| Objective:Danqiao Injection,a Chinese traditional medicine compound formulation,is manufactured by bile ointment,baicalein extract and forsythia suspensa extract.In the study,the pharmaceutical research of Danqiao Injection was carried out,which mainly included the research of production process technology,quality control and stability assessment,providing a research foundation for the further development of Danqiao Injection.Methods:1.Production process research:Selecting acid and alkali extraction and purification method,taking 1:1 hydrochloric acid dosage,sodium hydroxide dosage and purification time as the main factors,taking the content of goose deoxycholic acid and deoxycholic acid in the purified liquid as the investigation index,a L9（34）orthogonal table was utilized to optimize the extraction process.Using the content of cholic acid and baicalin as the detection index to optimize the process judgment,screen the best compatibility of the auxiliary materials in the prescription,and determine the best prescription process of the bile injection;under the optimum prescription process conditions,taking product characteristics,p H,identification and content requirements as the main inspection indicators,the pilot production of three batches of samples was studied.Through pilot study,the enlarged pilot process was verified.2.Quality standard research:TLC was used to establish the identification methods of bile ointment,baicalein extract and Forsythia suspensa extract in Danqiao injection,and high performance liquid chromatography（HPLC）was utilized to determinate the content of the main effective components of Danqiao injection,such as bile ointment and baicalein extract,and the quality standard of Danqiao injection was established on this basis.3.Stability study:The stability experiments,including light acceleration test,constant temperature and humidity acceleration study and long-term stability experiment,were used to investigate the stability of three batches of Danqiao injection according to the Guiding Principles of Veterinary Traditional Chinese Medicine and Natural Medicine Stability Test of Ministry of Agriculture.Results:1.Orthogonal test results showed that the optimum extraction process was to purify 10g bile paste by adding appropriate amount of water to melt,adding 1:1 HCl 4m L to precipitate for 12 hours,then adding appropriate amount of water,adding 0.2g sodium hydroxide,dissolving and filtering.The formulation of Danqiao injection was as follows:20g bile ointment,20g baicalein extract,10g weeping forsythia extract,supplementary materials were as follows:Anhydrous sodium sulfite,EDTA-2Na,sodium hydroxide and tween-80.The optimum formulation is:bile ointment 20g,baicalein extract 20g,weeping forsythia extract10g,anhydrous sodium sulfite 2g,EDTA-2Na 2%,sodium hydroxide 0.12%and Tween-801%.All three batches of pilot products are qualified and stable.2.According to the requirements of Chinese Veterinary Pharmacopoeia,the variety and origin of the original medicinal materials were identified,and the internal control quality standard of the extract of Danqiao injection was formulated after pilot production of several batches of Danqiao injection.The TLC identification methods of the main components of Danqiao injection,such as bile ointment,baicalein extract and weeping forsythia extract,were established through the study of preparation quality.The content determination methods of Danqiao injection’s main effective components,Dangao and baicalein extract by high performance liquid chromatography were established.On this basis,the quality standard of Danqiao injection was established.3.Light acceleration test of three batches of Danqiao injection samples showed that light had on significant influence on the active ingredients in the formulation;constant temperature and humidity acceleration experiment results showed that high humidity and temperature had a slight influence on the content of baicalin and bile ointment,the main ingredients of Danqiao injection,and at the same time,the samples were supplied within half a year.All the quality indexes are within the scope of the quality standard;combined with long term stability experiment,it is finally suggested that Danqiao injection should be preserved under cool and dark conditions,and its tentatively validity period is nine months.Conclusion:The process technology of Danqiao injection is reasonable and scientific,the method of quality control is simple and operable,and the stability is well with nine months.According to the systematic pharmaceutical research,the present study meet the requirements of clinical application,and provide scientific basis for the further development of clinical trials and industrial production. |
