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1.
China Pharmacy ; (12): 196-202, 2022.
Article in Chinese | WPRIM | ID: wpr-913111

ABSTRACT

OBJECTIVE To evalu ate the quality of crude drug and di fferent processed products of Eriobotryae Folium . METHODS Ten batches of Eriobotryae Folium were processed into honey-stir-baked Eriobotryae Folium ,ginger-juice-stir-baked Eriobotryae Folium ,ginger-juice-boiled Eriobotryae Folium ,licorice-juice-stir-baked Eriobotryae Folium ,licorice-juice-boiled Eriobotryae Folium ,stir-fried Eriobotryae Folium ,totally 70 batches of samples . The contents of alcohol-soluble extracts ,the contents of total triterpene acids (calculated by ursolic acid )and five triterpene acids such as euscaphic acid were determined by hot-dipping method ,ultraviolet and visibe spectrophotometry and high performance liquid chromatography (HPLC),respectively. The fingerprints were established with HPLC and their similarity evaluation was conducted with Similarity Evaluation System of TCM Chromatographic Fingerprint (2004A). Common peaks were identified by comparison with mixed control. Hierarchical clustering analysis ,principal component analysis and orthogonal partial least squares-discriminant analysis (OPLS-DA) were performed by using SPSS 22.0 software and SIMCA-P 14.1 software. RESULTS In Eriobotryae Folium ,honey-stir-baked Eriobotryae Folium ,ginger-juice-stir-baked Eriobotryae Folium ,ginger-juice-boiled Eriobotryae Folium ,licorice-juice-stir-baked Eriobotryae Folium ,licorice-juice-boiled Eriobotryae Folium ,stir-fried Eriobotryae Folium ,average contents of alcohol-soluble extracts were 25.90%,39.95%,27.44%,28.20%,28.38%,26.36% and 29.26%;average contents of total triterpene acids were 40.62,49.33,52.56,46.38,52.17,55.06 and 53.41 mg/g;average contents of euscaphic acid ,crataegolic acid ,corosolic acid , oleanolic acid ,ursolic acid and average total content were 1.966-4.808,1.459-2.824,4.525-8.172,1.294-1.817,6.294-8.470, 15.538-25.671 mg/g,respectively. There were 11 common peaks in 70 batches of samples ,and the peak 2,5,6,10 and 11 were identified as euscaphic acid ,crataegolic acid ,corosolic acid , oleanolic acid and ursolic acid. The similarities of crude drug different processed products with crude drug fringer print were 0.919-1.000. Among 70 batches of samples ,10 batches of Eriobotryae Folium could be clustered into one category ,and 10 batches of ginger- juice-boiled Eriobotryae Folium could be clustered into one category ;other 50 batches of processed products of Eriobotryae Folium could be clustered into one category ; the cumulative variance contribution rate of the first two principal components was 80.682%;variable importance in projection (VIP)value was in descending order ,i.e. peak 2(euscaphic acid )>peak 5(crataegolic acid )>peak 6(corosolic acid )>peak 9 (unknown component ) >peak 11 (ursolic acid )>peak 10 (oleanolic acid ), which of them were all higher than 1. CONCLUSIONS After processing ,the contents of alcohol-soluble extracts ,total triterpene acids and the total content of five triterpene acids (euscaphic acid ,crataegolic acid ,corosolic acid ,oleanolic acid and ursolic acid )increased in varying degrees , among which the content of alcohol-soluble extracts in honey-stir-baked Eriobotryae Folium was the highest ,the content of total triterpene acids in licorice-juice-boiled Eriobotryae Folium was the highest ,and total content of five triterpene acids in ginger- juice-boiled Eriobotryae Folium was the highest. Euscaphic acid ,crataegolic acid ,corosolic acid ,ursolic acid ,oleanolic acid and other components may be the differential components affecting the quality of raw and processed the leaves from Eriobotryae Folium .

2.
China Pharmacy ; (12): 185-190, 2022.
Article in Chinese | WPRIM | ID: wpr-913109

ABSTRACT

OBJECTIVE To establi sh the fingerprint of Cnidium monnieri and a method for the content determination of 4 kinds of coumarins. METHODS Ultra-high performance liquid chromatography (UPLC) method was adopted to establish the fingerprints of 21 batches of C. monnieri ; their similarities were evaluated with Similarity Evaluation System of TCM Chromatographic Fingerprint (2012 edition);common peaks were identification by comparison with reference substance. Using 10 common peak areas as variables ,cluster analysis was performed for 21 batches of C. monnieri by the method of between groups. The relative correction factors of xanthotoxin ,bergapten and imperatorin were calculated by the same UPLC method with osthole as the internal reference. The contents of them were calculated by quantitative analysis of multi-components by single marker (QAMS),and compared with the results of external standard method. RESULTS Totally 10 common peaks were identified in the fingerprints of 21 batches of C. monnieri ;the similarities ranged from 0.997 to 1.000. Peak 4 was identified as xanthotoxin ,peak 8 as bergapten ,peak 9 as imperatorin and peak 10 as osthole. A total of 21 batches of samples were divided into 3 categories,of which S 7 was clustered into one category ,S14 was clustered into one category ,and the other 19 batches were clustered into one category. The relative deviations of the contents of xanthotoxin ,bergapten and imperatorin determined by QAMS and external standard method were in the range of 0.88% -1.07% ,2.22% -2.29% ,0.67% -2.93% ,respectively. CONCLUSIONS UPLC fingerprint of C. monnieri is successfully established ,and QAMS method for content determination of 4 coumarins is also established.

