Several Chiral Drugs By Hplc

Chirality of drugs is an important aspect in fields of biological medicine. The separation of chiral drugs was once recognized as one of the most difficult work. With the development of various chiral technology, especially high-performance liquid chromatography, enantiospeciflc analysis is becoming a routine analytical task. In the present work, precolunin derivatization HPLC and chiral LCIMSIMS technology were used to separate and analyse several cbiral drugs. 1. Enantiospeciflc analysis of ketoprofen by RP-HIPLC with precolumn derivatization A high-performance liquid chromatographic (HPLC) assay for the determination of the R- and S-enantiomers of ketoprofen is described. The derivatization with tbionyl chloride and S-(-)-l-(1-naphthyl)-ethylamine was followed by reversed-phase chromatography with a mobile phase of acetonitrile-water-acetic acid-triethylamine (55 45 0.1 0.02 by vol) at a flow rate of 1.0 mL/min and UV detection was performed at 254 mu. The electrospray ionization-quadrupole ion trap mass spectrometer was applied to verify the structure of derivatives of ketoprofen. The retention times for the S- and R-ketoprofen diastereomeric amides were tR= 7.3 mm and tR? 8.5 nun respectively and had a resolution factor of 1.9. The present study provides a simple, reproducible and sensitive method for the quality evaluation of S-ketoprofen. 2. Enantiospecific analysis of ephedrine by RP-HIPLC with precolumn derivatization A high-performance liquid chromatographic method has been developed for the determination of the (-)- and (+)-enantiomers of ephedrine and the (-)- and (+)-enantiomers of pseudoephedrine simultaneously. The derivatization with (-)-menthylchloroformate was followed by reversed-phase chromatography with a mobile phase of acetonitrile-water-acetic acid-triethylamine (29 20 0.2 0.01 by vol) at a 4 flow rate of 1.0 mL/min and UV detection was performed at 254 nm. The electrospray ioriization-quadnipole ion trap mass spectrometer was applied to verify the structure of derivatives of ephedrine and pseudoephedrine. The retention times for the (-)- and (+)-.ephedrine diastereomeric derivatives were tR= 17.1 and tR= 18.3 mm respectively and have a resolution factor of 1.6. The retention times for the (+)~ and (-)-pseudoephedrine diastereomenc derivatives were tR= 21.3 and tR= 23.2 mm respectively and bad a resolution factor of 1.9. The present study provides a simple, reproducible and rapid method for the quality evaluation of (-)-ephedrine and (+)-pseudoephedrine. 3. Enantiospecific Analysis of Methylephedrine by Normal-Phase HPLC with Precolumn Derivatization A high-performance liquid chromatographic method for the determination of (-)- and (+)-.enantiomers of methylephedrine is reported. The derivatization with (-)-menthyl chloroforniate give two diastereomiric derivatives. These derivatives were separated on a LiCbrosorb Si 60 column using n-hexane-2-propanol-triethylaniine (94 6: 0.02 by vol) as the mobile phase and detected by CV detection at a wavelength of 220 nm. The electrospray ionization-quadrupole ion trap mass spectrometer was applied to verify the structure of derivatives of methylephedrine. The retention times for the (+)- and (-)-methylephedrine diastereomeric derivatives were tR= 3.6 mm and t~=~ 4.3 mm respectively and had a resolution factor of 1.8. The...