ABSTRACT
With the in-depth study of related substances and the development of consistency evaluation of generic drugs, relative correction factors are gaining increasing attention. By analyzing the domestic and foreign literature on correction factors in recent years, this paper describes the correction factor component, the current measurement method and its application. The rules and key points of use of an impurity correction factor and its determination and application are described, and some problems in its determination and application are discussed, providing a reference and basis for the standardization of research on impurity correction factors in the future.
ABSTRACT
OBJECTIVE： To establish a UHPLC method for determination of the contents of 11-keto-β-boswellic acid(KAB) and 11-keto-β-acetyl-boswellic acid(AKBA)in Frankincense and explore the suitability and accuracy of substitute reference substance method with DRS origin software for qualitative and quantitative determination of chromatographic peaks. METHODS ：The samples were separated by UHPLC for determination of AKBA and KBA. AKBA was used as a reference to investigate the accuracy of KBA identification using DRS origin software on 19 different C18 columns. The RSDs of relative correction factors were calculated for different detection wavelengths and instruments.The relative correction factor method and the external standard method were selected for quantification and the differences were compared. RESULTS: The established method met the requirements of methodology and the average recovery was 100.21%(n=6) with RSD of 2.47%. The DRS origin software can be used to accurately determine the chromatographic peaks. The correct factor of AKBA vs. KBA was 0.936 and it was consistent under different conditions. There were no significant differences between the content calculated by the relative correction factor method and by the external standard method. CONCLUSION： This method is intelligent, feasible, reliable and economical, and can be used for the determination of frankincense content.
ABSTRACT
OBJECTIVE: To propose a holistic strategy for quality control of Chinese patent medicines, and establish an HPLC analytical method for Tongzhi Surunjiang preparation according to the strategy. METHODS: The strategy contained three steps.The first step was multi-wavelength chromatographic detection.The second step was multivariate analysis for identification and assay. The third step was to establish substitute reference substance method.The preparations were extracted by ultrasound with methanol, chromatography was performed on ODS column with gradient elution with acetonitrile and 0.1%phosphoric acid aqueous solution.The detection wavelengths were set at 270, 350, 410 and 440 nm.The radar chart, HCA heatmap, principal component analysis and cosine similarity were used for data analysis.At last, linear calibration using two reference substances, relative retention time method and PDA spectrum method were used for peak identification, and relative correction factor method was used for quantitative analysis. RESULTS: The multi-components determination method and fingerprint analysis met the method validation requirements. Data analysis showed that there were some differences among the samples of different manufacturers. Strong characteristic peaks for classification were gallic acid, chebulinic acid, chebulea fructus, sennae folium, sennae folium and crocin.CONCLUSION: The method is specific, with low cost, and could be used to accurately control the quality of Tongzhi Surunjiang preparation.
ABSTRACT
Substitute reference substance method is an effective approach for quality control of multiple components in accordance with the characteristics of traditional Chinese medicines. The purpose of the guideline is to guide the establishment of substitute reference substance method, prove the conformance of the method to the requirements for testing, and standardize the study method and its application in national drug standards. The topics of the guideline include the definition and classification of substitute reference substance method, the principles and approaches of quantitative analysis, the identification and confirmation of chromatographic peaks, and technical requirements. When substitute reference substance method is used for fingerprint identification or multiple components assay in traditional Chinese medicines, the analytical method can be validated following the guideline.