045)
文摘In pH 4.5 Britton-Robinson(BR)buffer solution,erythrosin(ET)can react with diphenhydramine(DP)to form a 1:1 ion-association complex,which not only results in the change of the absorption spectra,but also results in the great enhancement of resonance Rayleigh scattering(RRS)and the quenching of fluorescence.Furthermore,a new RRS spectrum will appear,and the maximum RRS wavelength was located at about 580 nm.In this work,the spectral characteristics of the absorption,fluorescence and RRS,the optimum conditions of the reaction and the properties of an analytical chemistry were inves- tigated.A sensitive,simple and new method for the determination of DP by using erythrosin as a probe has been developed.The detection limits for DP were 0.0020μg/mL for RRS method,0.088μg/mL for absorption method and 0.094μg/mL for fluorophotometry.There was a linear relationship between the absorbance,RRS and fluorescence intensities and the drug concentration in the range of 0.0067-2.0, 0.29-6.4 and 0.31-3.2μg/mL,respectively.The effects of the interaction of diphenhydramine and erythrosin on the absorption,fluorescence and resonance Rayleigh scattering spectra were discussed. In light polarization experiment,the polarization of RRS at maximum wavelength was measured to be P =0.9779,and it revealed that the RRS spectrum of DP-ET complex consists mostly of resonance scat- tering and few resonance fluorescence.In this study,enthalpy of formation and mean polarizability were calculated by AM1 quantum chemistry method.In addition,the reaction mechanism and the rea- sons for the enhancement of scattering spectra and the energy transfer between absorption,fluores- cence and RRS were discussed.
