Study On The Preparation And Quality Standard Of Xiong-Bing Nasal Spray

1. ObjectXiongbing is empirical formula that from the first affiliated hospital of Guangzhou University of TCM. It is widely used in clinical for Acute Ischemic Stroke(AIS). The formula is made up of Rhizoma Chuanxiong and borneol. This study is aimed to established the praperation method of Xiongbing Nasal Spray.2. Method2.1 Preparation of Chuanxiong IntermediateComparision research on the two extraction and purification process:(1) the water extraction process based on the designs of cross experiment;the alcohol precipitation process based on the design of single factor experiment. (2)the alcohol extraction process based on the designs of cross experiment;the extract solution was purified by macroreticular resin. The content of FA has been used as a selection criterion to the extraction and purification method of Chuanxiong.2.2 Disslution methods of BornelTo study on the dissolution methods of bornel:solubilizer,β-CD,HP-β-CD. Comparing the different preparation methods and the stability of the inclusion compound.2.3 pH and PreservativeTo choose the proper pH and preservative according to the content of FA,2.4 Quality stander To establish the quality stander of the Xiongbing Nsal Spray, according to Chinese Pharmacopoeia. To establish the TLC and the determination method of FA and bornel.2.5 FingerprintsTo establish the fingerprints of Chuanxiong,Chuanxiong Intermediate,Xiongbing Nasal Spray.To explore the relateness of them.2.6 SaftyTo explore the irritation of Xiongbing Nasal Spray to the ocular mucous of rabbits and the upper jaw of toad.2.7 StabilityTo study on the influences of sunlight,high temperature,high humidity on the stability of Xiongbing Nasal Spray.3. Results3.1 Preparation of Chuanxiong IntermediateThe ethanol extraction experiment shows that 80% ethanol 12 times, extrcted twice,1.5h for once is the best extraction method. The optimum purified conditions were as follows:1BV/h adding sample flow rate,50% ethnol 9BV elute. The eluent was vacuum evaporated to recover the solvent, added distilled water to scale.3.2 Disslution methods of BornelThe optimal condition of the inclusion prepared by trituration method were Bornel to HP-β-CD(0.3:4), the inclusion time were 1.5 h.3.3 pH and PreservativeThe optimum pH and preservative are 6.0 and 0.01% bromogeramine.3.4 The preparation of Xiongbing Nasal SprayAdded the bornel inclusion and 0.01% bromogeramine into the Chuanxiong intermediate, adjust pH to 6.0.3.5 Quality Assessment of Xiongbing Nasal Spray The average pH is 6.28, RSD=1.72%. The average loading volume must be no fewer than 95%. The relative density is 1.2642～1.2664. The total spray times must be no fewer than 100,It is 0.145-0.166mg per press. FA and bornel can be identified by TLC. The content concentration required that the containing of FA is not less than 5.12mg, bornel is not less than 0.024mg in 1mL of Xiongbing Nasal Spray.3.6 FingerprintsThe similarity of Chuanxiong,Chuanxiong Intermediate,Xiongbing Nasal Spray is very well.3.7 SaftyXiongbing Nasal Spray has mild irritation.3.8 StabilityThe Xiongbing Nasal Spray has fairly good appearance,But the content of FA showed a downward trend.