3.
China Pharmacy ; (12): 160-164, 2022.
Article in Chinese | WPRIM | ID: wpr-913105

ABSTRACT

OBJE CTIVE To establish the finger prints for Yinhuang solution for inhalation and determine the contents of neochlorogenic acid ,chlorogenic acid and cryptochlorogenic acid simultaneously. METHODS Using baicalin as reference ,the fingerprints of Yinhuang solution for inhalation were established by high performance liquid chromatography (HPLC). Relative correction factors of neochlorogenic acid and cryptochlorogenic acid were calculated by slope correction method ,using chlorogenic acid as reference ;the contents of them were calculated according to relative correction factor. The results of quantitative analysis of multi-components by single marker (QAMS)were compared with those of external standard method (ESM). RESULTS There were 18 common peaks in the fingerprints of 10 batches of Yinhuang solution for inhalation ,and their similarities with reference fingerprint were higher than 0.90. A total of 7 common peaks were identified as baicalin ,neochlorogenic acid ,chlorogenic acid , cryptochlorogenic acid ,isochlorogenic acid B ,3,5-di-O-caffeoylquinic acid and 4,5-di-O-caffeoylquinic acid. The linear range of neochlorogenic acid ,chlorogenic acid and cryptochlorogenic acid were 0.025 0-1.247 4 μg(r=0.999 7),0.039 3-1.178 7 μg(r= 0.999 9),0.031 6-1.184 1 μg(r=0.999 9),respectively. RSDs of precision ,reproducibility and stability tests (48 h)were all lower than 1.0%. The average recoveries were 93.92%(RSD=1.32% ,n=6),94.46%(RSD=1.45%,n=6),93.93%(RSD= 1.57%,n=6). Relative correction factors of neochlorogenic acid and cryptochlorogenic acid were 1.068 and 1.233. The contents of neochlorogenic acid and cryptochlorogenic acid determined by QAMS method were 0.301 8-0.386 3 and 0.262 5-0.362 5 mg/mL, respectively. The contents of neochlorogenic acid ,chlorogenic acid and cryptochlorogenic acid by ESM were 0.302 6-0.387 2, 0.231 0- 0.334 0,0.261 6-0.361 3 mg/mL,respectively. The deviations of the content determination results of the two methods(except for chlorogenic acid )were both not higher than 0.20%. CONCLUSIONS Established HPLC fingerprints are stable and feasible. Established QAMS method is accurate and rapid. HPLC fingerprint combined with QAMS can be used for the quality control for Yinhuang solution for inhalation .

4.
China Pharmacy ; (12): 153-159, 2022.
Article in Chinese | WPRIM | ID: wpr-913104

ABSTRACT

OBJECTIVE To establish the infrared fingerprints of Achyranthes bidentata from different producing areas ,and to conduct multivariate statistical analysis. METHODS The infrared fingerprints of 61 batches of A. bidentata samples were established by Spectrum for Window 3.02 and OMNIC 9.2 software. Taking the relative peak height of common peaks of infrared fingerprint as the variable ,the normal distribution analysis was carried out by Excel 2016 software;SPSS 22.0 software was used for cluster analysis and principal component analysis ,and the comprehensive score was calculated ;the orthogonal partial least squares-discriminant analysis was carried out by SIMCA 14.1 software,and the marker wave numbers affecting the quality of A. bidentata were screened by taking the variable importance in projection (VIP)>1 as the standard. RESULTS The correlation coefficients of infrared spectra of 61 batches of A. bidentata samples were 0.967 2-0.997 7;there were 13 common peaks. The results of normal distribution analysis showed that the normal distribution curve of relative peak height of common peaks for A. bidentata from Henan and Hebei did not cross ,and the normal distribution curve of A. bidentata from Henan and Inner Mongolia crossed. The results of cluster analysis showed that when the distance between groups was 15,61 batches of A. bidentata samples could be clustered into 3 categories,including N 1-N12 were clustered into one category ,N13-N45 were clustered into one category,and N 46-N61 were clustered into one category. The results of principal component analysis showed that the cumulative variance contribution rate of the first three principal components was 91.121%;comprehensive score of qq.com A. bidentata (number N 40) in Jiabu village ,Jiaozuo City , Henan Province was the highest (2.39), and that of A.bidentata(number N 4)in Xin ’an village ,Anguo City ,Hebei Province was the lowest (-2.89). The results of orthogonal 163.com partial least squares-discriminant analysis showed that 61 batches of A. bidentata samples were divided into three categories ,including N 1-N12 were clustered into one category ,N13-N28 were clustered into one category and N 29-N61 were clustered into one category. Seven marker wave numbers affecting the quality were selected. The corresponding wave numbers of VIP from large to small were 1 059,927,2 933,813,1 732,1 128 and 3 367 cm-1,1 732 cm-1 was the characteristic obsorption peak of saponins ,1 059,1 128,927 cm-1 were the characteristic obsorption peaks of glycosides. CONCLUSIONS Infrared fingerprint combined with normal distribution analysis ,cluster analysis ,principal component analysis and orthogonal partial least squares-discriminant analysis can be used to identify A. bidentata from different producing areas.

