Study On The Quality Control Of Bushao Tiaozhi Jiaonang

Objective:The aim of this paper was to optimize and enhance the quality control of Bushao Tiaozhi Jiaonang’s crude medicinal materials,semi-finished and end products,based on modern analytical techniques and methods,under theguidance of traditional Chinese medicine（TCM）theory.In this research,the selection standards of crude medicinal materials were investigated,and the source and place of origin of the raw materials delivered were identified,in line with the technical study requirements of the quality standard of new traditional Chinese medicine.Meanwhile,the across-the-aboard qualitycontrol method of semi-finished and end products of Bushao Tiaozhi Jiaonang was established,in order to comprehensively control its quality,as well as to ensure stable and secure clinical efficacy.Methods:1.Study on the quality standard of crude medicinal materials（1）Collection—The four types of crude medicinal materials indicated in the prescription of Bushao Tiaozhi Jiaonang were collected,includingMicroctis Folium,Paeoniae Radix Rubra,Curcumae Rhizoma and Andrographis paniculata,which come from different sources,origins of place and batches.（2）Inspection—The four kinds of crude medicinal materials were inspected that have been collected according to 2015 Chinese Pharmacopoeia’s relevant laws and regulations on different kinds of medicinal materials,and selected qualified ones as samples for conducting research on fingerprint.（3）The establishment of fingerprint—To set up the HPLC fingerprint of crude medicinal materials of different sources,origins of place and batches,and identified its similarity via comparison software designated by Chinese Pharmacopoeia Commission,while assessed it with the assistance of the SPSS software.（4）Selection of study—According to the test results and the similarity of HPLC fingerprint,comprehensively assessed the quality of crude medicinal materials of different sources,origins of place and batches,thereforeultimately identified their sources and origins of place.2.Quality standard study on semi-finished products of Bushao Tiaozhi Jiaonang（1）Inspection—To carried out inspection on shape,properties,humidity,fineness and dissolubility of the semi-finished products of Bushao Tiaozhi Jiaonang.（2）TLC identification—To established ways to identify thin layer of the four kinds of medicines in the preparation respectively by TLC.（3）Content determination—According to the preparation process of Bushao Tiaozhi Jiaonang,was selected vitexin in Microctis Folium,paeoniflorin in Paeoniae Radix Rubra and germacrone in Curcumae Rhizoma as indicators to establish ways of identifying HPLC dose.（4）The establishment of fingerprint—To established fingerprint for semi-finished products of Bushao Tiaozhi Jiaonang,and conductedmethodological research on the ways of establishing it;made an analysis of fingerprint based on the Similarity Evaluation System for Chromatographic Fingerprint of TCM（Version 2004）,and confirmed where its common peak belongs and identified components,via its comparison with control articles,different kinds of medicinal materials and chromatographic peak under negative control.3.Quality standard study on end products of Bushao Tiaozhi Jiaonang（1）Inspection of the capsule—Inspection of the end products of Bushao Tiaozhi Jiaonang according to relevant laws and regulations on capsule under the Article 0103 stipulated in the four general guidelines of 2015 ChinesePharmacopoeia.（2）TLC identification—To established ways to identify thin layer of the four kinds of medicines in the preparation respectively.（3）Content determination—According to the preparation process of Bushao Tiaozhi Jiaonang,was selected vitexin in Microctis Folium,paeoniflorin in Paeoniae Radix Rubra and germacrone in Curcumae Rhizoma as indicators to establish ways of identifying HPLC dose.（4）The establishment of fingerprint—To established fingerprint for end products of Bushao Tiaozhi Jiaonang,made an analysis of fingerprint based on the Similarity Evaluation System for Chromatographic Fingerprint of TCM（Version 2004）,and confirmed where its common peak belongs and identified components,via its comparison with control articles,different kinds of medicinal materials and chromatographic peak under negative control.Results:1.Study on the quality standards of crude medicinal materials（1）The experiment was collected 30 batches of Microctis Folium,42 batches of Paeoniae Radix Rubra,50 batches of Curcumae Rhizoma and 36 batches of Andrographis paniculata as samples,and the results showed that the 4 crude medicinal materials were in conformity with the provisions of thePharmacopoeia of 14,42,41 and 11 batches,and the qualified rates were 46.67%,100%,82%and 30.56%.