Matrix-Assisted ¹H DOSY Applied to Flavonoid Analysis in <i>Scutellaria baicalensis</i>

Abstract

Matrix-assisted diffusion-ordered spectroscopy (MA DOSY) technology enables efficient the virtual separation of components in a mixture according to their coefficients (D). In the current research, MA DOSY technology was applied for the analysis of a flavonoid mixture. To establish the method, five representative active flavonoid ingredients, including baicalein, baicalin, quercetin, puerarin and rutinum, were selected for the mixture model. The effects of the type and concentration of the matrix, solvent polarity, and nuclear magnetic resonance (NMR) experimental conditions on the resolution of the DOSY spectrum were investigated. It turned out that sodium dodecyl sulfate (SDS) showed the best performance in increasing the resolution of different analytes, which initially increased to the peak below the added amount of 9 mg, and decreased upon the addition of more SDS. In addition, the five flavonoids showed higher resolution in DMSO–d6 than in MeOD. Experimental parameters of DOSY, including the number of scans (NS), dummy scans (DS), and value of the FID data points (TD), were also optimized. Finally, the above optimized method was used for the qualitative analysis of the total flavonoid mixture extracted from Scutellaria baicalensis Georgi. A total of nine compounds were identified and confirmed by comparing them with mass spectrometry data, which further verifies the practical value of this method upon analyzing flavonoid mixtures and provides some reference significance for the follow-up research.

Keywords

• NMR
• MA-DOSY
• flavonoids
• mixture separation