Comparison of HPLC fingerprints and determination of main components of Viticis Fructus from different species / 中国中药杂志

In order to comprehensively evaluate the quality of Viticis Fructus, this study established HPLC fingerprints and evaluated the quality of 24 batches of Viticis Fructus samples from different species by similarity evaluation and multivariate statistical analysis(PCA, HCA, PLS-DA). On this basis, an HPLC method was established to compare the content differences of the main components, including casticin, agnuside, homoorientin, and p-hydroxybenzoic acid. The analysis was performed on the chromatographic column(Waters Symmetry C_(18)) with a gradient mobile phase of acetonitrile(A)-0.05% phosphoric acid solution(B) at the flow rate of 1 mL·min~(-1) and detection wavelength of 258 nm. The column temperature was 30 ℃ and the injection volume was 10 μL. The HPLC fingerprint of 24 batches of Viticis Fructus samples was established with 21 common peaks, and nine peaks were identified. Similarity analysis was carried out based on chromatographic data of 24 batches of chromatographic data of Viticis Fructus, and the results showed that except for DYMJ-16, the similarity of Vitex trifolia var. simplicifolia was ≥0.900, while that of V. trifolia was ≤0.864. In addition, the similarity analysis of two different species showed that the similarity of 16 batches of V. trifolia var. simplicifolia was 0.894-0.997 and that of the eight batches of V. trifolia was between 0.990 and 0.997. The results showed that the similarity of fingerprints of these two species was different, but the similarity between the same species was good. The results of the three multivariate statistical analyses were consistent, which could distinguish the two different species. The VIP analysis results of PLS-DA showed that casticin and agnuside contributed the most to the distinction. The content determination results showed that there was no significant difference in the content of homoorientin and p-hydroxybenzoic acid in Viticis Fructus from different species, but the content of casticin and agnuside was significantly different in different species(P<0.01). The content of casticin was higher in V. trifolia var. simplicifolia, while agnuside was higher in V. trifolia. The findings of this study show that there are differences in fingerprint similarity and component content of Viticis Fructus from different species, which can provide references for the in-depth study of the quality and clinical application of Viticis Fructus.

Complanatoside A and complanatoside B in rats administered with raw and salt-processed Astragali Complanati Semen: a pharmacokinetics study / 中国中药杂志

An UPLC-MS/MS method was developed to simultaneously determine complanatoside A and complanatoside B in rat plasma with rutin as the internal standard and applied to examine the effect of salt-processing on pharmacokinetics of these two flavonoid glycosides. The pharmacokinetic parameters were estimated using DAS 3.2.6 and subjected to independent sample t-test with SPSS 23.0. No significant difference in T_(max) of complanatoside B was observed between the raw and processed groups; however, in the processed group, C_(max) and AUC_(0-12 h) of complanatoside B increased obviously(P<0.05), while MRT_(0-12 h) decreased from(3.34±0.44) h to(1.81±0.36) h(P<0.05). C_(max) [(14.72±11.13) μg·L~(-1)] and MRT_(0-24) [(3.93±0.26) h] of complanatoside A in the raw group were statistically different from those [(35.64±21.99) μg·L~(-1),(1.43±0.24) h] in the processed group(P<0.05). As a result, salt-processing can facilitate the in vivo adsorption and accelerate the excretion of complanatoside A and complanatoside B.

Comparison of UPLC Fingerprint and Determination of Index Components Before and After Processing of Cyperi Rhizoma Processed with Four Excipients / 中国实验方剂学杂志

Objective:To study the quality evaluation method of Cyperi Rhizoma processed with four excipients. Method:Ultra-performance liquid chromatography （UPLC） fingerprints of raw products and processed products with four excipients of Cyperi Rhizoma were established， and the changes of chemical components in the fingerprints before and after processing were compared by chemometric analysis. The mobile phase was consisted of methanol （A）-water （B） for gradient elution （0-10 min， 5%-40%A； 10-30 min， 40%-70%A； 30-40 min， 70%A） at a flow rate of 0.3 mL·min^-1. The injection volume was 3 μL， the column temperature was 35 ℃， and the detection wavelength was 280 nm. The content changes of main index components in Cyperi Rhizoma before and after processing were compared by UPLC. The mobile phase was methanol-water （75∶25） and the detection wavelength was 242 nm. Result:Processing with four excipients had a significant impact on the overall characteristics of chemical components in the fingerprint of Cyperi Rhizoma. A total of 28 characteristic peaks were identified in fingerprints of the raw and processed products. Among them， peaks 1， 2 and 4 were specific peaks of the processed products， peak 5 was characteristic peak of the raw products. Peak 2 was identified as 5-hydroxymethylfurfural， peak 24 as cyperenone and peak 27 as <italic>α</italic>-cyperone. The 5-hydroxymethylfurfural produced by the processing with four excipients came from rice vinegar， rice wine and Maillard reaction of polysaccharides in Cyperi Rhizoma. The results of determination showed that there was no significant difference in the content of cyperenone after processing， but the content of <italic>α</italic>-cyperone decreased significantly. Conclusion:In the process of Cyperi Rhizoma processed with four excipients， there are new components produced by structural transformation， which are accompanied by changes in the content of index components. In this study， the quality of raw and processed products of Cyperi Rhizoma can be rapidly and effectively evaluated from qualitative and quantitative aspects.