5.
China Pharmacy ; (12): 319-325, 2022.
Article in Chinese | WPRIM | ID: wpr-913090

ABSTRACT

OBJECTIVE To establish the HPLC fingerprint of Mongolian medicine Sanzisan ,and to evaluate its internal quality by chemical pattern recognition technique comprehensively. METHODS HPLC method was used. Using geniposide as reference,HPLC fingerprints of 15 batches of Sanzisan were drawn with Similarity Evaluation System of TCM Chromatogram Fingerprint(2012 edition). Similarity evaluation and common peaks identification were conducted. Combined with cluster analysis (CA),principal component analysis (PCA),and orthogonal partial least squares-discriminant analysis (OPLS-DA),the quality of 15 batches of Sanzisan was evaluated ,and the differential markers that affected its quality were screened. RESULTS There were 29 common peaks in 15 batches of Sanzisan ,and the similarity was no less than 0.952,indicating that the chemical composition of the 15 batches of Sanzisan had good consistency. A total of 13 common peaks were identified ,which were chebulic acid ,gallic acid,punicalin,punicalagin A ,punicalagin B ,jasminoside B ,caffeic acid ,corilagin,geniposide,chebulagic acid ,1,2,3,4,6- O-galloylglucose,chebulinic acid ,ellagic acid. Both CA and PCA could divide 15 batches of Sanzisan into four categories ,and the classification results were consistent ,indicating that the quality of 15 batches of Sanzisan had certain differences. Fourteen differential markers (chebulic acid ,gallic acid ,ellagic acid ,etc)that lead to the quality difference between batches were screened out by OPLS-DA. CONCLUSIONS Established HPLC fingerprint analysis method is simple and stable. Combined with chemical pattern recognition analysis ,it can be used for the quality control of Sanzisan.

6.
China Pharmacy ; (12): 293-298, 2022.
Article in Chinese | WPRIM | ID: wpr-913086

ABSTRACT

OBJ ECTIVE To predict the quality marker (Q-Marker)of Forsythia suspensa . METHODS The fingerprints of 10 batches of F. suspensa were established by high performance liquid chromatography. The common peaks were confirmed. The candidate components of Q-Marker in F. suspensa were screened. The volatile oil of F. suspensa were analyzed by gas chromatography-mass spectrometry (GC-MS),and the candidate components of Q-Marker in volatile oil were screened. The network pharmacology analysis was performed for the candidate components of Q-Marker. The network diagram of the “candidate components of F. suspensa Q-Marker-target-pathway”was constructed to predict the Q-marker of F. suspensa . RESULTS & CONCLUSIONS Twenty-one common peaks were obtained for 10 batches of F. suspensa ,and four components were identified as phillyrin,forsythoside A ,pinoresinol-4-O-β-D-glucoside and rutin. Seven candidate components were obtained by GC-MS analysis,such as β-pinene,α-pinene,terpinen-4-ol,limonene,γ-terpinene,α-phellandrene,β-myrcene. By network pharmacology analysis, 16 key targets and 17 pathways were obtained. It was preliminarily predicted that phillyrin , forsythoside A , pinoresinol-4-O-β-D-glucoside,rutin,terpinen-4-ol,α-phellandrene,α-pinene and β-pinene were Q-marker of F. suspensa .

7.
China Pharmacy ; (12): 280-286, 2022.
Article in Chinese | WPRIM | ID: wpr-913084

ABSTRACT

OBJECTIVE To establish H PLC fingerprint of Rheum palmatum before and after steaming with wine ,and to determine the contents of 3 differential components. METHODS HPLC method was used to establish the fingerprints of 15 batches of R. palmatum (before wine-steaming )and prepared rhubarb (after wine-steaming )and the similarity evaluation was conducted. The chemical pattern recognition analysis was carried out by principal component analysis ,cluster analysis ,partial least squares- discriminant analysis and orthogonal partial least squares-discriminant analysis. The contents of gallic acid ,resveratrol-4′-O- glucoside and resveratrol- 4′-O-(6″-galloyl)-glucoside in 30 batches of samples were determined. RESULTS In the fingerprint study,48 common peaks were demarcated for R. palmatum and 47 for prepared rhubarb as well as 17 common peaks were identified by reference substance. Cluster analysis and principal component analysis showed that R. palmatum derived from Qinghai before and after steaming with wine could be distinguished from those from Sichuan and Gansu. The results of content determination showed that the contents of 3 differential components in R. palmatum derived from Qinghai before and after steaming with wine were higher than those from other two production areas ;the contents of gallic acid in prepared rhubarb derived from those production areas were higher than R. palmatum ;the contents of resveratrol- 4′-O-glucoside and resveratrol- 4′-O- (6″-galloyl)-glucoside in R. palmatum derived from those production areas were higher than prepared rhubarb. CONCLUSIONS Fingerprint and content determination method established in this study can quickly ,scientifically and accurately evaluate the quality of R. palmatum from different producing areas before and after wine steaming ,which provide a basis for the processing specification and quality control of R. palmatum .

