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Objective:To establish the fingerprints of Plantaginis Herba.Methods:The fingerprints were determined by UPLC. The peak areas of fingerprints of different parts and origins were analyzed by variance analysis and independent sample t-test. PCA, HCA, PLS-DA and other chemical patterns were analyzed by Simca14.1. The index weight was calculated by CRITIC, and the quality of plantain evaluation was combined with grey correlation degree.Results:The fingerprints of grass, stem, leaf and spike of Plantago depressa Willd. calibrated for 24, 16, 23 and 22 common peaks. The fingerprints of grass, stem, leaf and spike of Plantaginis Herba calibrated for 22, 10, 16 and 22 common peaks, and the fingerprints of commercial mixed plantain calibrated for 23 common peaks. 10 peaks were identified. The analysis of variance showed that there were differences in chromatographic peak areas between different parts of Plantago asiatica L. and Plantago depressa Willd.. And combinedede with PLS-DA, it showed that there were 16 important characteristic indexes in the classification, and the importance ranking was peak 3, 8, 28, 12, 14, 7, 5, 17, 6, 19, 23, 11, 22, 27, 9, 16. The quality evaluation results of critical method combined with grey correlation degree showed that among Plantago depressa Willd., Plantago asiatica L. and commercial mixed plantain herbs, the quality of Plantago asiatica L. was the best. Conclusion:The mixture of plantain exists in the market. The fingerprints established in this study can be used for the identification and quality evaluation of Plantaginis Herba from different sources.
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OBJECTIVE:To study the co rrelation of the chro maticity value of Schizonepeta tenuifolia charcoal of different processing time(0-40 min,similarly herein after)with multiple indicators ,and to reveal the quality change law of S. tenuifolia charcoal during processing and confirm the terminal time. METHODS :The contents of ethanol-soluble extracts from S. tenuifolia charcoal decoction pieces of different processing time were determined. UPLC fingerprint of S. tenuifolia decoction pieces and S. tenuifolia charcoal decoction pieces of different processing time were established ,and the similarity evaluation was also conducted. The chromatographic peaks were confirmed by comparison with substance control. The same UPLC conditions were used to determine the contents of index components (hesperidin,rosmarinic acid ,menthone)in S. tenuifolia charcoal decoction pieces of different processing time. The colorimetric method was used to measure the chromaticity value of S. tenuifolia charcoal decoction pieces of different processing time. Meanwhile ,sample of processing 0 min was used as a control to calculate the total color value (E)and the total color difference value (ΔE). Pearson correlation analysis ,cluster analysis and orthogonal partial least squares discriminant analysis (OPLS-DA)were performed on the ethanol-soluble extracts ,index component contents ,chromatographic peak area and chromaticity value. The terminal time of processing S. tenuifolia charcoal was conf irmed,and validation test was also conducted. RESULTS :With the extension of processing time , the content of ethanol-soluble extract in S. tenuifolia charcoal qq.com decoction pieces gradually decreased. A total of 17 chromato- graphic peaks were identified in 12 batches of S. tenuifolia decoction piece ,and its si milarity with the control fingerprint was greater than 0.9. 21 chromatographic peaks were identified in S. tenuifolia charcoal decoction pieces of different processing time,and its similarity with the chromatogram of sample of processing 0 min decreased with the processing time ,and the similarity after 18 min was lower than 0.9. The chromatographic peak 9 was hesperidin ,peak 10 was rosmarinic acid and peak 17 was menthone. The determination of content and chromaticity value showed that with the extension of processing time ,the contents of hesperidin ,rosmarinic acid and menthone decreased gradually ;the color L,b and E values of S. tenuifolia charcoal decoction piece powder decreased gradually ,and the a and ΔE values increased gradually. Pearson correlation analysis showed that the contents of ethanol-soluble extract ,hesperidin,rosmarinic acid and menthone ,the peak areas of 15 chromatographic peaks (peak 2,7-15,17-21)were significantly positively correlated with E value(P<0.01);the peak areas of 5 chromatographic peaks (peak 1,3-6)were significantly negatively correlated with E value(P<0.01),but peak area of peak 16 was not related to E value(P> 0.05). Results of cluster analysis showed that S. tenuifolia charcoal decoction pieces of different processing time were divided into 2 categories;the first category was processed for 0-16 min,and the second category was processed for 18-40 min. The results of OPLS-DA showed that the VIP values of peak 6 area(2.800 75),L value(2.327 54),peak 3 area(1.793 39),b value(1.735 78) and peak 5 area(1.244 04)were greater than 1. The final processing time of S. tenuifolia charcoal was 18 min. The results of validation experiment showed that the L,a and b values of S. tenuifolia charcoal decoction piece were 20.22-22.00,4.44-7.67, 9.78-13.00,and ΔE were 13.50-14.12,respectively. CONCLUSIONS :The chromaticity value of S. tenuifolia charcoal decoction pieces of different processing time is closely related to the contents of ethanol-soluble extract ,hesperidin,rosmarinic acid , menthone and the area of 20 chromatographic peaks. It is suggested that the terminal time of processing S. tenuifolia is 18 min.
