Quality Standard Reaserch On Paeonia Lactiflora Formula Granule

Objective:According to the“Technical Requirements for Quality Control and Standard Formulation of Chinese Medicinal Formula Granules?Exposure Draft?”?hereinafter referred to as the“Exposure Draft”?:“The standards that need to be established for traditional Chinese medicine formula granules mainly include the Chinese herbal medicine standard used as the initial raw material,as the extraction Standards for the preparation of raw materials,standards for intermediates used as raw materials for preparations,and finished product standards for finished products."Collected 15batches of the Paeoniae?not less than 3 batches of origin for each medicinal material?,established the standard for the raw materials of the Paeoniae Standards,standards for the Paeoniae standard decoctions,standards for dry extracts of the Paeoniae intermediates,optimization of technical parameters for the completion of the Paeoniae formula granules,and establishment of standards,preliminary drafting of draft quality standards for the Paeoniae formula granules,realization the production process is standardized and the quality standards are scientific.Methods:1.The quality standards for the raw materials of the Paeoniae:According to the requirements of the“Chinese Pharmacopoeia”version of the 2015 edition of the“the Paeoniae”,the original medicinal materials of the Paeoniae were studied in terms of traits,identification,examination,determination of extract,and content determination.2.The quality standard for the Paeoniae pieces:According to the requirements of the“Chinese Pharmacopoeia”version of the 2015 edition of the Paeoniae item,the the Paeoniae medicinal herbs should be washed,run through,cut into thin slices,and dried to obtain the Paeoniae pieces,and the traits,identification,and examination,determination of extract,content determination,and other aspects,the study was conducted on the Paeoniae pieces.3.Quality standard of the Paeoniae standard decoction:Prepare the Paeoniae standard decoction,and establish the quality standard of the Paeoniae standard decoction through the determination of the rate of paste,the determination of paeoniflorin content and the transfer rate,and characteristic characterization parameters.4.The quality standard of the Paeoniae dry extract:through L₉?3⁴?orthogonal test,taking out the paste rate and paeoniflorin content as the inspection index,the optimal extraction process of the Paeoniae is optimized,and the content of paeoniflorin and the content of paeoniflorin are optimized.The quality standards for the dry extract of the Paeoniae were established based on the determination and transfer rate and the characteristics of the characterization parameters.5.The quality standard of the Paeoniae formula granules:screening the preparation process of the Paeoniae formula granules and carrying out three batches of pilot tests.From the aspects of traits,identification,inspection,extracts,content determination,characteristic maps and preliminary stability inspection,systematic research was conducted on the Paeoniae formula granules to establish the quality standard of the Paeoniae granules.The identification method uses thin layer chromatography with peoniculin as a reference substance.Results:1.The raw materials of the Paeoniae:The diameter of the Paeoniae in Sichuan Zhongjiang and Pan'an of Zhejiang is about 1.5 cm-2 cm,the diameter of the Paeoniae in Bozhou is about 1 cm-2 cm,and the diameter of the Paeoniae in Heze,Shandong is about 0.5 cm-1 cm;the length of the Paeoniae in each producing area is about 10-20 cm,there is a disconnection during picking or concoction;the pale reddish browns on the surfaces of Sichuan Zhongjiang and Pan'an Zhejiang are mostly reddish brown,and the surface whites of Bozhou and Shandong Heze are mostly white;the cross-section wood of all the producing areas is shown radiant daisy heart-shaped.15 batches of the Paeoniae were identified by thin-layer chromatography and the spot after the coloration was clear and accurate,showing a blue-purple;the water content was 3.61%-15.84%;the total ash content ranged from 1.88%-3.67%;the contents of Pb in heavy metals and harmful elements?mg/kg?range from 0.935 to 1.278,the content of Cd ranges from 0.040 to 0.077,the content of As ranges from 0.433 to0.643,the content of Hg from 0.028 