8.
China Pharmacy ; (12): 32-37, 2022.
Article in Chinese | WPRIM | ID: wpr-907009

ABSTRACT

OBJECTIVE To study the spectru m-toxicity relationship of in vitro hepatotoxicity of aqueous extract from Euodia rutaecarpa. METHODS The aqueous extract from 16 batches of E. rutaecarpa from different habitats were prepared. The fingerprints of aqueous extract from E. rutaecarpa were established by ultra high performance liquid chromatography (UPLC) method and Similarity Evaluation System of TCM Fingerprint (2012A edition ),and common peaks were identified and the similarity was evaluated. Using normal human hepatocytes L 02 as subject ,inhibitory effect of aqueous extract from 16 batches of E. rutaecarpa to them were investigated. The spectrum-toxicity relationship of UPLC fingerprint of aqueous extract from E. rutaecarpa with the hepatotoxicity of hepatocytes L 02 was analyzed by grey relational analysis (GRA)and partial least squares regression analysis (PLSR). The corresponding compound of the chromatographic peak with the greatest correlation with the in vitro hepatotoxicity of E. rutaecarpa were isolated ,prepared and identified. RESULTS There were 27 common peaks in UPLC fingerprints of aqueous extract from 16 batches of E. rutaecarpa ,with similarity of 0.375-0.995. Totally 9 peaks were confirmed ,i.e. neochlorogenic acid (peak 5),chlorogenic acid (peak 9),cryptochlorogenic acid (peak 10),caffeic acid (peak 12),rutin (peak 16),hyperin(peak 17),dehydroevotarine(peak 19),evotarine(peak 24),rutecarpine(peak 25). The aqueous extract from 16 batches of E. rutaecarpa showed significant inhibitory effect on the growth of L 02 cells(P<0.05 or P<0.01),and the inhibitory rate ranged from 6.68% to 67.95%. GRA showed that there were 18 common peaks with correlation degree greater than 0.8,which were peak 8>peak 3>peak 23>peak 7>peak 4>peak 9>peak 12>peak 2>peak 19>peak 6> 4928381。E-mail:799247687@qq.com peak 15>peak 5>peak 1>peak 17>peak 21>peak 26> peak 20>peak 14 in descending order of correlation degree. PLSR showed that there were 14 peaks with regression coefficient>0 and variable importance projection value >1,and the order of regression coefficient was peak 8>peak 3>peak 23> peak 2>peak 7>peak 4>peak 12>peak 9>peak 19>peak 5>peak 17>peak 26>peak 10>peak 15. Peak 8 had the greatest correlation with in vitro hepatotoxicity,and the corresponding compound of this peak was identified as 6-O-trans caffeoyl gluconic acid. CONCLUSIONS The in vitro hepatotoxicity of aqueous extract from E. rutaecarpa is the result of multiple component interaction,among which 6-O-trans caffeoyl gluconic acid shows closest relation with in vitro hepatotoxicity.

9.
China Pharmacy ; (12): 861-866, 2022.
Article in Chinese | WPRIM | ID: wpr-923194

ABSTRACT

OBJECTIV E To optimize the s alt-processing technology of Rosa laevigata ,and to study high performance liquid chromatography(HPLC)fingerprints and chromaticity values of R. laevigata before and after salt-processing. METHODS The comprehensive scoring method was adopted to optimize the salt-processing technology of R. laevigata using appearance character , moisture and polysaccharide content as index. Fingerprints were established by HPLC method before and after salt-processing ,and chromaticity values (L*,a*,b*)of the powder before and after salt-processing were determined. The multivariate statistical analysis was carried out for raw product and salt-processing product of R. laevigata by using common peak areas and chromaticity values as index. RESULTS The optimal salt-processing technology of R. laevigata was to mix it with appropriate amount of salt water ,place them in the preheated frying wok at 140 ℃,fry them for 25 min,and rotate frying wok 20 times/min. Ten common peaks were calibrated by HPLC fingerprints before and after salt-processing ,and 3 components were identified ,such as gallic acid ,catechin and ellagic acid. The chromaticity values L*,b* and E* changed significantly after salt-processing. The multivariate statistical analysis method could distinguish raw products and salt-processing products into two categories ,in which peaks 1,5,6 and 10 and chromaticity values b* and E* were important characteristic factors. CONCLUSIONS The optimized salt-processing technology is stable and reliable ,and the established fingerprint has good repeatability and stability. Fingerprint and chromaticity values combined with multivariate statistical analysis can provide reference for the identification and quality analysis of R. laevigata before and after salt-processing.

10.
China Pharmacy ; (12): 808-812, 2022.
Article in Chinese | WPRIM | ID: wpr-923185

ABSTRACT

OBJECTIVE To establish the method for t he content determination of 5 active components in Yixin badiran jibuya granules and their fingerprints. METHODS High performance liquid chromatography method was adopted to determine the contents of luteolin- 7-O-β-D-glucuronide(LG),apigenin-7-O-glucuronide(APG),rosmarinic acid (RA),diosmetin-7-O-β-D-glucuronide (DG)and tilianin (TL)in 10 batches(No. S 1-S10)of Yixin badiran jibuya granules. The fingerprints of 10 batches of Yixin badiran jibuya granules were drawn by Similarity Evaluation System of Chromatographic Fingerprint of Traditional Chinese Medicine(2004 A edition ),and similarity evaluation and cluster analysis were also performed. RESULTS The contents of LG , APG,RA,DG and TL in 10 batches of Yixin badiran jibuya granules were 0.279 5-0.449 9,0.082 4-0.135 3,0.184 8-0.472 1, 0.149 0-0.332 6,0.311 2-0.623 3 mg/g,respectively. A total of 13 common peaks were demarcated in the fingerprints and were identified as LG (peak 2)APG(peak 6),RA(peak 7),DG(peak 8),TL(peak 11). The similarity ranged from 0.598 to 0.990. The results of cluster analysis showed that S 6-S10 were clustered into one category and S 1-S5 were clustered into one category. CONCLUSIONS Established method for content determination and fingerprints can be used for the quality control for Yixin badiran jibuya granules.

