Dynamic changes of volatile components of Qiai from different harvest time based on GC-MS and chemometrics analysis / 中国中药杂志

Artemisiae Argyi Folium, the dried leaves of Artemisia argyi, has been widely used in traditional Chinese and folk medicines for a long time. Qiai is one of the top-geoherb of Artemisiae Argyi Folium. Qiai contains various bioactive constituents, such as volatile oils, phenolic acids, flavonoids and terpenoids. Phytochemical studies demonstrated that volatile compounds are the main bioactive constituents in Qiai. Try to investigate dynamic changes of volatile components of Qiai from different harvest time and explore the optimum harvest time of Qiai, in this study, the contents of total volatile oils in Qiai collected from five different harvest time were analyzed by steam distillation method. The results showed that the contents of volatile oils of Qiai were higher in the third harvest time(around the Dragon Boat Festival), which is basically consistent with the traditional harvest time. Furthermore, a sensitive method based on gas chromatography-mass spectrometry(GC-MS) was established for qualitative analysis of volatile compounds in Qiai, and a total of thirty volatile compounds were identified. Chemometrics methods including principal component analysis(PCA) and orthogonal partial least-squares discriminate analysis(OPLS-DA) were applied to explore chemical markers and dynamic changes of volatile components in Qiai from different harvest time, and the results indicated that there were obvious differences in the relative contents of volatile compounds of Qiai samples from different harvest time. Eight volatile compounds, including α-terpinene, γ-terpinene, D-camphor, trans-carveol, α-copaene, isobornylisobutyrate, humulene, and caryophyllene oxide were selected as potential chemical markers. Among the eight chemical markers, the relative contents of α-terpinene, γ-terpinene, α-copaene and caryophyllene oxide were higher in the third harvest period(around the Dragon Boat Festival), which is consistent with the contents of total volatile oils. The present study could provide the basis for investigating the optimum harvest time of Qiai, and might be useful for the quality control of this herbal medicine.

HPLC fingerprints research on decoction pieces of Citri Reticulatae Pericarpium based on chemometrics methods combined with orthogonal partial least square discriminate analysis / 中草药

Objective To establish an HPLC method for the fingerprints analysis of decoction pieces of tangerine peel, so as to provide reference for the quality control of it. Methods Fingerprints of 17 batches of decoction pieces of tangerine peel were established by HPLC and evaluated by cluster analysis (CA), principal component analysis (PCA) and orthogonal partial least square discriminate analysis (OPLS-DA). Results The method of fingerprint of decoction pieces of tangerine peel was established, the similarities were greater than 0.9. There were 25 common peaks in the HPLC fingerprint, of which variable importance projection (VIP) of 14 peaks were greater than 1. Compared with the spectrogram of reference substances, peak 13 was narirutin, peak 14 was hesperidin, peak 23 was nobiletin, peak 24 was 3,5,6,7,8,3’,4’-heptamethoxy flavone, and peak 25 was hesperetin. Conclusion This simple and reliable method can be used for the identification and quality control of decoction pieces of Citri Reticulatae Pericarpium.

Application of quality by design in granulation process for ginkgo leaf tablet (Ⅱ)： identification of critical quality attributes / 中国中药杂志

Quality by design (QbD) highlights the concept of "begin with the end", which means to thoroughly understand the target product quality first, and then guide pharmaceutical process development and quality control throughout the whole manufacturing process. In this paper, the Ginkgo biloba granules intermediates were taken as the research object, and the requirements of the tensile strength of tablets were treated as the goals to establish the methods for identification of granules' critical quality attributes (CQAs) and establishment of CQAs' limits. Firstly, the orthogonal partial least square (OPLS) model was adopted to build the relationship between the micromeritic properties of 29 batches of granules and the tensile strength of ginkgo leaf tablets, and thereby the potential critical quality attributes (pCQAs) were screened by variable importance in the projection (VIP) indexes. Then, a series of OPLS models were rebuilt by reducing pCQAs variables one by one in view of the rule of VIP values from low to high in sequence. The model performance results demonstrated that calibration and predictive performance of the model had no decreasing trend after variables reduction. In consideration of the results from variables selection as well as the collinearity test and testability of the pCQAs, the median particle size (D₅₀) and the bulk density (Da) were identified as critical quality attributes (CQAs). The design space of CQAs was developed based on a multiple linear regression model established between the CQAs (D₅₀ and Da) and the tensile strength. The control constraints of the CQAs were determined as 170 μm< D₅₀<500 μm and 0.30 g•cm⁻³<Da<0.44 g•cm⁻³ according to the design space, which provided a basis for controlling and optimizing the wet granulation process of the ginkgo leaf tablet..