title: Preparation of a new chiral stationary phase for HPLC based on the (R)- 1-phenyl-2-(4-methylphenyl)ethylamine amide derivative of (S)-valine and 2-chloro-3,5-dinitrobenzoic acid: enantioseparation of amino acid derivatives and pyrethroid insecticides.
abstract: A novel chiral stationary phase (CSP) for HPLC was prepared by bonding (R)-1-phenyl-2-(4-methylphenyl)ethylamine amide derivative of (S)-valine to aminopropyl silica gel through a 2-amino-3,5-dinitro-1-carboxamido-benzene unit. The CSP was used for the separation of some amino acid derivatives and pyrethroid insecticides by chiral HPLC. Satisfactory baseline separation required optimization of the variables of mobile phase composition. Use of dichloromethane as modifier in the mobile phase gave baseline separations of amino acid derivatives. The two enantiomers of fenpropathrin and four stereoisomers of fenvalerate were baseline separated using hexane-dichloromethane-ethanol as mobile phase. The results show that the enantioselectivity of the new CSP is better than Pirkle type 1-A column for these compounds. Only partial separations were observed for the stereoisomers of cypermethrin and cyfluthrin, which gave even and eight peaks, respectively.
authors.affiliation: Department of Applied Chemistry, College of Science, China Agricultural University, Yuanmingyuan West Road 2, Beijing 100094, PR China.
authors.forename: Xulin
authors.initials: X
authors.lastname: Tan
authors.forename: Shicong
authors.initials: S
authors.lastname: Hou
authors.forename: Jingli
authors.initials: J
authors.lastname: Jiang
authors.forename: Min
authors.initials: M
authors.lastname: Wang
mesh_terms: D001565:Benzoates / Q000032:analysis*; D002623:Chemistry Techniques, Analytical / Q000379:methods; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D007306:Insecticides / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification*; D009682:Magnetic Resonance Spectroscopy; D008694:Methamphetamine / Q000031:analogs & derivatives* / Q000032:analysis; D008752:Methylene Chloride / Q000032:analysis / Q000302:isolation & purification; D008956:Models, Chemical; D009570:Nitriles / Q000032:analysis / Q000302:isolation & purification; D011722:Pyrethrins / Q000032:analysis / Q000302:isolation & purification; D015203:Reproducibility of Results; D013055:Spectrophotometry, Infrared; D013237:Stereoisomerism; D013997:Time Factors
chemical_list: D001565:Benzoates; D007306:Insecticides; D009570:Nitriles; D011722:Pyrethrins; C027141:N-methylphenethylamine; C017160:cypermethrin; D008694:Methamphetamine; D008752:Methylene Chloride; C052570:cyfluthrin