Comparison of UPLC Fingerprint and Determination of Main Components Before and After Processing of Artemisiae Argyi Folium Processed with Four Excipients / 中国实验方剂学杂志

Objective:To establish the ultra-performance liquid chromatography （UPLC） fingerprints of Artemisiae Argyi Folium and Artemisiae Argyi Folium processed with four excipients， and quantitatively analyze the 8 phenolic acids and flavonoids contained in them， in order to explore the quality evaluation method of Artemisiae Argyi Folium processed with four excipients. Method:UPLC was used with Shim-pack XR-ODS C₁₈ column （2.0 mm×75 mm， 2.2 µm）， mobile phase of acetonitrile （A） -0.2% formic acid aqueous solution （B） for gradient elution （0-1 min， 10%A； 1-2 min， 10%-15%A； 2-17 min， 15%-18%A； 17-24 min， 18%-28%A； 24-36 min， 28%-38%A； 36-41 min， 38%-60%A； 41-45 min， 60%-100%A）， detection wavelength of 330 nm and flow rate of 0.2 mL·min^-1. The UPLC fingerprints of Artemisiae Argyi Folium before and after processing were established， and analyzed by chemometrics. Contents of 5-caffeoylquinic acid， 3-caffeoylquinic acid， 4-caffeoylquinic acid， 3，4-dicaffeoylquinic acid， 3，5-dicaffeoylquinic acid， 4，5-dicaffeoylquinic acid， jaceosidin and epuatilin in the decoction pieces were determined. Result:The fingerprints of Artemisiae Argyi Folium before and after processing were established， and the UPLC characteristic chromatograms of Artemisiae Argyi Folium before and after processing had good consistency， and the similarity was >0.94. Compared with Artemisiae Argyi Folium， the contents of 3-caffeoylquinic acid and 3，4-dicaffeoylquinic acid had no significant change after processing， the contents of jaceosidin and epuatilin decreased after processing， while the contents of 5-caffeoylquinic acid， 4-caffeoylquinic acid and 4，5-dicaffeoylquinic acid increased significantly （<italic>P<</italic>0.01）， their average increasing rates were 32.50%， 66.83%， 29.39%， respectively. And content of 3，5-dicaffeoylquinic acid was significantly decreased （<italic>P<</italic>0.01） ， and the average reduction rate was 51.25%. Conclusion:The contents of chemical components in Artemisiae Argyi Folium and Artemisiae Argyi Folium processed with four excipients have changed to a certain extent. Among them， 5-caffeoylquinic acid， 3，5-dicaffeoylquinic acid， 4-caffeoylquinic acid and 4，5-dicaffeoylquinic acid can be used as the key indicators for quality evaluation of Artemisiae Argyi Folium before and after processing.

Analysis on Content Change and Transformation Rule of Main Characteristic Components in Stir-frying Process of Glycyrrhizae Radix et Rhizoma / 中国实验方剂学杂志

