OBJECTIVE To establish the HPLC fingerprints, determine the contents of chlorogenic acid, liquiritin, lobetyolin, liquiritigenin, glycyrrhetinic acid, atractylenolide Ⅲ, atractylenolide Ⅱ, atractylenolide Ⅰ, 10-gingerol in Lizhong Pills, and lay the foundation for its quality control. METHODS A Eclipse Plus C₁₈ column was used with acetonitrile-0.1% aqueous phosphoric acid as the mobile phase in gradient elution at a flow rate of 0.8 mL·min^-1. The detection wavelengths were set at 215 nm and 254 nm, and the column temperature was maintained at 30 ℃. Through similarity evaluation, combined with chemical pattern recognition, the fingerprints of 21 batches of Li Zhong Pills were evaluated and analyzed, and 9 index components were quantitatively determined. RESULTS The fingerprints of 21 batches of Lizhong Pills were established, with 29 peaks identified, the similarity of each batch was greater than 0.9, and 21 batches of samples from 3 manufacturers could be clustered into 3 categories, with 16 compounds differing between groups. Nine components showed good linear relationships within their respective linear ranges (r≥0.998 7), the average recoveries ranged from 95.34% to 104.41%, and the RSDs ranged from 0.95% to 2.95%. CONCLUSION The fingerprint and quantitative determination method of Lizhong Pills is simple, accurate and reproducible, and can be used for the evaluation of the overall quality of Lizhong Pills.

OBJECTIVE To develop a method for the determination of dracorhodin in Draconis Sanguis scald ointment based on the concept of quality by design (QbD), and to study its preparation process for quantitative transfer. METHODS Using the content of dracorhodin as key quality attribute, the key analytical parameters in preparation of test solution were selected through Plackett-Burman design. The relationship between key quality attribute and key analysis parameters was evaluated through Box-Behnken design. According to characteristics of the medicinal material, intermediate and finished product of scald ointment, the different methods for determining content of dracorhodin were established, and the law of quantity transfer was studied. The preparation conditions of test solution for content determination of Draconis Sanguis scald ointment were as follows: lanolin was removed by petroleum ether, extraction solvent was 7% phosphoric acid methanol solution, and extraction was carried out in a water bath at 60 ℃ for 30 min. The chromatographic conditions were as follows: the mobile phase was consisted of acetonitrile and 0.05 mol·L^-1 sodium dihydrogen phosphate solution using a gradient elution. Temperature was 40 ℃ and flow rate was 1.0 mL·min^-1, at a detector wavelength of 440 nm. RESULTS The feasibility of preparation process of Draconis Sanguis scald ointment was proven. The transfer rate of dracorhodin from medicinal material to finished product was over 90%. CONCLUSION The analytical method developed based on concept of QbD could accurately determine content of dracorhodin in Draconis Sanguis scald ointment, which is conducive to product quality evaluation and process value transfer research.

OBJECTIVE To analyze the characteristics and drug cost of hepatoprotective drugs among outpatients in domestic hospitals and provide references for rational drug use. METHODS The outpatient prescription data of 119 hospitals in 9 cities from January 2016 to December 2023 was collected, and the clinical application of hepatoprotective drugs was analyzed. RESULTS A total of 8 635 977 prescriptions from 3 194 167 patients were obtained in this study. The most frequent diagnoses of hepatoprotective drugs were hepatitis B (7.59%), liver cirrhosis (5.11%) and non-alcoholic steatohepatitis (4.53%).98.15% of prescriptions for 1-2 hepatoprotective drugs are prescribed, and oral dosage forms account for 97.29%. The total drug cost of hepatoprotective drugs increased from 85.38 million yuan to 109.8 million yuan, and the average drug cost per time increased from 85.15 yuan to 95.52 yuan. The glycyrrhizin preparation was the most used regimen, and the polyene phosphatidylcholine+glycyrrhizin preparation was the most used regimen. CONCLUSIONS The aggregate costs on hepatoprotective medications appears a consistent annual increase, which brings economic burden to medical insurance. This study analyzes the trend of hepatoprotective drug costs in the past 8 years, which is of great significance to the drug management of patients with liver disease.

