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%.

Functionalized monolithic columns: Recent advancements and their applications for high-efficiency separation and enrichment in food and medicine

“…They achieved a detection limit and a quantification limit of 0.03 and 0.1 g kg −1 , respectively, which could effectively monitor residual AZI and its analogues in edible animal tissues to reduce their damage to human liver and heart. In recent years, the application of monolithic columns in medicine has increased, as shown in Table 3 (Xiao et al, 2015;Chen et al, 2016;Wang et al, 2018a;Salih et al, 2018;Peng et al, 2020;Andre and Guillaume, 2021;Derazshamshir et al, 2021;Wang L. et al, 2021;Wu F. et al, 2021;Zhao et al, 2021;Ghanem et al, 2022).…”

Polar and nonpolar organic polymer‐based monolithic columns for capillary electrochromatography and high‐performance liquid chromatography

“…Along the above guidelines, a hydrophilic monolithic column has been prepared by postpolymerization functionalization of a GMA‐based monolith . The template monolithic column was first prepared via the in situ polymerization of AM, GMA, MBA, 2‐acrylamido‐2‐methyl‐1‐propane sulfonic acid in a ternary porogen solvent system consisting of cyclohexanol, dodecanol, and toluene.…”