School of Pharmacy, Shanxi Medical University, Taiyuan, P. R. China.
Shanxi Provincial Key Laboratory of Drug Synthesis and Novel Pharmaceutical Preparation Technology, Shanxi Medical University, Taiyuan, P. R. China.
J Sep Sci. 2024 Oct;47(19):e202400363. doi: 10.1002/jssc.202400363.
A dispersive liquid-liquid microextraction based on hydrophobic deep eutectic solvent (hDES) was developed for the extraction and quantification of four cinnamic acid derivatives in traditional Chinese medicines coupled with high-performance liquid chromatography-ultraviolet detection. In this method, a hDES (tetrabutylammonium chloride-hexanoic acid, molar ratio of 1:2) was prepared as the extractant. It only took 15 s to handle multiple samples simultaneously by hand-assisted dispersion. The use of a narrow-bore tube reduced the amount of the hydrophobic extractant with easier recovery. The approach was influenced by several key parameters, including the composition and consumption of the DES, sample phase pH, salt amount, extraction time, and centrifugation time, all of which had been investigated and optimized. Moreover, the formation of the DES was characterized by Fourier-transform infrared spectroscopy and differential scanning calorimetry. Under the optimal conditions, enrichment factors of the target analytes ranged from 135 to 220. Satisfactory linearities (r ≥ 0.9977), detection limits (0.2-0.4 ng/mL), precision (<8.5%), and accuracy (recoveries: 90.0%-104.6%) were obtained. The method has been successfully applied to the simultaneous extraction and preconcentration of four cinnamic acid derivatives in Chinese medicinal samples with rapidness, high efficiency, and convenience.
基于疏水型深共晶溶剂(hDES)的分散液液微萃取方法已被开发用于传统中药中四种肉桂酸衍生物的提取和定量分析,结合高效液相色谱-紫外检测法。在该方法中,制备了一种 hDES(四丁基氯化铵-己酸,摩尔比为 1:2)作为萃取剂。通过手动辅助分散,仅需 15 秒即可同时处理多个样品。使用小口径管减少了疏水性萃取剂的用量,更易于回收。该方法受到几个关键参数的影响,包括 DES 的组成和用量、样品相 pH 值、盐量、萃取时间和离心时间,所有这些参数都经过了研究和优化。此外,DES 的形成通过傅里叶变换红外光谱和差示扫描量热法进行了表征。在最佳条件下,目标分析物的富集因子范围为 135-220。获得了令人满意的线性度(r≥0.9977)、检测限(0.2-0.4ng/mL)、精密度(<8.5%)和准确度(回收率:90.0%-104.6%)。该方法已成功应用于中药样品中四种肉桂酸衍生物的同时提取和预浓缩,具有快速、高效、方便的特点。