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. 2024 May 16;29(10):2344.
doi: 10.3390/molecules29102344.

Separation and Detection of Catechins and Epicatechins in Shanxi Aged Vinegar Using Solid-Phase Extraction and Hydrophobic Deep Eutectic Solvents Combined with HPLC

Baoqing Bai  1   2 , Dan Shen  1 , Siyuan Meng  1 , Yanli Guo  1 , Bin Feng  3   4 , Tao Bo  1   5 , Jinhua Zhang  1   2 , Yukun Yang  1   2 , Sanhong Fan  1   2
Affiliations

Separation and Detection of Catechins and Epicatechins in Shanxi Aged Vinegar Using Solid-Phase Extraction and Hydrophobic Deep Eutectic Solvents Combined with HPLC

Baoqing Bai et al. Molecules. .

Abstract

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.

Keywords: Shanxi aged vinegar; catechin; epicatechin; hydrophobic deep eutectic solvent; vortex-assisted solid phase extraction.

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Conflict of interest statement

The authors declare no conflicts of interest.

Figures

Figure 1
Figure 1
The structure of catechins and epicatechins.
Figure 2
Figure 2
The results of the effect of the types of elution solvents (a), the amount of adsorption resin (b), the molar ratio of DES1 (c), the volume of the DES1 (d), adsorption time (e), and desorption time (f).
Figure 3
Figure 3
Pareto chart of the standardized effects in the screening. (a) Catechin. (b) Epicatechin.
Figure 4
Figure 4
Three-dimensional response surface plots and two-dimensional contour plots of HDES-SPE. (a–l) indicate the interactions among the molar ratio of HDES, the amount of the adsorption resin XAD-2, and the adsorption time, respectively.
Figure 5
Figure 5
Normal plot of the residual.
Figure 6
Figure 6
Relationship between the residual and predicted response.
Figure 7
Figure 7
Relationship between the predicted and actual response.
Figure 8
Figure 8
AGREE assessment tool scoring values.
Figure 9
Figure 9
The schematic procedure of the SPE-DES-HPLC.
See this image and copyright information in PMC

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