11.
China Pharmacy ; (12): 706-712, 2022.
Article in Chinese | WPRIM | ID: wpr-923006

ABSTRACT

OBJE CTIVE To establish a method for quality evaluation of Xin ’an capsule by combining fingerprint , multi-component quantitative analysis and chemical pattern recognition analysis. METHODS High performance liquid chromatography(HPLC)combined with Similarity Evaluation System of TCM Chromatogram Fingerprint (2012 edition)were used to establish the fingerprints of 24 batches of Xin ’an capsules and evaluate the similarity. The common peaks were determined. The contents of glucosylvitexin ,rhamnosylvitexin,vitexin,hyperoside and isoquercetin in Xin ’an capsules were determined by the same HPLC method. Taking the common peak area of fingerprint as the variable ,MetaboAnalyst 5.0 tool was used to draw the cluster analysis (CA)heat map. SIMCA 14.1 software was used to perform principle component analysis (PCA)and partial least squares-discriminant analysis (PLS-DA). RESULTS Twelve common peaks were identified with the similarity greater than 0.97. Six common peaks were identified as chlorogenic acid ,glucosylvitexin,rhamnosylvitexin,vitexin,hyperoside and isoquercetin.The linear range of glucosylvitexin ,rhamnosylvitexin,vitexin, hyperoside and isoquercetin were 2.36-151.35,9.15-585.20, 1.20-76.50, 0.68-43.20, 0.44-27.90 µg/mL(all r>0.999).RSDs of precision ,repeatability and stability (24 h)tests were 163.com all less than 2.00% . The average recoveries were 95.80%(RSD=0.96% ,n=6),102.10% (RSD=0.93% ,n=6), 103.26%(RSD=1.28%,n=6),103.89%(RSD=0.73%,n=6) and 102.09%(RSD=1.79%,n=6),respectively. The contents of the five components were 0.988 8-1.559 1,4.336 6-11.220 1, 0.065 1-0.830 5,0.043 8-0.692 5 and 0.023 2-0.427 2 mg/grain,respectively. The results of CA and PCA showed that 24 batches of samples could be divided into three categories ,i.e. S 1-S15,S16-S18 and S 19-S24. PLS-DA showed that variable importance in projection values of the corresponding component of peak 6 and glucosylvitexin (peak 7),rhamnosylvitexin(peak 8),hyperoside (peak 10) and isoquercetin (peak 11) were greater than 1. CONCLUSIONS The established HPLC fingerprint and multi-component quantitative method are simple and feasible. Combined with chemical pattern recognition analysis ,it can be used for the quality control of Xin ’an capsules. Glucosylvitexin ,rhamnosylvitexin and other components may be differentital markers affecting the quality of each batch of samples.

12.
China Pharmacy ; (12): 673-679, 2022.
Article in Chinese | WPRIM | ID: wpr-923001

ABSTRACT

OBJECTIVE To establis h the fingerprint of Cynanchum auriculatum,to conduct its chemical pattern recognition analysis,and to determine the contents of four components at the same time. METHODS High performance liquid chromatography (HPLC)method was adopted. The determination was performed on ACE UExcel C 18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid solution (gradient elution )at the flow rate of 1.2 mL/min. The determination wavelength was set at 210 nm,and the column temperature was 40 ℃. The sample size wa s 10 μL. Taking qingyang shengenin as the reference ,HPLC fingerprints of 16 batches of C. auriculatum medicinal materials were drawn and similarity was evaluated by using the Similarity Evaluation of Chromatographic Fingerprints of Traditional Chinese Medicine (2012 edition), and the common peaks were determined. SPSS 26.0 software andSIMCA 14.0 software were used for cluster analysis ,principal component analysis and orthogonal partial least squares- discriminant analysis. The differential components affecting the quality of C. auriculatum were screened by taking the value of variable importance in projection (VIP)greater than 1 as the standard ;same HPLC method was used to determine the contents of syringic acid ,acyl asclepiadelenin ,baishouwubenzophenone and qingyang shengenin. RESULTS There were 29 common peaks in 16 batches of C. auriculatum ,with a similarity of 0.723-0.998. Four common peaks were identified ,namely syringic acid (peak 7),acyl asclepiadoidin (peak 9),baishouwubenzophenone(peak 13)and qingyang shengenin(peak 15). The results of cluster analysis showed that 16 batches of C. auriculatum could be clustered into three categories ,among which S 1 were grouped into one category,S3 were grouped into one c ategory,S2,and S 4-S16 were grouped into one category. The results of principal component analysis showed that the cumulative variance contribution rate of the five principal components was 88.706%,and the classification results were consistent with the results of cluster analysis. The results of orthogonal partial least squares-discriminant analysis showed that the common peaks (from large to small )with VIP value greater than 1 were peak 20,peak 10,peak 25,peak 12, peak 15(qingyangshengenin),peak 21,peak 14,peak 16,peak 26,peak 22 and peak 17. The linear ranges of syringic acid,acyl asclepterin,baishouwubenzophenone and qingyangshengenin were 0.715 3-45.778 0,2.379 4-152.281 0,0.642 0- 41.085 0,14.541 6- 930.662 0 µg/mL respectively (all R 2>0.999). The quantitative limits were 0.357 7,0.475 9,0.642 0 and 2.423 6 μg/mL;the detective limits were 0.146 0,0.164 1,0.248 8 and 0.833 3 μg/mL,respectively. RSDs of precision ,repeatability and stability (24 h)tests were less than 3%;the average recoveries were 99.11%(RSD=2.00%,n=9),98.54%(RSD=2.21%,n=9), 96.33%(RSD=2.54%,n=9)and 95.96%(RSD=2.93%,n=9);the contents were 17.12-147.80,95.23-583.10(S8 below the quantitative limit ),16.91-210.88 and 211.68-3 587.15(S1 below the quantitative limit )μg/g,respectively. CONCLUSIONS Established HPLC fingerprint and the method of content determination are stable ,reliable,accurate and reproducible. Combined with analysis of chemical pattern recognition ,it can be used for the quality control of C. auriculatum .

