Study On Pharmaceutical Of Xiaoer Cough Relieved Granules

Xiaoer Cough Relieved Granules is a compound preparation made up by the refined extract of nine kinds of Chinese herbal medicine and they are Ephedra, Bupleurum, Bitter Almond, Peucedanum, Anemarrhena, Gardenia, Shegan, Scutellari-a and Licorice. This subject regards traditional Chinese medicine theory as the guiding principle. Meanwhile, it has done researches on systematic experimental studies for preparation process, quality standards and preliminary stability test by using modern pharmaceutical technology.Preparing process studyExtraction process study:Design L9(34) orthogonal experiments by using the Multi-Stage Dynamic Countercurrent Extraction to find out the optimal process. The study factors are material-liquid ratio, extraction temperature, extraction time, the number of extraction unit group. The best process of the tank group dynamic continuous countercurrent extraction is A2B1C1D3(the material-liquid ratio is1to10; the temperature50℃; the extraction time is15min; the number of extraction unit group is four). The dry extract yield is18.21%and RSD%is0.11. Ephedrine extraction rate is as high as66.95%and RSD%is0.88. The results show that the process is stable and repeatable.Purification process study:Use water extraction and alcohol precipitation refining process. Select the transfer rate of ephedrine and the dry extract yield as the indexes of this process. Design L9(34) orthogonal experiment to optimize the the best refining process of water extraction and alcohol precipitation method. The optimum process of water extraction and alcohol precipitation is A3B3C1D1(the extract was concentrated to a concentration of1g/mL; adding ethanol to reach a concentration of85%; alcohol precipitation for12h). The supernatant is separated and concentrated to a thick paste. The transfer rate of ephedrine is as high as90.52%and RSD%is0.51; the dry extract yield is16.83%and RSD%is1.4. The results show that water extraction and alcohol precipitation refining process is stable and feasible, and can effectively shorten the standing time. The ephedrine transfer rate and extract rate are high.Molding process study:Study the forming process of dry extract by using granulation technique.Select extract relative density, the inlet velocity of liquid, atomizing pressure and the inlet air temperature as study factors, and the qualified particle yield and moisture content as indicators. Using L9(34) orthogonal test to select the best process. The optimal process of spray granulation is A3B1C3D1(the atomization pressure is2.6Pa; the inlet air temperature is180℃; the inlet velocity of liquid is8mL/min; the relative density of the dry extract is1.2). The dry extract is sprayed into the granulator and mixed with excipients, and then dried to form granules.The granules yield is92.54%and RSD%is1.5. The moisture content of granules is0.96%and RSD%is1.15. The results show that the process is stable, inter-quality of product is stable, reproducibility is good and it can be enlarged to production.Quality standard studyTLC method is used to do qualitative identification of Bupleurum, Bitter Almond, Gardenia, Shegan, Scutellaria; the content of the primary efficacy component ephedrine is determined by HPLC method. Chromatographic column is Ultimate XB-C18column(5mm,4.6x250mm); Mobile phase is acetonitrile-0.1%H3PO4(including0.05%triethylamine)(5:95); flow rate is1.0mL/min; column temperature is25℃; sample quantity is10μl. Results:the TLC spots were fairly clear and the negative control shows no interference; Ephedrine sample quantity ranging from0.097μg～0.582μg share a good linear relationship (r=0.9999); average recovery rate is98.26%(RSD%=1.72, n=6); Repeatability is good (RSD%=0.34, n=6). These results show that this method is accurate and reliable for qualitative and quantitative detection, reproducible and can be used as the quality control method of this product.Preliminary stability test studyThe preliminary investigation of stability of Xiaoer Cough Relieved Granules is decided by influencial factors test, accelerated test and long-term stability test. And then speculate the validity of this product. Put the Commercially available packaging drugs under the condition of60℃,92%relative humidity and4500±500Lx light intensity for ten days. In the accelerated stability test, the drugs are placed under the condition of40℃±2℃,75%±5%relative humidity for six months. In the Long-term stability test, the drugs are placed under the condition of25℃±2℃,60±10%relative humidity for twelve months. After these tests, check the stability of drugs within the prescribed time. The influencial factor tests show that the granules should be stored in a cool dry place. During the accelerated stability test period and long-term stability test period, various quality checks indicators of the sample are in accordance with the provisions, which indicate that sample stability is good. I preliminary speculate that this product is valid for two years.