Objective::To study on the content change and transformation rule of eight main characteristic components in stir-frying process of Glycyrrhizae Radix et Rhizoma. Method::The contents of liquiritin apioside, liquiritin, isoliquiritin apioside, isoliquiritin, liquiritigenin, isoliquiritigenin, glycyrrhizic acid and glycyrrhetinic acid in Glycyrrhizae Radix et Rhizoma were determined simultaneously by HPLC. The chromatographic conditions were Waters Symmetry® C18 column (4.6 mm×250 mm, 5 μm), and the mobile phase of acetonitrile (A)-0.05%phosphoric acid solution (B) for gradient elution (0-9 min, 19%-25%A; 9-18 min, 25%-34%A; 18-38 min, 34%-51%A; 38-58 min, 51%-89%A), the flow rate of 1 mL·min-1, the detection wavelengths at 320 nm (0-16 min), 276 nm (16-25 min), 370 nm (25-28 min), 254 nm (28-58 min), the injection volume of 10 μL and the column temperature at 30 ℃. Result::After stir-frying, the total content of three components with dihydroflavone as mother nucleus was decreased, while the total content of three components with chalcone as mother nucleus showed an upward trend, the content change of glycyrrhizic acid was not obvious, but glycyrrhetinic acid content showed a slight upward trend. When the monomer heating temperature reached 130 ℃, dihydroflavones and chalcones could be isomerized with each other, and with the increase of temperature, the isomerization became more obvious. When the heating temperature rose to 180 ℃ (isoliquiritin apioside was 130 ℃), in addition to the isomerization, the glucosidic bond of flavonoid glycosides began to break and gradually transformed into the corresponding secondary glycosides or aglycones. Glucosidic bond of glycyrrhizic acid could also be broken to form glycyrrhetinic acid, which was detected at 150 ℃. Conclusion::The change of chemical composition is complex during stir-frying process of Glycyrrhizae Radix et Rhizoma, in addition to the isomerization and glucosidic bonds breaking observed in this experiment, there may be other complex reactions. The content of one compound in the herb is affected by many factors during its processing, such as the time and temperature of frying, the stability of the compound itself and so on.

Determination of Contents of Five Components in Descurainiae Semen Before and After Being Processed by HPLC / 中国实验方剂学杂志

Objective:HPLC for the determination of five components in Descurainiae Semen was established to investigate the change rule of contents of five components in the herb before and after being processed. Method:The contents of quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside(QGG),sinapic acid,quercetin-3-O-β-D-glucopyranoside(QG),isorhamnetin-3-O-β-D-glucopyranoside(IG) and 1,2-di-O-sinapoyl-β-D-glucopyranose(SG) was determined simultaneously by HPLC,the change rule of contents of these components before and after processing and its reasons were analyzed.Waters Symmetry® C18 column(4.6 mm×250 mm,5 μm) was employed,and the mobile phase was acetonitrile(A)-1% acetic acid aqueous solution(B) for gradient elution(0-5 min,5%-10%A;5-15 min,10%-13%A;15-23 min,13%-20%A;23-43 min,20%-25%A;43-46 min,25%A;46-55 min,25%-40%A;55-60 min,40%A).The flow rate was 1 mL·min-1.The detection wavelength was set at 265 nm,the injection volume was 10 μL,and the column temperature was 30℃. Result:Contents of the above five components before processing were 0.114 3%,0.041 6%,0.036 2%,0.022 6% and 0.097 6%;after processing,the contents of these five components turn into 0.107 4%,0.011 3%,0.034 2%,0.021 9% and 0.058 9%;among them,the contents of these five components decreased by 6.04%,72.84%,5.52%,3.10% and 39.65%,respectively. Conclusion:The contents of these five components in Descurainiae Semen is reduced to varying degrees after processing.The contents of phenylpropanoids decrease significantly,while the contents of flavonoid glycosides do not change significantly.

Quality Evaluation of Andrographis Herba Based On Electronic-eye Technique / 中国实验方剂学杂志

Objective: Taking electronic-eye (visual analyzer) technique,based on the powder color of Andrographis Herba,to investigate the applicability of electronic-eye technique and evaluate the quality of Andrographis Herba with different commercial specifications. Method: HPLC was employed to determine contents of andrographolide,dehydroandrographolide,14-deoxyandrographolide,neoandrographolide in 50 batches of Andrographis Herba with different commercial specifications(stems,leaves and aerial parts).Color of these samples were measured by electronic-eye technique.The data were analyzed by principal component analysis(PCA) and Pearson correlation analysis.The ability of electronic-eye to distinguish the different commercial specifications of Andrographis Herba was investigated and the correlation of chroma space system parameters (L*,a*,b*) with active components was investigated. Result: There was remarkable difference in contents of 4 diterpenoids in Andrographis Herba from different parts,their contents in leaves was the highest,followed by the aerial parts(mixture of stems and leaves),and their contents in stems was the lowest.The results of PCA was divided into two classes,namely the stem part,leaf and aerial parts,indicating that electronic-eye could be used to distinguish the quality of Andrographis Herba.The correlation results showed that there were significant negative correlation(PL*(lightness value) and the contents of andrographolide,dehydroandrographolide,14-deoxyandrographolide,neoandrographolide and the total content of these 4 components.In addition,L* of samples that did not conform to the lower limit of determination in the 2015 edition of Chinese Pharmacopeia was ≥ 69.5,and the L* of more than 90% of the samples in accordance with the requirements was Conclusion: Electronic-eye technique provides a new method and idea for the quality evaluation of Andrographis Herba.