OBJECTIVE To develop the limited standard and supporting detection methods of commonly used pesticides in Lycium barbarum L. (L. barbarum). METHODS In previous research, the “the Principle of Conversion of Limit Standards of Traditional Chinese Medicine in <GB 2763 national food safety standard-maximum residue limits for pesticides in food>” have been drafted. In this research, the L. barbarum was used as the research object to study the conversion scope, risk assessment, detection methods and conversion judgment principle. RESULTS A method for the determination of 13 pesticide residues in the L. barbarum was established by using acetonitrile extraction and HLB column purification. And the GC-MS/MS and LC-MS/MS technology were used to detect the pesticide residues. In addition, the maximum residue limit of 13 pesticides in L. barbarum was finally formulated by sample determination. CONCLUSION The specific implementation steps are provided for the conversion of GB 2763 standard to traditional Chinese medicine standard in this study, and it is of great significance for promoting the connection between planting and circulation supervision of L. barbarum.

OBJECTIVE To screen the commonly used pesticides in Dendrobium officinale to understand their pesticide residues, and explore the establishment of a method for determining the transformation of pesticide residues in Dendrobium officinale and the development of limit standards in accordance with the requirements of GB 2763 Food Safety Standards for Maximum Residue Limits of Pesticides in Food and the Chinese Pharmacopoeia. METHODS LC-MS/MS methods were used to screen and risk assess 6 transformation pesticides in 53 batches of Dendrobium officinale, and the pesticide registration status and the maximum residue limit standards for Dendrobium officinale (dry) in GB 2763 were used to determine the indicators for the transformation of pesticides. RESULTS The pesticides in 53 batches of Dendrobium officinale were analyzed. The transformation pesticide were confirmed in accordance with GB 2763 and the requirements of the Chinese Pharmacopoeia 2020 Edition, and a method for determining the transformation of pesticide residues in Dendrobium officinale was established, along with the development of limit standards. CONCLUSION This study screened 40 commonly used pesticides and 6 transformation in 53 batches of Dendrobium officinale, established a method for determining the transformation of pesticide residues in accordance with GB 2763, and developed limit standards. This study is helpful for understanding the risk of pesticide residues in Dendrobium officinale, regulating the use of pesticides during its cultivation process, and improving its quality standards.

OBJECTIVE To establish a method for the transformation of some commonly used pesticide limit standards in Chrysanthemi Flos based on ‘GB 2763 National Food Safety Standard-Maximum Residue Limits for Pesticides in Food’. METHODS The indexes of Chrysanthemi Flos (dry) in GB 2763 were sorted out, and the quasi-transformation pesticides were determined as pymetrozine, imidacloprid, boscalid and fluazinam according to the transformation principle. The UPLC-MS/MS method was used to establish the transformation method of Chrysanthemi Flos, and the methodological verification was carried out. RESULTS The four pesticides had good linear relationship in the range of 1-50 ng·mL^-1, the correlation coefficients were 0.999 9, the average recovery was 77.9%-95.5%, and the RSD was 1.7%-6.8%. The overall detection rate of the samples was 60%, and the pesticide with the highest detection rate was imidacloprid. The maximum detectable amount was 1 mg·kg^-1 (imidacloprid), and the results did not exceed the maximum residue limit specified in GB 2763. The risk assessment system of pesticide residues in traditional Chinese medicine was used to evaluate the chronic risk of the four pesticide limit values to be transformed. The results showed that the chronic risk of fluazinam was greater than 1, and the chronic risk quotients of the other three pesticides were less than 1. Therefore, fluazinam is not converted temporarily, and only pymetrozine, imidacloprid and boscalid are converted. CONCLUSION The three limit standards of pymetrozine, imidacloprid and boscalid in Chrysanthemi Flos were transformed. The established limit standard transformation method is simple and accurate, which is of great significance for standardizing the use of pesticides and medicinal safety in the process of chrysanthemum planting.