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OBJECTIVE:To analysis the correlation between chrom aticity value and quality index of Atractylodis chinensis decoction piece powder stir-fired with bran ,and to determine its processing time. METHODS :The processed samples of 16 batches of A. chinensis decoction piece stir-fired with bran (S0-S15,S0 is the raw product of A. chinensis )were prepared ,and chromaticity values of all samples were determined ,such as lightness value (L*),yellow blue value (b*),red green value (a*). UPLC fingerprint of sample were analyzed ,and the contents of extract and volatile oil were also determined. Pearson correlation was used to analyze the correlation between the chromaticity value and quality index (relative peak area of each chromatographic peak in UPLC fingerprint ,water-soluble extract content ,alcohol-soluble extract content and volatile oil content ). Multivariate statistical analysis (principal component analysis ,cluster analysis ,partial least squares discriminant analysis )was carried out with chromaticity value and quality index ,and the processing time of A. chinensis decoction piece stir-fired with bran was determined by grey correlation method. RESULTS :In the process of bran frying ,with the extension of processing time ,L* and b* of decoction pieces powder decreased ,and a* increased first and then decreased ;relative areas of peak 1 and peak 2 increased first and then decreased,while relative areas of peak 3(5-hydroxymethyl furfural )increased,and the areas of the other peaks decreased. The content of the extract did not change significantly with time ,and the content of the volatile oil decreased. The results of correlation analysis showed that the relative peak area of peak 2-27,alcohol-soluble extract content and volatile oil content had a certain correlation with the chromaticity value ,while the relative peak area of peak 1 and water-soluble extract content had no linear correlation with the chromaticity value. Results of multivariate statistical analysis showed that the samples were divided into mild (S0-S5),excessive (S12-S15),moderate (S6-processing time of 18-33 min). The results of grey correlation method showed that the processing time of A. chinensis decoction piece stir-fired w ith bran should be controlled in the range of 18-24 min,and the optimal processing time was 18 min. CONCLUSIONS :There is a correlation between chromaticity value of A. chinensis decoction piece powder stir-fired with bran and the relative peak area of 27 chromatographic peaks ,and content of extract and volatile oil. It is suggested that the processing time should be 18 min.
