School of Pharmacy, Shanxi Medical University, Taiyuan, P. R. China.
J Sep Sci. 2024 Jan;47(1):e2300796. doi: 10.1002/jssc.202300796.
In this study, a hydroxyl-rich ferrofluid was prepared by dispersing silica-coated magnetic nanoparticles into a methyltrioctylammonium chloride-glycerol deep eutectic solvent and then employed in the preconcentration of trace-level of cinnamic acid derivatives (caffeic acid, p-hydroxycinnamic acid, ferulic acid, and cinnamic acid) in traditional Chinese medicine prior to high-performance liquid chromatography analysis. The structures of the synthesized materials were characterized by X-ray diffraction and infrared spectroscopy. The experimental parameters affecting the extraction performance, such as deep eutectic solvent composition, dosage of ferrofluid, pH of aqueous sample solution, salt concentration, extraction time, type, and volume of desorption solvent, were studied and optimized. Under the optimum conditions, the enrichment factors of four cinnamic acid derivatives were in the range of 107-114. Low detection limits (0.2-0.9 ng/mL), good precisions (relative standard deviations 1.2%-9.5%), and satisfactory recoveries (96.0%-104.7%) were achieved. Subsequently, the possible microextraction mechanism of the proposed method was explored and elucidated. It showed that the prepared ferrofluid is easily dispersed in the aqueous sample and achieved recovery after the extraction. The developed approach is a simple, convenient, and efficient method for preconcentration and determination of cinnamic acid derivatives in complex matrices.
在这项研究中,通过将硅涂层磁性纳米粒子分散在甲基三辛基氯化铵-甘油深共晶溶剂中,制备了富含羟基的磁性纳米流体,并将其用于高效液相色谱分析前,对中药中痕量肉桂酸衍生物(咖啡酸、对羟基肉桂酸、阿魏酸和肉桂酸)进行预浓缩。通过 X 射线衍射和红外光谱对合成材料的结构进行了表征。研究并优化了影响萃取性能的实验参数,如深共晶溶剂组成、磁性纳米流体用量、水相样品溶液 pH 值、盐浓度、萃取时间、解吸溶剂的类型和体积。在最佳条件下,四种肉桂酸衍生物的富集因子在 107-114 范围内。检测限低(0.2-0.9ng/mL)、精密度好(相对标准偏差 1.2%-9.5%)、回收率令人满意(96.0%-104.7%)。随后,探讨并阐明了所提出方法的可能微观萃取机制。结果表明,所制备的磁性纳米流体易于分散在水相样品中,并在萃取后实现了回收。该方法是一种简单、方便、高效的用于复杂基质中肉桂酸衍生物预浓缩和测定的方法。