（2）The HPLC fingerprint for crude medicinal materials（includingMicroctis Folium,Paeoniae Radix Rubra,Curcumae Rhizoma and Andrographis paniculata）of Bushao Tiaozhi Jiaonang was established,where allcharacteristic peaks overall have good resolution and strong specificity,and the HPLC fingerprint for Paeoniae Radix Rubra as well as the Curcumae Rhizoma can be used to quickly and accurately identified medicinal materials ofdifferent sources.（3）By making a similarity analysis of test results and fingerprint,the medicinal materials delivered to make Bushao Tiaozhi Jiaonang were identified,including Microctis Folium,Paeoniae Radix Rubra,Curcumae Rhizoma andAndrographis paniculata originating in Guangdong,Inner Mongolia,Sichuan and Guangdong respectively.2.Quality standard study on semi-finished products of Bushao Tiaozhi Jiaonang（1）Quality standards for different items of Bushao Tiaozhi Jiaonang were established,including shape,properties,humidity,fineness and dissolubility.（2）The TLC methods with strong specificity for Microctis Folium,Paeoniae Radix Rubra,Curcumae Rhizoma and Andrographis paniculata included in Bushao Tiaozhi Jiaonang were also established.（3）The method for assay of vitexin in Microctis Folium,paeoniflorin in Paeoniae Radix Rubra and germacrone in Curcumae Rhizoma was also established,and respectively no less than 0.56mg·g^-1,5.09mg·g^-1 and 0.15mg·g^-1 of vitexin,paeoniflorin and germacrone have temporarily been confirmed to be contained in the semi-finished products of this capsule,based on the contentdetermination results and transfer rate of medicinal materials of the 20batches of semi-finished products.（4）The UPLC fingerprint of Bushao Tiaozhi Jiaonang’s semi-finished products was established,and among the 27 commonly marked characteristic peaks,13 of them come from Microctis Folium,7 come from Paeoniae Radix Rubra,7 come from Curcumae Rhizoma,and 4 come from Andrographis paniculata.Nine of them were identified,which accordingly were 1#Gallic acid,8#paeoniflorin,9#ferulic acid,13#vitexin,15#propyl gallate,16#isovitexin,18#kaempferol-3-O-β-D-rutinoside,20#narcissoside and 26#germacrone.The UPLC fingerprint of the 20 batches of Bushao Tiaozhi Jiaonang’s semi-finished products bears the similarity of 0.9 average with the compared standardfingerprint.3.Quality standard study on end products of Bushao Tiaozhi Jiaonang（1）The shape,properties,humidity,difference of pack volumes,disintegration and microbial limit of this capsule all conformed to relevant laws and regulations on capsule under the Article 0103 stipulated in the fourth general guideline of 2015 Chinese Pharmacopoeia.（2）The TCL identification was carried out to Microctis Folium,Paeoniae Radix Rubra,Curcumae Rhizoma and Andrographis paniculata contained in Bushao Tiaozhi Jiaonang,which identified fluorescent speckles/speckles corresponding to check sample and medicinal materials.（3）The method for assay of vitexin in Microctis Folium,paeoniflorin in Paeoniae Radix Rubra and germacrone in Curcumae Rhizoma was also established,and respectively no less than 0.28mg,2.50mg and 0.08mg of vitexin,paeoniflorin and germacrone have temporarily been confirmed to be contained per softgel of the capsule,based on the content determination results and transfer rate of medicinal materials of the 20 batches of end finishedproducts.（4）The UPLC fingerprint of Bushao Tiaozhi Jiaonang’s end products was established,and among the 27 commonly marked characteristic peaks,13 of them come from Microctis Folium,7 come from Paeoniae Radix Rubra,7 come from Curcumae Rhizoma,and 4 come from Andrographis paniculata.Nine of them were identified,which accordingly were 1#Gallic acid,8#paeoniflorin,9#ferulic acid,13#vitexin,15#propyl gallate,16#isovitexin,18#kaempferol-3-O-β-D-rutinoside,20#narcissoside and 26#germacrone.The UPLC fingerprint of the 20 batches of Bushao Tiaozhi Jiaonang’s end products bears the similarity of 0.9 average with the compared standard fingerprint.Conclusions:This paper overall contributes to controlling the quality of BushaoTiaozhi Jiaonang,a Chinese medicine compound preparation so as to ensure its secure and effective clinical medication via establishing its quality standard,from crude medicinal material to semi-finished product and end product.