The Use of 1H-qNMR Method for Simultaneous Determination of Osthol, Columbianadin, and Isoimperatorin in Angelicae Pubescentis Radix

2020 
OBJECTIVE The goal of this work was to establish a method to identify and quantify the main active components in Angelicae Pubescentis Radix (APR) quickly, simply, and accurately. This paper reports a novel method which can determine osthol, isoimperatorin, and columbianadin using 1H-qNMR simultaneously and quantitatively. METHODS In comprehensive consideration of resolution of target signals and the solubility of materials, dimethyl sulfoxide-d6 (DMSO-d6) was selected as an optimal 1H-qNMR solvent and pyrazine was used as internal standard substance (δ8.66 ppm). The quantitative peaks of three active components were determined using specific 1H resonances at δ7.54-7.56 ppm for osthol, δ6.83-6.85 ppm for columbianadin, and δ6.31-6.32 ppm for isoimperatorin. RESULTS The results show that the method has good precision, stability, and repeatability. The content of APR plant material from Huating is 9.8 mg/g, 5.6 mg/g, and 15.6 mg/g for osthol, columbianadin, and isoimperatorin, respectively. Furthermore, the experimental process is simple and the test time is short (1 min). CONCLUSIONS The proposed quantitative 1H-qNMR methodology can be used for the quality control of APR.
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