13.
Acta Pharmaceutica Sinica ; (12): 474-479, 2022.
Article in Chinese | WPRIM | ID: wpr-922920

ABSTRACT

In this paper, the low-field nuclear magnetic resonance technology CPMG (Carr-Purcell-Meiboom-Gill) echo method was used to determine the cross-linking degree and cross-linking density of crospovidone (PVPP) from different manufacturers. Based on the seven physical properties of PVPP, a fingerprint spectrum (radar chart) of twenty secondary quality indicators were obtained, and three compressibility evaluation indicators, index of the parameter (IP), index of parametric profile (IPP), index of good compression (IGC) were calculated by the fingerprint spectrum. It was found that the cross-linking degree and compressibility index IP of PVPP showed a strong correlation (r = 0.816) by the correlation analysis, indicating that the cross-linking degree is one of the key quality attributes for evaluating the compressibility of PVPP.

14.
Acta Pharmaceutica Sinica ; (12): 766-774, 2022.
Article in Chinese | WPRIM | ID: wpr-922889

ABSTRACT

Aa a characteristic medicinal plant in China, Gentiana rigescens Franch. has the function of protecting the liver and invigorating the spleen. At present, there are a few studies on the content determination method of characteristic components of G. rigescens, so it is necessary to establish a scientific and effective quality control method; In this study, The high performance liquid chromatography (HPLC) fingerprint of G. rigescens was established, based on literature reviewed and characteristic spectrum identified, the source range of G. rigescens quality marker (Q-marker) was screened. The effectiveness of the ingredients and the corresponding targets and pathways was analyzed through network pharmacology, and drew the diagram of ''component-target-pathway''. Qualitative and quantitative analysis of G. rigescens was performed by HPLC, and screen the main marker components leading to the differences between groups which were determined the Q-marker of G. rigescens; The literature and HPLC had determined that five iridoids were the main source of G. rigescens Q-marker. The network pharmacology (effectiveness) and qualitative and quantitative (detectability) analysis of G. rigescens from different producing areas confirmed that gentiopicroside, swertiamarin, and sweroside can be used as the main landmark components, and there were significant differences in their contents among different producing areas; The analysis of G. rigescens from different producing areas was carried out by network pharmacology and chemical fingerprints, it is confirmed can be used as potential Q-marker to provide sufficient theoretical basis for the quality control of G. rigescens in the later period.

15.
China Pharmacy ; (12): 586-591, 2022.
Article in Chinese | WPRIM | ID: wpr-920729

ABSTRACT

OBJECTIVE To establish HPLC finger print of Leonurus japonicus granules,and to determine the contents of 4 index components such as leonurine hydrochloride ,ferulic acid ,rutin,hyperoside. METHODS The determination was performed on Inertsil TM ODS-3 column with mobile phase consisted of acetonitrile (A)-0.1% formic acid solution (B)in the form of gradient elution;the flow rate was 1.0 mL/min,the detection wavelength was 280 nm,the column temperature was 25 ℃,and the sample size was 5 µL. Similarity Evaluation System of Chromatogram Fingerprint of TCM (2012 edition)was used for establishing the HPLC fingerprints of 10 batches of L. japonicus granules and analyzing their similarities. By comparing with HPLC fingerprints of reference substance ,the common peaks were identified. SPSS 25.0 and SIMCA 13.0 software were used for cluster analysis and principal component analysis ;the above HPLC method was used for the content determination of 4 index components in L. japonicus granules such as leonurine hydrochloride ,ferulic acid ,rutin,hyperoside. RESULTS HPLC fingerprints of 10 batches of L. japonicus granules were established ,and 16 common peaks were matched ,and 4 peaks identified were leonurine hydrochloride (peak 6),ferulic acid (peak 13),rutin(peak 14),hyperoside(peak 16);the similarities of 10 batches of samples were all higher than 0.970. The 10 batches of samples could be divided into four categories by cluster analysis and principal component analysis;the classification results were consistent. The contents of leonurine hydrochloride ,ferulic acid ,rutin and hyperoside were 122.10-138.82 μ g/g,9.33-10.45 μ g/g,14.12-18.95 μ g/g,5.87-8.06 μ g/g,respectively. CONCLUSIONS Established HPLC fingerprint of L. japonicus granules and the method for the content determination of 4 index components are simple and easy to operate,and have high precision and good repeatability ,which provide reference for the quality evaluation of L. japonicus granules.

16.
China Pharmacy ; (12): 575-578, 2022.
Article in Chinese | WPRIM | ID: wpr-920727

ABSTRACT

OBJECTI VE To establish the high performan ce liquid c hromatography(HPLC)fingerprint of carotenoid in Lycium barbarum,and to investigate the spectrum-effect relationship between its common peak and antioxidant activity. METHODS HPLC method was adopted. The fingerprints of carotenoid in 34 batches of L. barbarum from different producing areas were established by Similarity Evaluation System of TCM Fingerprint (2012 edition),and similarity evaluation and common peak identification were carried out. Taking scavenging rate of DPPH free radical as index ,in vitro antioxidant activity of carotenoid in L. barbarum was investigated. The spectrum-effect relationship between the common peaks of carotenoids in L. barbarum and antioxidant activity was analyzed by grey correlation method. RESULTS There were 4 common peaks in the fingerprints of carotenoids in 34 batches of L. barbarum ,and the similarity was not less than 0.903. Peak 1 was identified as zeaxanthin ,and peak 4 as zeaxanthin dipalmitate. The scavenging rates of them to DPPH free radical were 1.792%-3.160%. The common peaks of carotenoids in L. barbarum were positively correlated with scavenging rate of DPPH free radical ,and the correlation degree was greater than 0.6;the correlation degree of peak 2 and peak 4(zeaxanthin dipalmitate )with scavenging rate of DPPH free radical was greater than 0.8. According to the correlation degree ,the contribution of each common peak to scavenging rate of DPPH free radical was determined as peak 2> peak 4(zeaxanthin dipalmitate )>peak 1(zeaxanthin)>peak 3. CONCLUSIONS In this study ,HPLC fingerprint of carotenoid in L. barbarum is successfully established ,and two common peaks are identified. The chemical components represented by peak 2 and zeaxanthin palmitate may be the material basis of antioxidant activity of carotenoid in L. barbarum .

