ABSTRACT
The purpose of this study was to compare pharmacokinetic (PK) parameters obtained using two newly developed assays,HPLC-UV and UPLC-ESI-MS/MS.Selection of assay and results obtained therefrom are very important in PK studies and can have a major impact on the PK-based clinical dose and usage settings.For this study,we developed two new methods that are most commonly used in biosample analysis and focused on PK parameters obtained from them.By HPLC-UV equipped with a Luna-C8 column using UV detector,cefprozil diastereomers were separated using water containing 2％ (V/V) acetic acid and acetonitrile as a mobile phase.By UPLC-ESI-MS/MS equipped with a HALO-C18column,cefprozil diastereomers were separated using 0.5％ (V/V) aqueous formic acid containing 5 mM ammonium-formate buffer and methanol as a mobile phase.Chromatograms showed high resolution,sensitivity,and selectivity without interference by plasma constituents.Both intra-and inter-day precisions (CV,％)were within 8.88％ for HPLC-UV and UPLC-ESI-MS/MS.Accuracy of both methods was 95.67％-107.50％.These two analytical methods satisfied the criteria of international guidance and could be successfully applied to PK study.Comparison of PK parameters between two assays confirmed that there is a dif-ference in the predicted minimum plasma concentrations at steady state,which may affect clinical dose and usage settings.Furthermore,we confirmed possible correlation between PK parameters and various biochemical parameters after oral administration of 1000 mg cefprozil to humans.
ABSTRACT
A direct enantio-, diastereo-, and chemo-selective high-performance liquid chromatographic method was developed for determining the content, enantiomeric purity, and related substances of the chiral antidepressant drug sertraline HCl in a single chromatographic run. The separation was achieved on a chiral stationary phase based on amylose tris(3-chloro-5-methylphenylcarbamate) under reversed-phase conditions. The method was optimized by evaluating the influence of the temperature and mobile phase composition on the retention and selectivity. The application of the single-run approach allowed to baseline resolve all investigated species in less than 15 min, without using buffers or tandem-coupled columns. The chromatographic method was validated according to the guidelines of the Official Medi-cines Control Laboratory and applied to control the content of sertraline HCl and related chiral sub-stances in a generic antidepressant formulation.
ABSTRACT
Seeds of Trigonella foenum-graecum L., as a raditional Chinese medicine, are rich n steroidal saponins. The systematic research on steroidal saponins of Trigonella foenum-graecum, including the study on furostanol saponins and spirostanol saponins, the rapid characterization and dentification of steroidal saponins, and he analytical and preparative separation of C-25 R/S-spirostanol saponin diastereomers using supercritical fluid chromatography, was performed. The results of research are helpful to the development and utilization of Trigonella foenum-graecum seeds, and the methods could provide reference for the chemical research on other traditional Chinese medicines.
ABSTRACT
AIM: To investigate the application of microemulsion TLC to separation and identification of(Z)-and(E)-resveratrol and piceid in Polygonum cuspidatum based on polyamide film as stationary phase.METH-ODS: SDS-n-butane-n-heptane-aqueous microemulsion as the development in combination with aminic acid and methonal as the modifier,the influence of the change in components of microemulsion on the resolution was exam-ined to search for the optimal separation condition of Polygonm cuspidatum extract collected from 6 production places.RESULTS: The best mobile phase was the microemulsion containing 4% SDS,80% water-methyl acid-methanol(1.0 ∶ 2.0 ∶ 1.0).As compared with conventional TLC,resolution of microemulsion TLC for resveratrol and piceid were improved markedly.CONCLUSION: Microemulsion TLC is an efficient,simple and new method for separating and identifing(Z)-and(E)-diastereomers of resveratrol and piceid in Polygonum cuspidatum.