Chemical study on Cassiae Semen processing procedure / 中国中药杂志

References and our previous experiment showed that the contents of glycosides were significantly decreased，while the contents of aglycones were significantly increased after processing of Cassiae Semen.It may be related to its glycosidases or the heating process. In order to investigate the reasons, high performance liquid chromatographic (HPLC) was used to study the effects of these two factors on contents of Cassiae Semen's main chemical components in processing. The results showed that glycoside hydrolases was present in Cassiae Semen and could rapidly hydrolyze glycosides from Cassiae Semen into aglycones in suitable temperature with sufficient water.However，it didn't show effect on contents change of main constituents in the procedure of Cassiae Semen processing.The reason for content decrease of glycosides and content increase of aglycones in processed Cassiae Semen was glycoside bond cracking to produce corresponding aglycone at high temperature.This study further provides basis for further revealing of the processing mechanism of Cassiae Semen.

Chemical constituents from seeds of Astragali complanati / 中国中药杂志

A new flavonoid glycoside, named complanatoside C (1), and 19 known compounds (2-20) were isolated from an 95% ethanol extract of Astragali Semen by various chromatographic methods. Their structures were identified on the basis of UV, IR, NMR, MS spectroscopic data analysis, and comparison with those in literature, including fifteen flavonoid glycoside (1-15), and six other constituents (16-20), among which compounds 16-19 were isolated from this plant for the first time.

Discrimination of Descurainiae Semen and Pantagirus Semen by HPLC fingerprints / 中国中药杂志

<p><b>OBJECTIVE</b>To discriminate Descurainiae Semen and Pantagirus Semen.</p><p><b>METHOD</b>A high-performance liquid chromatographic method was developed to establish the fingerprint of Descurainiae Semen, and hierarchical cluster analysis (HCA) and partial least squares discriminant analysis (PLS-DA) were applied to study HPLC fingerprinting and chemical recognition.</p><p><b>RESULT</b>There exists large difference of chromatographic peaks and its relative peak area of HPLC fingerprints between Descurainiae Semen and Pantagirus Semen, and after conducting statistical analysis, the result demonstrated that all samples were classified into three categories: Descurainiae Semen, Pantagirus Semen and their mixtures.</p><p><b>CONCLUSION</b>The developed HPLC fingerprint combined with chemometrics can be utilized to discriminate between Descurainiae Semen and Pantagirus Semen, which was quick, simple, accurate and reliable an can provide the basis for the characterization and quality assess of Descurainiae Semen and Pantagirus Semen.</p>

Advances on Lepidii Semen and Descurainiae Semen / 中国中药杂志

"Tinglizi", the ripe seed of Descurainia sophia and Lepidium apetalum, is a member of Brassicaceae (Cruciferae). Traditionally, the former is called "Nantinglizi" (Descurainiae Semen) while the latter is called "Beitinglizi" (Lepidii Semen). In the theory of traditional Chinese medicine, it has the power to purge lung-fire, relieve dyspnea, promote diuresis and reduce edema, and it is mainly indicated in a case with phlegm-fluid accumulation, cough with excessive sputum, dyspnea with being unable to lie, and general swelling. In view of its wide-spread application in clinic, a comprehensive review of Lepidii Semen and Descurainiae Semen was conducted from the following aspects: herbalogical study, variety identification, historical evolution of processing, chemical constituents, pharmacological effects, quantitative determination and toxicity which could provide reference for further research and development of "Tinglizi".

Determination of five primary chemical constituents in Cassia angustifolia by HPLC / 中国中药杂志

<p><b>OBJECTIVE</b>To establish a method for determining the content of primary chemical constituents in the leaves of Cassia angustifolia.</p><p><b>METHOD</b>The HPLC with Diamonsil C18 (4.6 mm x 250 mm, 5 microm) column was used , acetonitrile-1% acetic acid (10:90-15: 85-18: 82-20: 80-25: 75) in a gradient manner was used as a mobile phase, with flow rate of 1 mL x min(-1), column temperature at 40 degrees C and detection wavelength at 270 nm.</p><p><b>RESULT</b>The results showed that 5 effective components all separated well and showed good linearity.</p><p><b>CONCLUSION</b>The method was proved to be rapid, sensitive, accurate, credible and repeatable. It can be applied to quality control of Folium Sennae.</p>

Determination of rubrofusarin gentiobioside in Cassia obtusifolia by HPLC / 中国中药杂志