17.
China Pharmacy ; (12): 569-574, 2022.
Article in Chinese | WPRIM | ID: wpr-920726

ABSTRACT

OBJECTIVE To compare t he diff erences of the fingerprint and in vitro antioxidant activity between decoction pieces of Polygonum cuspidatum by integrated technology of habitat processing and processing (short for IPDP )and traditional processing decoction pieces (short for TPDP ). METHODS Ten batches of IPDP and ten batches of TPDP were prepared by integrated technology and traditional technology ,respectively. HPLC method was used to establish and compare the fingerprints of IPDP and TPDP. The scavenging rates of DPPH free radical ,ABTS free radical ,superoxide free radical and hydroxyl free radical and reducing activity of Fe 3+ were detected for IPDP and TPDP. In vitro antioxidant activities were compared between IPDP and TPDP. RESULTS There were 11 common peaks in the fingerprints of IPDP and TPDP ,among which 17 came from IPDP and 13 came from TPDP. The peak heights of peak 6(polydatin)and peak 15(emodin-8-O-β-D-glucoside)in IPDP were significantly higher than those in the TPDP ,and the peak heights of peak 13(resveratrol),peak 17(emodin)and peak 19(physcion)in the TPDP were significantly higher than those in the IPDP. The results of in vitro antioxidant test showed that IPDP and TPDP had a certain scavenging capacity on DPPH free radical ,ABTS free radical ,superoxide free radical and hydroxyl free radicals ,and also had a certain reducing capacity on Fe 3+. CONCLUSIONS The integrated processing technology of P. cuspidatum has a good retention effect on the glycosides in P. cuspidatum ,and the in vitro antioxidant activity of IPDP is stronger than that of TPDP.

18.
China Pharmacy ; (12): 452-457, 2022.
Article in Chinese | WPRIM | ID: wpr-920462

ABSTRACT

OBJECTIVE To establish the fing erprint of Temurin- 5 powder,conduct chemical pattern recognition analysis ,and determine the contents of 4 components simultaneously. METHODS The fingerprints of 10 batches of Temurin- 5 powder were established and similarity evaluation was performed by using high performance liquid chromatography (HPLC)combined with the Similarity Evaluation System of Chromatographic Fingerprints of Traditional Chinese Medicine (2012 edition);common peaks were identified by comparing with mixed substance control. The common peaks were analyzed by systematic cluster analysis and principal component analysis with SPSS 26.0 software. The HPLC method was used to determine the contents of gallic acid , geniposide,chlorogenic acid and ellagic acid in 10 batches of samples. RESULTS A total of 15 common peaks were identified from the fingerprints of 10 batches of Temurin-5 powder,and the similarity was 0.997-0.999. It was identified that peak 1 was gallic acid ,peak 3 was geniposide ,peak 5 was chlorogenic acid and peak 12 was ellagic acid. Among the 10 batches of samples , S4 and S 9 were grouped into one category ,S6-S8 were grouped into one category ,and the other batches of samples were grouped into one category. The accumulative variance contribution rate of first three principal components was 89.245%. The linear ranges of gallic acid ,geniposide,chlorogenic acid and ellagic acid were 5.55-177.5,15.98-511.5,2.56-82.0 and 13.48-431.5 μg/mL, respectively. RSDs of precision ,stability(24 h)and repeatability tests were all less than 2%(n=6 or n=7). The average recoveries were 101.56%,102.21%,98.60% and 96.62%,respectively,RSDs were 1.90%,1.61%,1.58% and 1.73%(n=6). Average contents of above components were 5.03-5.64,10.38-12.16,1.40-1.69,6.47-7.11 mg/g,respectively. CONCLUSIONS The established fingerprint is stable and feasible ,and the content determination method meets the relevant regulations. Combined with chemical pattern recognition analysis ,it can be used for the quality control of Temurin- 5 powder.

