School of Life Science, Shanxi University, Taiyuan 030006, China.
Xinghuacun College, Shanxi University, Taiyuan 030006, China.
Molecules. 2024 May 16;29(10):2344. doi: 10.3390/molecules29102344.
This research presents a new, eco-friendly, and swift method combining solid-phase extraction and hydrophobic deep eutectic solvents (DES) with high-performance liquid chromatography (SPE-DES-HPLC) for extracting and quantifying catechin and epicatechin in Shanxi aged vinegar (SAV). The parameters, such as the elution solvent type, the XAD-2 macroporous resin dosage, the DES ratio, the DES volume, the adsorption time, and the desorption time, were optimized via a one-way experiment. A central composite design using the Box-Behnken methodology was employed to investigate the effects of various factors, including 17 experimental runs and the construction of three-dimensional response surface plots to identify the optimal conditions. The results show that the optimal conditions were an HDES (tetraethylammonium chloride and octanoic acid) ratio of 1:3, an XAD-2 macroporous resin dosage of 188 mg, and an adsorption time of 11 min. Under these optimal conditions, the coefficients of determination of the method were greater than or equal to 0.9917, the precision was less than 5%, and the recoveries ranged from 98.8% to 118.8%. The environmentally friendly nature of the analytical process and sample preparation was assessed via the Analytical Eco-Scale and AGREE, demonstrating that this method is a practical and eco-friendly alternative to conventional determination techniques. In summary, this innovative approach offers a solid foundation for the assessment of flavanol compounds present in SAV samples.
本研究提出了一种新的、环保且快速的方法,结合固相萃取和疏水深共晶溶剂(DES)与高效液相色谱(SPE-DES-HPLC),用于提取和定量山西老陈醋(SAV)中的儿茶素和表儿茶素。通过单向实验优化了洗脱溶剂类型、XAD-2 大孔树脂用量、DES 比例、DES 体积、吸附时间和洗脱时间等参数。采用 Box-Behnken 方法的中心组合设计研究了各种因素的影响,包括 17 个实验运行和构建三维响应面图以确定最佳条件。结果表明,最佳条件为 HDES(四乙基氯化铵和辛酸)比例为 1:3,XAD-2 大孔树脂用量为 188mg,吸附时间为 11min。在这些最佳条件下,方法的确定系数大于或等于 0.9917,精密度小于 5%,回收率在 98.8%至 118.8%之间。通过分析生态规模和 AGREE 评估分析过程和样品制备的环保性质,表明该方法是传统测定技术的实用且环保的替代方法。总之,这种创新方法为评估 SAV 样品中黄烷醇化合物提供了坚实的基础。