to 0.046,and the content range of Cu.It is2.389-3.981;the sulfur dioxide residual?mg/kg?range 85.87-201.83,extracts content range 19.80%-31.50%;the content of paeoniflorin was 1.97%-4.50%.2.The Paeoniae pieces:The diameter of the Paeoniae pieces in Sichuan Zhongjiang and Pan'an in Zhejiang is about 1.5 cm-2 cm in diameter,the diameter of the Paeoniae in Bozhou is about 1 cm-2 cm,and the diameter of the Paeoniae in Shandong Heze is about 0.5 cm-1 cm,and the thickness is about 1-2 mm;the surface of Sichuan Zhongjiang and Zhejiang Pan'an decoction pieces are mostly reddish-brown,and the surfaces of Bozhou and Shandong Heze are white.All cross-sections of the Paeoniae Debris Slices have obvious formation rings and the rays are radial.15 batches of the Paeoniae pieces were identified by thin-layer chromatography and the spot after the coloration was clear and accurate,showing a blue-purple;the water content was 5.29%to 14.24%;the total ash content ranged from 2.02%to 3.52%;the sulfur dioxide residue?mg/kg?range is 96.69-201.12;the extracts content range is17.76-34.61%;the content of paeoniflorin ranged from 1.52%to 4.43%.3.The Paeoniae standard decoction:The average acceptable rate of 15 batches of the Paeoniae standard soup decoction was:16.84%-24.24%.The acceptable range of average paeoniflorin content was:1.24%-3.50%,and the acceptable range of transfer rate was 60.07%-99.79%.The acceptable range for the similarity profile of the standard soup decoction is 0.874-1.069 and the concentration of the sample is 0.004 g/ml?corresponding to 0.004 gram pieces per milliliter?.4.The Paeoniae dry extract:The preparation process of the Paeoniae dry extract was immersed for 1 h,decocted with water 10 times,kept boiling for 80 min after boiling,extracted twice,filtered hot,rapidly cooled and combined with filtrate,and centrifuged to remove impurities?12000 r/min,15 min?take the supernatant,decompression concentrate?temperature<50°C?to 0.2 g/ml decoction and vacuum drying at 60°C to obtain the Paeoniae dry extract.The content range of paeoniflorin in the 15 batches of the Paeoniae dry extract was1.34%-3.67%,the extract ratio was 17.96%-25.16%,and the transfer rate of the paeoniflorin was 69.24%-99.49%.The acceptable range for the similarity of the characteristics of the 15 batches of dried Paeoniae extract was 0.862-1.072,and the concentration of the sample was 0.004 g/ml?corresponding to 0.004 gram pieces per milliliter?.5.The Paeoniae formula granules:The production process of the Paeoniae formula granules is to prepare the Paeoniae dry extract,“and the amount of dextrin is determined according to the amount of auxiliary material=amount charged pieces/equivalent-amount of dry extract”,and mixing dextrin and dry extract,the embryonic tablet is pressed with a tableting machine and broken.Sieve?12#⁴0#?,the whole grain,sub-packing,that is,too.The angles of repose of the particles are all less than 40^o,indicating that the particles have good fluidity;the critical relative humidity of the Paeoniae formula particles is 60°C;the granules have a loading specification of 1.0 g/bag;and the packaging material is a polypropylene composite film bag.Three batches of pilot tests are conducted,the process is stable,the yield of pellets and the content of index components are basically stable,and industrial production can be carried out.The quality standard of the Paeoniae granules was studied.The traits,identification,inspection,extracts,content determination,characteristic map and preliminary stability inspection were systematically investigated.The Paeoniae granules total size of the granules was 10.48%-11.45%;the content range is 4.73%-5.38%;the leachate content range is 10.84%-21.43%;the paeoniflorin content range is 7.79%-9.42%;and the acceptable range of the characteristic spectrum of the Paeoniae formulation particle is0.867-1.071.The concentration is 0.004 g/ml?corresponds to 0.004 g pieces per milliliter?,and the final content limit is not less than 7.79 mg per g of the Paeoniae granules.Preliminary stability test results indicate that the Paeoniae granules are stable under the above conditions.Prepare a draft quality standard for the Paeoniae formula granules.Conclusion:The successful establishment of the quality standard for the Paeoniae formula granules provides a reference for the quality control of white peony granules.