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Introduction: Despite numerous successful cases, there are still some challenges in using analytical quality by design (AQbD) for the development of analytical methods. Knowledge organization helps to enhance the objectivity of risk assessment, reduce the number of preliminary exploratory experiments, identify potential critical method parameters (CMPs) and their scope. Objective: In the present study, we aimed to develop a simple, rapid, and robust analytical method for detecting phenolic compounds in Xiaochaihu capsule intermediates utilizing knowledge organization. Methods: Knowledge organization and AQbD were combined to obtain the initial analytical conditions through knowledge collection, extraction, reorganization, and analysis. The quantitative relationship between critical method attributes (CMAs) and CMPs was then established by a definitive screening design. The method operable design region was calculated using an exhaustive Monte Carlo approach based on the probability of reaching the standard. Robustness investigation and methodological validation were finally performed. Results: Analytical target profiles, CMAs, potential CMPs, and initial analytical conditions were initially identified, and the optimized ranges of operating parameters were obtained. A UHPLC method was successfully established for the analysis of phenolic compounds in ginger–ginger pinellia percolate, and the method validation outcomes were also satisfactory. Conclusion: The developed method can be a reliable means to detect the phenolic compounds of Xiaochaihu capsule intermediates. Knowledge organization provides a new approach for making better use of prior knowledge, significantly enhancing the efficiency of analytical method development. The approach is versatile and can be similarly applied to the development of other methods. This study employed an AQbD process based on knowledge organization to develop an analytical method for detecting phenolic compounds in Xiaochaihu capsule intermediate, improving the efficiency of conducting single‐factor experiments and identifying potential CMPs in the early stage of method development. Simultaneously, it offers a new approach for utilizing prior knowledge effectively. This analytical method can be used for quality control of intermediate in Xiaochaihu capsule. [ABSTRACT FROM AUTHOR]

In this study, we analyzed the components of Mentha spp. essential oils (EOs) and evaluated their major constituents and binary combinations against Reticulitermes dabieshanensis. We also determined the activities of esterases (ESTs), glutathione S-transferases (GSTs), and acetylcholinesterase activity (AChE) in treated insects. According to our findings, the most effective oils were those obtained from M. citrata (with the major constituent linalool constituting 45.1%), M. piperita (menthol, 49.1%), and M. spicata (carvone, 69.0%), with LC50 values of 0.176, 0.366, and 0.146 μL/L, respectively. The LC50 values were recorded for linalool (0.303 μL/L), followed by menthol (0.272 μL/L), and carvone (0.147 μL/L). The insecticidal potency increased with binary mixtures of major active constituents, with carvone strongly synergizing the toxicity of linalool and menthol against R. dabieshanensis. Compared to the control, except for M. citrata treated with no difference in α-NA or GST activity, the activities of ESTs and GST in other treatment groups were significantly increased. Additionally, our results found that Mentha spp. EOs and their major constituents inhibited the activity of AChE in vivo and in vitro. Finally, we performed a structure-based virtual screening of linalool, menthol, and carvone to identify that linalool had the greatest potential to bind to the active site of AChE. The present study suggests that Mentha spp. EOs could provide an additional approach for the management of termites over synthetic insecticides. [ABSTRACT FROM AUTHOR]

Background: Xiaochaihu capsule is composed of seven traditional Chinese medicines. The pharmacopoeia only focuses on the quantitative detection of baicalin, which cannot fully reflect the quality of the preparation. Some medium polar components were used to establish the fingerprint of Xiaochaihu capsule, but there was no report on the strong polar components. Methods: A high performance liquid chromatography-corona charged aerosol detection technology was used to establish a fingerprint analysis method for Xiaochaihu capsules following an analytical quality by design approach. Definitive screening designed experiments were used to optimize the method parameters. A stepwise regression method was used to build quantitative models. The method operable design region was calculated using the experimental error simulation method. Plackett–Burman designed experiments were carried out to test robustness. Results: The contents of four components were simultaneously determined. There were seven common peaks in the fingerprint. The common peak area accounted for 91.72%. Both fingerprint and quantitative analysis methods were validated as applicable in the methodology study. The quantitative fingerprint analysis method for sugar components can fill the gap in the detection of strong polar components in the existing methods. It provides a new technology for the comprehensive overall evaluation of Xiaochaihu capsule. [ABSTRACT FROM AUTHOR]