Content determination of ephedrine hydrochloride and pseudoephedrine hydrochloride in Shexiang zhuanggu plaster and its quality evaluation / 中国药房

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.

Determination of camphor,menthol,synthetic bornel and the wintergreen oil in Shexiang Zhuanggu Plaster by GC / 中成药

AIM:To study the method of determing camphor, menthol, synthetic bornel and the wintergreen oil contents in Shexiang Zhunggu Plaster. METHODS: Gas phase chromatogram was used to determine contents of camphor, menthol, synthetic bornel and the wintergreen oil in Shexiang Zhuanggu Plaster. The chromatogram condition consisted of the capillary vessel column(PEG-20M, 30 m?0.32 mm?0.25 ?m). The temperature programing rose from 100 ?C to 130 ?C by 5 ?C /minute, then 30 ?C /minute to 200 ?C , lasting 2 minutes in the end. The temperature of the entrance of the capillary vessel column: at 220 ?C , temperature of the detector was 240 ?C ; N_2: 5 mL/minute, H_2: 45 mL/minute, Air: 450 mL/minute; sample quantity was 0.2 ?L. RESULTS: Under certain chromatogram condition, there was linear relation among the camphor, menthol, synthetic bornel and the wintergreen oil and the peak area in the scope of 0.027 38 mg/mL-0.438 08 mg/mL, 0.041 15 mg/mL-0.658 4 mg/mL, 0.033 38 mg/mL-0.534 1 mg/mL, 0.042 15 mg/mL-0.674 4 mg/mL, respectively. The average recoveries were 98.37%, 99.76%, 98.80% and 97.61%, respectively. RSD were 1.7%, 1.8%, 0.96% and 1.5%, respectively. CONCLUSION: This experiment provides an accurate and reliable method to control the quality of Shexiang Zhuanggu Plaster.

Simultaneous determination of camphor,menthol,synthetic borneol and methyl salicylate in Shexiang Zhuanggu Plaster by GC / 中成药

AIM: To establish the simultaneous determination of camphor,menthol,synthetic borneol and methyl salicylate in Shexiang Zhuanggu Plaster(Camphor,Mentholum,Borneolum Syntheticum,etc). by GC. METHODS: The sample solution was distilled in volatile oil determination apparatus.Naphthalene was used for the internal standard.The GC system consisted of capillary column,PEG-20M as the stationary phase,nitrogen as the carrier gas,FID as the detector.The programmed temperature-GC and internal standard method was employed to determine four kinds of components in Shexiang Zhuanggu Plaster. RESULTS: Camphor,menthol,synthetic borneol(borneol and isoborneol) and methyl salicylate in Shexiang Zhuanggu Plaster and naphthalene have been separated well under the same chromatographic condition.The average recovery of camphor,menthol,synthetic borneol and methyl salicylate were 96.92%(RSD=2.42%),98.03%(RSD=1.81%),99.02%(RSD=1.47%) and 98.15%(RSD=1.59%),respectively. CONCLUSION: The method is simple,accurate and separable,and can be used to control the quality of Shexiang Zhuanggu Plaster