In this study, a quantitative 1 H NMR method ( 1 H-qNMR) for determining the contents of imperatorin, byakangelicin, and oxypeucedanin in A. dahurica in traditional Chinese medicine (TCM) has been established. Dried plant material was extracted exhaustively with methanol by an ultrasonication-assisted extraction method. e 1 H-qNMR measurements were performed on a 600 -MHz spectrometer with hydroquinone as the internal standard reference in deuterated dimethyl sulfoxide (DMSO-d 6 ) solvent. Quantification was carried out using the 1 H resonance signals at 6.55 ppm for hydroquinone and 7.68, 7.38-7.39, and 6.38-6.39 ppm for imperatorin, byakangelicin, and oxypeucedanin, respectively. e linearity, limit of detection (LOD), limit of quantitation (LOQ), precision, reproducibility, stability, and recovery of the methodology were evaluated, and results were good. e newly developed method has been applied to determine the three coumarins in A. dahurica.
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.
The chemical components and medicinal properties of different medicinal parts of Angelica sinensis are often used as medicine after being divided into the head, body and tail of Angelica sinensis. In this study, the chemical components of different medicinal parts in different periods were analyzed by GC-MS for the first time, and the differences of the accumulation rules of chemical components in different medicinal parts of Angelica sinensis were obtained. This study demonstrated that the differences of composition accumulation in different medicinal parts of Angelica sinensis were mainly reflected in the types and relative contents of compounds. The study found that the number of compounds in different medicinal parts of Angelica sinensis in each period were different and the change rules of the same compound in different medicinal parts were also different. The number of compounds in the tail of Angelica sinensis was the least in April, and the largest in October. The content of ligustilide in the body of Angelica sinensis was higher in April and was the highest in the tail in October. The relative content of butylidenephthalide in the head was the highest in October. The relative contents of senkyunolide A and butylphthalide in the head were decreased in October, while the contents in the body and tail increased, indicating that the compounds that accumulate in the head may transfer to the body and tail in later stages of growth. This study clarified the differences in the accumulation of chemical components in different medicinal parts of Angelica sinensis, which could provide a theoretical basis for the reasons for the differences of chemical components in the different medicinal parts.
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