<p><b>OBJECTIVE</b>To establish a method for determining the content of rubrofusarin gentiobioside in Cassia obtusifolia.</p><p><b>METHOD</b>The HPLC with Diamonsil C18 (4.6 mm x 250 mm, 5 microm) column was used, acetonitrile-THF-1% acetic acid (18: 3:79) was used as a mobile phase, with flow rate of 1 mL x min(-1), column temperature at 40 degrees 2 and detection wavelength at 278 nm.</p><p><b>RESULT</b>A good linearity was obtained from 0.1-0.5 microg with r = 0.999 9 for rubrofusarin gentiobioside. The average recovery was 101.1%, and RSD was 2.23% (n = 5).</p><p><b>CONCLUSION</b>The method was proved to be simple, rapid, sensitive, precise, reliable and repeatable. It can be applied to the quality control of Semen Cassia.</p>

Clustering analysis of HPLC chromatographic fingerprints of Paeonia suffruticosa / 中国中药杂志

<p><b>OBJECTIVE</b>To explore the utility of chromatographic data for quality control of Paeonia suffruticosa, a Chinese herbal medicine.</p><p><b>METHOD</b>Chromatographic fingerprints of Paeonia suffruticosa were determined by HPLC, the clustering analysis was used for data processing.</p><p><b>RESULT</b>The quantitative differences among different growing areas were found and could be used to classify herbals from different growing areas, while there seemed to be no quantitative differences for processing factor.</p><p><b>CONCLUSION</b>The method could be used in quality control for monitoring herbal quality control, and the result also suggested that different growing areas may greatly affected the herbal qualities.</p>

Quantititive study for chromatographic fingerprints of processed products of Paeonia lactiflora / 中国中药杂志

<p><b>OBJECTIVE</b>To explore the utility of Principal Factor Analysis (PFA) in chromatographic data for quality control.</p><p><b>METHOD</b>Chromatographic fingerprints of processed root pieces of Paeonia lactiflora were determined by HPLC, the PFA was used for data processing.</p><p><b>RESULT</b>The quantitative differences among different growing areas and different processing batches were found with the method.</p><p><b>CONCLUSION</b>The method could be used in quality control for monitoring between-batch products of traditional Chinese pharmaceutical process.</p>

Experimental study on processing of Paeonia lactiflora / 中国中药杂志

<p><b>OBJECTIVE</b>To provide experimental data for the quality control of processed Paeonia lactiflora, a Chinese herbal medicine.</p><p><b>METHOD</b>Traditional processing of P. lactiflora was simulated, content of paeoniflorin and water extracts among different preparations were assayed by HPLC; The quantitative correlations among different processing conditions were analyzed, the effects of processing parameters on the contents of paeoniflorin and water extracts were assayed a nanalysed.</p><p><b>RESULT AND CONCLUSION</b>The controlled processing parameters were correlated with covariables which showed that processing procedures was controllable, and the heating temperature was a factor impacting the content of paeoniflorin.</p>

Study on quality control of Paeonia lactiflora / 中国中药杂志

<p><b>OBJECTIVE</b>To provide the experimental data for the quality control of Paeonia lactiflora a prepared Chinese medicinal herb.</p><p><b>METHOD</b>The contents paeoniflorin among different growing areas and different processing methods methods were assayed by HPLC.</p><p><b>RESULT</b>The quantitative differences of paeoniflorin content among different growing areas and different processing methods wereanalyzed quantitatively.</p><p><b>CONCLUSION</b>The quantitative differences among different growing areas were not significant and the quantitative differences among different processing methods within 10%.</p>

Study on applying chromatographic fingerprints to establishing quality criterion of processed tuber of Pinellia pedatisecta / 中国中药杂志

<p><b>OBJECTIVE</b>To explore the utility of principal component analysis (PCA) in conjunction with the window preprocessing scheme on chromatographic data for quality control.</p><p><b>METHOD</b>Chromatographic fingerprints of processed tuber of Pinellia pedatisecta were determined by HPLC, and the Window Preprocessing and PCA were used for data processing.</p><p><b>RESULT</b>The quantitative differences among different growing areas and different process batches were found with this method.</p><p><b>CONCLUSION</b>The method can be used in quality control for monitoring between-batch products of traditional Chinese pharmaceutical process.</p>

Study on traditional Chinese pharmaceutical processing of radix Pinellia pedatisecta / 中国中药杂志

<p><b>OBJECTIVE</b>To study the effects of concentration, volume and temperature of aluminium water on the change of chromatoghraphic data of processed Rhizoina Arisaematis.</p><p><b>METHOD</b>Chromatographic fingerprints of processed Radix Pinellia pedatisecta were determined by HPLC, and multivariate analysis was made for data processing.</p><p><b>RESULT AND CONCLUSION</b>No change on the whole chromatoghraphic data was observed at different levels of concentrition and volume of aluminium water, while there was a great change at different levels of temperature.</p>