title: Simultaneous Determination of Five Alkaloid Compounds in a Drug Based on a Hydrophilic Monolithic Column by Capillary Electrochromatography.
abstract: A novel capillary electrochromatography (CEC) method was developed by using a hydrophilic monolithic column for the simultaneous determination of five alkaloids in a drug. The monolithic stationary phase was first prepared via in situ polymerization of acrylamide (AM), glycidyl methacrylate (GMA), N,N'-methylenebisacrylamide (MBA) and 2-acrylamido-2-methyl-1-propane-sulfonic acid (AMPS) in a ternary porogen solvent system consisting of cyclohexanol, dodecanol and toluene. The obtained monolithic stationary phase was subsequently modified by 0.1 mol/L ammonia water for opening epoxide groups of GMA. The separation performance and efficiency of the resulting monolithic column were investigated by the use of five compounds (thiourea, aniline, naphthylamine, diphenylamine and dimethyl acetamide) by CEC. The optimized monolithic column has obtained high column efficiencies with 74,000-121,000 theoretical plates/m. Finally, the prepared monolithic column was used to separate and determine five alkaloids (piperine, nuciferine, kukoline, berberine and tetrandrine) using CEC. Under the conditions of acetonitrile/10 mM phosphate buffer solution (65/35, v/v, pH 8.5) and 15 kV applied voltage, the baseline separation of five alkaloids was achieved. The proposed method has been successfully applied to the determination of berberine in a tablet sample. The percentage of recovery of spiked tablet samples ranged from 93.4 to 108.0% with relative standard deviations (RSDs) <9.20%.
authors.affiliation: Key Laboratory of Applied Organic Chemistry, College of Jiangxi Province, Department of Chemistry, Shangrao Normal University, Shangrao, Jiangxi 334001, PR China Ministry of Education Key Laboratory of Analysis and Detection for Food Safety, Fuzhou University, Fuzhou, Fujian 335002, PR China chenzongbao19780920@126.com.
authors.forename: Zongbao
authors.initials: Z
authors.lastname: Chen
authors.affiliation: Key Laboratory of Applied Organic Chemistry, College of Jiangxi Province, Department of Chemistry, Shangrao Normal University, Shangrao, Jiangxi 334001, PR China.
authors.forename: Qing
authors.initials: Q
authors.lastname: Ye
authors.affiliation: Key Laboratory of Applied Organic Chemistry, College of Jiangxi Province, Department of Chemistry, Shangrao Normal University, Shangrao, Jiangxi 334001, PR China.
authors.forename: Linghai
authors.initials: L
authors.lastname: Liu
authors.affiliation: Key Laboratory of Applied Organic Chemistry, College of Jiangxi Province, Department of Chemistry, Shangrao Normal University, Shangrao, Jiangxi 334001, PR China.
authors.forename: Hongxia
authors.initials: H
authors.lastname: Dong
mesh_terms: D000470:Alkaloids / Q000032:analysis*; D002021:Buffers; D053801:Capillary Electrochromatography / Q000379:methods*; D006863:Hydrogen-Ion Concentration; D057927:Hydrophobic and Hydrophilic Interactions; D008855:Microscopy, Electron, Scanning; D015203:Reproducibility of Results
chemical_list: D000470:Alkaloids; D002021:Buffers