OBJECTIVE To establish a method for simultaneous determination of registered pesticides, prohibited pesticides, and proposed new prohibited pesticide residues in Fritillaria Medicinal Herbs, and propose reference limits. METHODS The detection method for 95 pesticide residues in Fritillaria Medicinal Herbs was established using GC-MS/MS and LC-MS/MS. The prepared samples were extracted with acetonitrile and then purified with the QuEChERs method. A total of 70 batches of samples were detected by the established method. RESULTS According to the GB 2763 conversion guidelines, imidacloprid and avermectin in Fritillaria Medicinal Herbs should be converted to the maximum residue limit (MRL) standards. Additionally, reference limit values are proposed for the 18 prohibited pesticides that were previously suggested for addition. CONCLUSION The study of Fritillaria Medicinal Herbs aims to offer guidance and inspiration for the transformation of traditional Chinese medicine standards and the expansion of the list of banned pesticides. It also provides a reference for the regulatory policies and technological advancements related to pesticide residue management in Fritillaria Medicinal Herbs and other traditional Chinese medicines.

OBJECTIVE To carry out screening of pesticide residues in Panax notoginseng for the pesticide residues commonly used in Panax notoginseng,understand the pesticide residues situation and carry out the related risk assenssment study. METHODS GC-MS/MS and LC-MS/MS methods were used to establish detection methods for commonly used pesticides in Panax notoginseng, as well as those regulated by laws and regulations; the methods were used to conduct a comprehensive screening and risk assessment of the collected Panax notoginseng samples; and the indexes of the transformed pesticides were confirmed in accordance with the pesticide residue limits of Panax notoginseng in the GB 2763 standard. RESULTS In this study, the residue determination methods for about 40 commonly used pesticides and pesticides regulated by regulations in Panax notoginseng were successfully established, and the corresponding limits were set according to the GB 2763 standard. Eight pesticides including tebuconazole, phenyl ether metronidazole and carbendazim were finally recognized as transformed pesticide indicators. CONCLUSION The pesticide residue detection method for Panax notoginseng established in this study is characterized by simple and rapid operation, high specificity and high sensitivity, and the related risk assessment and limit setting provide technical support for the improvement of the quality standard of Panax notoginseng.

In recent years, in the process of drug research and development, insoluble drugs are faced with the problem of low bioavailability and poor absorption effect. Drug nanocrystals have attracted much attention due to their nano size and unique physical and chemical properties, which can effectively increase drug solubility and permeability, and have advantages such as low dosage of excipients, high drug load and few adverse reactions. However, instability limits their further development. Multieffect stabilizers can significantly improve their stability through steric hindrance, electrostatic repulsion and solvation. The author reviews the main characteristics and limitations of drug nanocrystals, the classification of multi-effect stabilizers and their applications in vivo and in vitro by reviewing and sorting out relevant literature, in order to provide reference for the research and development of drug nanocrystals.

OBJECTIVE To develop and validate a peptide mapping method of an anti-CD33 monoclonal antibody. METHODS Different types of chromatographs (HPLC, UPLC) and different mobile phase systems (formic acid, trifluoroacetic acid) were used for peptide map detection of anti-CD33 antibody. The signature peptide segments were localized using synthetic CDR peptide of the antibody and the localization results were confirmed by mass spectrometry. Based on the relative retention time (RRT), the specificity, precision, and robustness of the method were validated according to the Pharmacopoeia of the People's Republic of China (ChP, 2020). RESULTS The separation time of the peptides by UPLC was shorter than that by HPLC, and the degrees of separation with trifluoroacetic acid in the mobile phase were higher than that with formic acid. The identification results of the signature peptide segment using the maps of synthetic peptide segments were consistent with the results of mass spectrometry. The specificity validation demonstrated that the formulation blank and sample solution blank did not interfere with the detection of signature peptide segments, and there were significant differences between peptide mapping results of different antibodies. The repeatability validation showed that the RSDs (RRT) of signature peptide segments between six parallel samples were 0.01%-0.05%; the intermediate precision validation proved that the RSDs (RRT) of signature peptide segments for different analysts were 0.04%-0.32%; the robustness validation exhibited that the RSDs (RRT) of signature peptide segments were 0.02%-0.09% under different enzyme treatment conditions and 0.36%-1.43% under different chromatographic conditions. Within 25 h in detection, the RSDs (RRT) of the signature peptide segments were 0.01%-0.04%. CONCLUSION This study uses synthetic peptide segments for peptide localization in peptide mapping detection and uses relative retention time to determine the results, which provide a new approach for biopharmaceutical peptide mapping detection.