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 establish a method for content determination of aflatoxin （AF） G2， G1， B2 and B1 in Qinghuo tablets （capsules）， and to evaluate the safety of the preparation. METHODS： HPLC-post-column photochemical derivatization was adopted， and 266 batches of Qinghuo tablets （capsules） from 37 manufacturers as sample. The determination was performed on Agilent C18 column with mobile phase consisted of water-acetonitrile-methanol （V/V/V， gradient elution） at the flow rate of 1.0 mL/min. The column temperature was set at 40 ℃. Excitation wavelength and emission wavelength of fluorescence detector were 360 and 450 nm. RESULTS： The linear ranges of AF G2， AF G1， AF B2 and AF B1 were 10.197-101.97 （r＝0.999 7）， 10.197-101.97 （r＝0.999 6）， 9.958 6-99.586 （r＝0.999 1）， 9.999 0-99.990 （r＝0.998 3） pg， respectively. RSDs of precision （n＝6）， reproducibility （n＝6） and stability tests （12 h， n＝5） were all lower than 3.0％. The detection limits were 0.80， 4.00， 0.80 and 4.00 pg， respectively. The quantitation limits were 1.60， 8.00， 1.60 and 8.00 pg， respectively. The recoveries were 85％-90％， 85％-90％， 55％-65％， 65％-75％ （RSD＝1.8％-4.7％， n＝6）. AF G2， AF G1， AF B2 and AF B1 were not detected in 266 batches of samples. CONCLUSIONS： This method is suitable for the determination of AF in Qinghuo tablets （capsules）. Although AF was not detected in the sample， it is advisable to add the determination of AF so as to improve its safety.
ABSTRACT
The authors discuss the technical problems in clinical evaluation of newly-developed Chinese medicines.For improvement of evaluation quality,this paper puts forward some suggestions for solving the common problems such as unitary intervention pattern,lack of corresponding treatment for the changed syndrome,subjectivity in standards of syndrome-differentiated diagnosis,ill-chosen medicine in control group,and mismanagement of medicine combination.