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OBJECTIVE:To e stablish UPLC characteristics fingerprints of Lysimachia christinae ,and to simultaneously determine 3 effective components and to comprehensively evaluate the quality of L. christinae from different production areas. METHODS:UPLC method was adopted to establish characteristics fingerprint of the whole plant ,stem and leaves of 10 batches of L. christinae ,and determine the contents of kaemperfol- 3-O-rutinoside,quercetin,kaemperfol. The determination was performed on Waters CORTECS UPLC T 3 column with mobile phase consisted of acetonitrile- 0.2% phosphoric acid aqueous solution (gradient elution )at the flow rate of 0.2 mL/min. The detection wavelength was set at 364 nm,and column temperature was 30 ℃. The sample size was 1 µL. Similarity Evaluation System for TCM Chromatographic Fingerprint (2012 edition)was adopted to evaluate its similarity , and common peaks were confirmed. Using the contents of kaemperfol- 3-O-rutinoside, quercetin, kaemperfol,total ash ,acid-insoluble ash and sulfur dioxide residue ,the ethanol-soluble extract as index ,entropy weight TOPSIS was used to evaluate the overall quality of L. christinae comprehensively. RESULTS :There were 7 common peaks in the whole plant,stem and leaves of 10 batches of L. christinae ,among which 3 peaks were identified as kaemperfol- 3-O-rutinoside, quercetin and kaemperfol. The similarity of same part in the whole plant of L. christinae from different batches were not lower than 0.830. The similarity between stem and leaves of L. christinae in same batch was 0.504-0.859; the similarity between whole plant and stem was 0.593-0.904;the similarity between whole plant and leaves was 0.885-0.995. The linear ranges were 0.392 0-39.197 0 μg/mL for kaempferol-3-O-rutinoside, 0.397 0- 39.703 4 μg/mL for quercetin,0.380 9-38.093 0 μg/mL for kaempferol(r>0.999 0). RSDs of precision ,stability and repeatability tests were all lower than 2%. The recoveries were 96.43%(RSD=0.63%,n=9),100.32%(RSD=0.46%,n=9), 101.80%(RSD=0.32%,n=9),respectively. The content range of above components in L. christinae were 0.006 3%-0.041 1%, 0.002 9%-0.008 6%,0.004 4%-0.017 5%(stem);0.024 8%-0.290 5%,0.000 9%-0.009 0%,0.001 3%-0.012 4%(leaves); 0.007 9%-0.118 0%,0.001 5%-0.008 8%,0.002 8%-0.012 5%(whole plant ). There was no significant difference in the contents of 3 components in L. christinae among different producing areas (P>0.05). The order of the contents of kaempferol- 3-O- rutinoside in different parts of L. christinae was leaves >whole plant >stem. The contents of quercetin and kaempferol were high relatively in the stem. Results of entropy weight TOPSIS method showed that mean values of Ci for L. christinae from Zhongjiang county and Shuangliu county of Sichuan province ,Shizhu county of Chongqing city were 0.446,0.512,0.287. CONCLUSIONS : Established fingerprint and content determination method are stable and feasible ,and multi-index evaluation model constructed by characteristic chromatogram combined with entropy weight TOPSIS analysis method can be used for comprehensive quality evaluation of L. christinae . The quality of L. christinae from Sichuan province is better.
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OBJECTIVE:To establish an overall quality evaluation model for Agrimonia pilosa based on extract and characteristic spectrum,and to provide evidence for comprehensive quality evaluation of the medicinal material and screening of high-quality provenance. METHODS :Referring to different extraction method and solvent condition stated in 2015 edition of Chinese Pharmacopoeia (part Ⅳ),using the content and total peak area of HPLC characteristic chromatogram of extract as indexes,and the extraction technology was optimized by weighted comprehensive score. HPLC characteristic spectrum of 15 batches of A. pilosa was established ,and similarity evaluation and characteristic peak identification were performed. SPSS 25.0 software was used to conduct single factor analysis and Pearson correlation analysis for the extract content and total peak area of A. pilosa from different origins. The quality of medicinal materials from different origins were compared. Entropy weight TOPSIS method was adopted to evaluate comprehensive quality of A. pilosa using the extract content and total peak area of 15 batches of A. pilosa . RESULTS :The extraction technology of A. pilosa extract,which was extracted with hot dip plating using 50% ethanol as solvent ,was optimized. The similarity of 15 batches of A. pilosa was higher than 0.92,and 4 characteristic components were identified(ellagic acid ,quercetin,apigenin,kaempferol). There were significant differences in average extract content and total peak area of characteristic chromatogram of A. pilosa from different origins (P<0.05 or P<0.01),and there was a certain positive correlation between them (r=0.86,P<0.01). Results of entropy weight TOPSIS evaluation showed that the average Ci values of A. pilosa in Anhui ,Zhejiang,Sichuan,Henan and Jiangsu provinces were 0.689,0.351,0.218,0.308 and 0.361 respectively. CONCLUSIONS:The quality of A. pilosa from Anhui was the best ,that from Zhejiang and Jiangsu was better ,that from Henan was the second ,and that from Sichuan was poor. Established extraction technology and characteristic spectrum determination method of A. pilosa are stable and feasible. The entropy weight TOPSIS model is objective and quantifiable for comprehensive quality evaluation of A. pilosa ,and can effectively evaluate its quality.