ABSTRACT
OBJECTIVE To establish the method for the content determination of ephedrine hydrochloride and pseudoephedrine hydrochloride in Shexiang zhuanggu plaster ，and to evaluate the quality of 222 batches of Shexiang zhuanggu plaster from 41 manufacturers. METHODS HPLC method was established. The determination was performed on Shimadzu Shim-pack GIS-C 18 column with mobile phase consisted of acetonitrile- 0.1％ phosphoric acid （3∶97，V/V）at the flow rate of 0.9 mL/min. The column temperature was set at 30 ℃，the detection wavelength was 210 nm，the sample size was 10 μL. Taking the content data of 222 batches of samples as index ，the cluster heatmap was drawn by Hiplot biomedical data visualization and analysis platform. RESULTS The results of the methodological investigation were in line with the requirements of the general principles stated in 2020 edition of Chinese Pharmacopoeia （part Ⅳ ）. The total contents of ephedrine hydrochloride and pseudoephedrine hydrochloride in 222 batches of samples from 41 manufacturers were 0.646-6.325 μg/cm2. Results of cluster heatmap analysis showed that these samples of 41 manufacturers could be divided into 3 categories. The contents of components in samples from different manufacturers varied greatly ，and the contents of components in different batches of samples from the same manufacturers also varied greatly. If the proposed limit of this product was that the total amount of ephedrine hydrochloride and pseudoephedrine hydrochloride per 1 cm2 would not be less than 1.00 μg，23 of the 222 batches of samples were unqualified. CONCLUSIONS The established method for the content determination of ephedrine hydrochloride and pseudoephedrine hydrochloride in Shexiang zhuanggu plaster is accurate and precise ，and can be used for the quality control. Some manufacturers should pay attention to optimizing production process and strengthening quality control.
ABSTRACT
OBJECTIVE：To identify t he chemical constituents of Fengliaoxing fengshi dieda wine. METHODS ：An ultra-high performance liquid chromatography-quadrupole-electrostatic field orbital trap high-resolution mass spectrometry （UPLC-Q-Exactive- MS）technique was used for identifying chemical constituents of Fengliaoxing fengshi dieda wine. The determination was performed on Thermo Accucore aQ RP 18 column with mobile phase consisted of 0.1％ formic acid-methanol （gradient elution ）at the flow rate of 0.3 mL/min. The column temperature was 30 ℃，and the sample size was 2 μL. HESI source was adopted，ion mode was positive and negative ion mode ，nitrogen as sheath gas and auxiliary gas. The positive ion mode had spray voltage of 3.5 kV， capillary heating temperature of 350 ℃，sheath gas pressure of 35 psi，auxiliary gas pressure of 15 arb，and ion source heating temperature of 320 ℃. The negative ion mode had spray voltage of 3.2 kV，capillary heating temperature of 350 ℃， sheath gas pressure of 35 psi，auxiliary gas pressure of 15 arb，and ion source heating temperature of 300 ℃. The mass axis was calibrated by external standard method （mass error less than 5 ppm）. The scanning range of the first mass spectrometry was m/z 80.0-1 200.0 （the resolution was 70 000），the scanning range of secondary mass spectrometry was m/z 80.0-1 200.0（the resolution was 17 500），and the collision voltage was 20，40，60 eV. Retrieved from CNKI ，VIP，PubMed and other database ，the chemical constituents information of each Chinese traditional medicine in Fengliaoxing fengshi dieda wine were collected to establish chemical constituents database. The structure of the compounds was identified on the basis of above constituents database ，the relevant literature ，retention time of reference substance and MS fragmentation regularity. RESULTS & CONCLUSIONS ： Fifty-nine compounds were identified in Fengliaoxing fengshi dieda wine ，including 12 flavones（e.g. neoeriocitrin ，hesperidin.），8 alkaloids （e.g. baogongteng C or erycibellin ， ephedrine，pseudoephedrine）， 9 organic acids （e.g. chlorogenic acid ， cryptochlorogenic acid ，neochlorogenic acid ），7 coumarins（e.g. xanthotoxol）， 4 esters， 4 amino acids ， and 15 other categories（including volatile oils ，terpenes，amides）. UPLC- 5103YX11SF37（17）] Q-Exactive-MS technology can quickly and accurately identify the chemical constituents in Fengliaoxing fengshi dieda wine.
