| Ganmaoling capsule, a compound preparation of traditional Chinese and Western medicine, is included in the13th volume of Chinese traditional patent formulation, drug standards of Ministry of Health, consists of five traditional Chinese medicines i.e. Evodia lepta, Bidens biternata, wild dendranthema flower, Ilex asprella and peppermint oil, and three chemical drugs i.e. paracetamol, chlorphenamine maleate and caffeine. The capsule has the effect of antipyretic analgesic, and is mainly used for symptoms of headache, fever, nasal obstruction and discharge, pharyngalgia, caused by cold.Because the current standard of Ganmaoling capsule exists weakness of less and poor representative quality indicators, poor specific method, complicated operation and poor reproducibility, this study carried out improving research on the basis of existing standard, established a series of simple, rapid and accurate new methods, thereby forming a more consummate and scientific quality standard of Ganmaoling capsule.Objective:to optimize and establish the thin layer identification method of Chinese drug ingredient in the prescription Ganmaoling capsule; to establish the HPLC method for simultaneous determining three chemical drugs i.e. paracetamol, chlorphenamine maleate and caffeine, and index component of wild dendranthema flower i.e. linarin; to establish the mensuration for determining the dissolution of Ganmaoling capsule.Methods:1. Used control drug as standard control, to conduct thin layer identification of Evodia lepta, Ilex asprella in the prescription; and to identify HPLC retention time of three chemical drugs i.e. paracetamol, chlorphenamine maleate and caffeine;2. Used the contents of index component of wild dendranthema flower i.e. linarin and three chemical drugs i.e. paracetamol, chlorphenamine maleate and caffeine as quality control index of Ganmaoling capsule, to establish HPLC method for simultaneous determining the respective content of above four components: chromatographic column:Shibadzu Inertsil ODS-SP column (5μm,250mmX4.6mm), mobile phase:methanol-water-glacial acetic acid (26:23:1), flow rate:1.0ml/min, detection wavelength:260nm (paracetamol, caffeine and chlorphenamine maleate) and334nm (linarin), column temperature:35℃, sample size:20μl.3. Screened and determined the dissolution phenomenon of three components in the preparation prescription i.e. paracetamol, caffeine and chlorphenamine maleate under conditions of different dissolution medias, different methods and different rotation speeds, drew the dissolution curve, established the dissolution mensuration of preparation, and ascertained to adopt oar method (75revolutions/min), dissolution media:900ml of0.1%HCl solution, sampling time45min, and high performance liquid chromatography (chromatographic condition:Shibadzu Inertsil ODS-SP column (5μm,250mm X4.6mm), mobile phase:methanol-water-glacial acetic acid (26:23:1), flow rate:l.Oml/min, detection wavelength:260nm, column temperature:35℃, sample size:50μl).Results:1.The thin layer chromatography method using control drug and the identification method of HPLC retention time established by optimization is simple, feasible and specific.2. The content of four components detected by dual-wavelength HPLC: paracetamol in109.22×g/ml～1092.20μg/ml showed a good linear relationship (r=0.9999), the average recovery rate was99.09%, RSD was0.95%; caffeine in2.05μg/ml～20.50μg/ml showed a good linear relationship (r=0.9999), the average recovery rate was100.17%, RSD was0.85%; chlorphenamine maleate in2.06μg/ml～20.59μg/ml showed a good linear relationship (r=1.0000), the average recovery rate was99.74%, RSD was1.05%; linarin in9.77μg/ml～97.69μg/ml showed a good linear relationship (r=0.9998), the average recovery rate was98.22%, RSD was1.48%.3. Mensuration of dissolution:the linear range of paracetamol, caffeine and chlorphenamine maleate was the same with determination, and the average recovery rate was not less than99%. The dissolution behavior of preparations selected from three different manufacturers was similar, and the dissolution of three components in45min exceeded more than80%of the labeled amount.Conclusion:On the basis of current standard of Ganmaoling capsule, the present study established the thin-layer chromatography identification method of Evodia lepta and Ilex asprella using control medical material, ascertained HPLC retention time identification method of paracetamol, chlorphenamine maleate and caffeine; the established dual-wavelength HPLC method, which can determine paracetamol, caffeine, chlorphenamine maleate and linarin simultaneously, had relatively good precision, accuracy, repeatability and durability, and can be used as assay method for determining contents of the four components in Ganmaoling capsule; the established mensuration of dissolution was convenient and quick, accurate and reliable, and can be used for determining the dissolution of Ganmaoling capsule; the study established new method for quality control and new index for quality evaluation, and laid a solid foundation for formulating more consummate quality standard. |
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