Introduction: Citri Reticulatae Pericarpium Viride (Qing Pi in Chinese) is a clinically effective Chinese herb, which contains biologically valuable flavonoids. Qing Pi is divided into two commodity specifications, Si Hua Qing Pi (SHQP) and Ge Qing Pi (GQP), based on the harvesting time. The flavonoid contents in Qing Pi from different origins and commodity specifications may vary significantly, which will affect their therapeutic functions. Thus, it is crucial to set up a reliable and comprehensive quality evaluation method for flavonoid analysis in Qing Pi.Objectives: We aimed to establish a rapid and sensitive ultrahigh-performance liquid chromatography method coupled with diode-array detection and high-resolution mass spectrometry (UPLC-DAD-HRMS) for identification and quantification of ten flavonoids in Qing Pi. Chemometric methods were further applied to distinguish Qing Pi of different origins and specifications.Methodology: An UPLC-DAD-HRMS method was developed for the simultaneous separation and quantification of ten flavonoids in 46 batches of Qing Pi samples from different sources in China. Chemometric approaches were applied to discriminate Qing Pi from different origins and commodity specifications.Results: The chemometric procedures (i.e., hierarchical clustering analysis and principal component analysis) were employed to identify the differences of Qing Pi samples with different origins and commodity specifications. The results showed that the contents of ten flavonoids in Qing Pi samples of different origins were significantly different, and the same results were found out between SHQP and GQP.
Conclusions:This study provides a chemical basis for quality control of Qing Pi.
Introduction: Aurantii Fructus Immaturus (Zhishi in Chinese) is the dried young fruit of Citrus aurantium L. (CA) and its cultivated varieties or Citrus sinensis Osbeck (CS).The content of flavonoids in different varieties of Zhishi may be significantly different. However, there is confusion about the botanical origin of Zhishi, and there is no reliable and systematic method to control Zhishi quality.Objectives: We aimed to establish an ultrahigh-performance liquid chromatography method coupled with diode-array detection and high-resolution tandem mass spectrometry (UPLC-DAD-HRMS/MS) for the quantitative analysis of 10 flavonoids in Zhishi that could be used for quality control and botanical origin identification.Methodology: A UPLC-DAD-HRMS/MS method was established for simultaneous identification and quantification of 10 flavonoids. Separation was performed on a Waters Acquity UPLC HSS T3 column (100 mm  2.1 mm, 1.8 μm) with 0.1% formic acid and acetonitrile as mobile phase under gradient elution. MS was performed in positive and negative ionisation modes. The flavonoids in 41 batches were isolated and quantified. Zhishi of different botanical origins were identified by chemometrics.
Results:The results showed that the established method for the determination of 10 components was reliable and accurate. Chemometrics could be used to distinguish Zhishi of different botanical origins. There were significant differences in the contents of 10 flavonoids in samples of different botanical origins.
In this study, we established a comprehensive high‐performance liquid chromatography coupled with diode array detection and high‐resolution mass spectrometry method to identify 10 and quantified eight constituents in Corydalis Decumbentis Rhizoma (“Xiatianwu” in Chinese) and Corydalis Rhizoma (“Yanhusuo” in Chinese). Chemometric methods were applied to distinguish the botanical origins of the Xiatianwu and Yanhusuo samples. Chromatographic separation was achieved using an Agilent Poroshell EC‐C18 column with mobile phases A (1000 ml of 0.2% acetic acid solution containing 2.8 ml of triethylamine) and B (acetonitrile) and stepwise gradient elution. The analytical method was fully validated in terms of linearity, sensitivity, intra‐ and interday precision and repeatability, the limit of detection, the limit of quantitation, and recovery. Twenty‐six Xiatianwu samples and 10 Yanhusuo samples were analyzed for quality evaluation. In addition, hierarchical clustering analysis and principal component analysis were used to discriminate among samples of different botanical origins. The results showed that the contents of eight alkaloids in Xiatianwu and Yanhusuo were significantly different. Moreover, it was found that chemometric methods could be applied to accurately distinguish these two often conflated Chinese medicinal materials. In conclusion, this study provides a relatively comprehensive method for botanical origin identification and Xiatianwu and Yanhusuo quality control.
Astragali Radix (Huangqi) is an important herb medicine that is always processed into pieces for clinical use. Many operations need to be performed before use, among which drying of Astragali Radix (AR) pieces is a key step. Unfortunately, research on its drying mechanism is still limited. Low-field nuclear magnetic resonance (LF-NMR) and magnetic resonance imaging (MRI) techniques were applied to study the moisture state and distribution during drying. The content of bioactive components and texture changes were measured by HPLC and texture analyzer, respectively. The moisture content of the AR pieces decreased significantly during drying, and the time to reach the drying equilibrium were different at different temperatures. The time when at 70°C, 80°C, and 90°C reach complete drying are 180 min, 150 min and 120 min, respectively. 80°C was determined as the optimum drying temperature, and it was observed that the four flavonoids and astragaloside IV have some thermal stability in AR pieces. When dried at 80°C, although the total water content decreased, the free water content decreased from 99.38% to 15.49%, in contrast to the increase in bound water content from 0.62% to 84.51%. The texture parameters such as hardness changed to some extent, with the hardness rising most significantly from 686.23 g to 2656.67 g. Correlation analysis revealed some connection between moisture content and LF-NMR and texture analyzer parameters, but the springiness did not show a clear correlation with most parameters. This study shows that HPLC, LF-NMR, MRI, and texture analyzers provide a scientific basis for elucidating the drying principles of AR pieces. The method is useful and shows potential for extension and application; therefore, it can be easily extended to other natural herb medicines.
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