19.
China Pharmacy ; (12): 439-451, 2022.
Article in Chinese | WPRIM | ID: wpr-920460

ABSTRACT

OBJECTIVE To establish the fingerprint of Zhuang medicine Jinmu granules and carry out chemometric analysis , and determine the contents of three components . METHODS High performance liquid chromatography (HPLC) method was adopted. Using rutin as the reference ,HPLC fingerprints of 10 batches of Jinmu granules were drawn and similarity evaluation was performed by Similarity Evaluation of Chromatographic Fingerprint of Traditional Chinese Medicine (2012 edition);the common peak was determined by comparing with mixed control ;SPSS 21.0 software was used for cluster analysis ,and SIMCA 14.1 software was used for principal component analysis and orthogonal partial least squares-discriminant analysis. The differential components affecting the quality of Jinmu granules were screened by taking the variable importance in projection (VIP)value >1 as the standard ;the HPLC method was used to determine the contents of astilbin ,polydatin and berberine hydrochloride in Jinmu granules. RESULTS There were 22 common peaks in 10 batches of Jinmu granules ,and the similarities were 0.962-0.997;five common peaks were identified ,namely gallic acid (peak 2),polydatin(peak 9),rutin(peak 11),astilbin(peak 13)and kaempferol (peak 20). The results of cluster analysis showed that 10 batches of Jinmu granules could be clustered into 3 categories:S1 and S 3-S4 were grouped into one category ;S5-S6 and S 9 were grouped into one category ;S2,S7-S8 and S 10 were grouped into one category. The results of principal component analysis showed that the parameter of model interpretation was 0.951 and that of prediction ability was 0.723. The classification results were basically consistent with cluster analysis. The classifica tion results of orthogonal partial least squares- com discriminant analysis were also ba sically consistent with clus- ter analysis. The common peaks with VIP value >1 in the order were peak 7>peak 11(rutin)>peak 17>peak 13(astilbin)> peak 3>peak 8>peak 6>peak 16 respectively. The linear ranges of astilbin ,polydatin and berberine hydrochloride were 0.012 6- 1.225 0,0.010 8-1.052 5 and 0.020 0-1.562 5 mg/mL,respectively(all R 2=0.999 9). RSDs of precision ,stability(24 h)and repeatability tests were all less than 3%. The average recoveries were 99.48%(RSD=2.67%,n=9),98.57%(RSD=1.77%,n= 9)and 100.84%(RSD=2.49%,n=9). The contents were 1.221 0-7.011 6,2.251 1-4.462 9,1.252 4-3.328 7 mg/g,respectively. CONCLUSIONS Established fingerprint and the method of content determination are accurate ,stable and simple. Combined with chemometric analysis ,it can be used for the quality control and evaluation of Zhuang medicine Jinmu granules.

20.
China Pharmacy ; (12): 425-432, 2022.
Article in Chinese | WPRIM | ID: wpr-920458

ABSTRACT

OBJECTIVE To determi ne the contents of total fla vonoids i n Scutellaria barbata standard decoction ,evaluate in vitro antioxidant activity ,establish the fingerprint and conduct chemical pattern recognition analysis. METHODS The contents of total flavonoids in S. barbata standard decoction (calculated by scutellarein )were determined by ultraviet-visible spectrophotometry. In vitro antioxidant activity of S. barbata standard decoction was investigated by free radical scavenging tests of 1,1-diphenyl- 2-trinitrophenylhydrazine(DPPH)and 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid )ammonium salt (ABTS);HPLC method was adopted. Using scutellarin as reference ,the fingerprints of 16 batches of S. barbata standard decoction were drawn and evaluated by Similarity Evaluation System of TCM Chromatogram Fingerprint (2004 A edition ),and the common peaks were determined;Pearson correlation analysis was carried out by using SPSS 24.0 software to screen substances with in vitro antioxidant activity. Taking them as variables ,cluster analysis and principal component analysis were carried out by using SPSS 24.0 and SIMCA 14.1 software. RESULTS The linear range of total flavonoids were 2.106-21.06 μg/mL(R2=0.999 3);RSDs of precision , reproducibility and stability tests (120 min)were all lower than 2%;the recovery was 100.62%(RSD=0.55%,n=6);the contents of total flavonoids were 0.634-1.053 mg/mL. Median inhibitory concentration (IC50) of DPPH radical scavenging experiment ranged 1.120-3.602 mg/mL,and IC 50 of ABTS radical scavenging e xperiment range d 0.684-1.327 mg/mL. The results of correlation analysis showed that the content of total flavonoids Δ 基金项目 :河北省高校省级重点学科建设项目 (No.冀教 in S. barbata standard decoction was negatively correlated 高〔2013〕4号);承德医学院自然科学研究计划项目(No.201824) *讲师,硕士。研究方向:中药质量控制 。电话:0314-2291186。 with the IC 50 of DPPH free radical and ABTS free radical E-mail:duyilongww@sina.com scavenging experiment ,and the correlation coefficients were # 通信作者 :教授,硕士。研究方向 :中药质量控制 。电话: -0.976 and -0.940 respectively(P<0.01). There were 18 0314-2291186。E-mail:phf2301@163.com common peaks in the fin gerprints of 16 batches of S. barbata 中国药房 2022年第33卷第4期 China Pharmacy 2022Vol. 33 No. 4 ·425· standard decoction ;the s imilarities were 0.964-0.997. A total of 4 common peaks were identified ,such as scutellarin (peak 8), scutellarein(peak 14),luteolin(peak 15),apigenin(peak 17).In the HPLC fingerprints of S. barbata standard decoction ,the peak areas of peak 3-4,8-9,12-15 and 17 were significantly negatively correlated with the IC 50 of DPPH free radical and ABTS free radical scavenging experiment (P<0.05). The results of cluster analysis showed that 16 batches of S. barbata standard decoction could be clustered into two categories ,of which S 2,S7-S8 and S 14-S16 were clustered into one category ,S1,S3-S6 and S 9-S13 were clustered into one category. By principal component analysis ,16 batches of S. barbata standard decoction were divided into two categories ,of which S 2,S4,S7 and S 14-S16 were clustered into one category ,and S 1,S3,S5-S6 and S 8-S13 were clustered into one. The comprehensive scores were high in the samples of S 4,S13,S15. CONCLUSIONS Established HPLC fingerprint and chemical pattern recognition analysis method can be used to evaluate the quality of S. barbata standard decoction ; peak 3-4,8-9,12-15 and 17 and total flavonoids are the potential material basis for S. barbata standard decoction to scavenge DPPH free radical and ABTS free radical.

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