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ObjectiveTo establish a high performance liquid chromatography（HPLC） fingerprint of Yanghetang benchmark sample， and evaluate its quality with chemometric methods， so as to provide a reference for the quality control of this benchmark sample. MethodHPLC was used to establish the fingerprint of Yanghetang benchmark sample with ZORBAX SB-C18 column（4.6 mm×250 mm， 5 μm）， the mobile phase was consisted of acetonitrile（A） -0.05% phosphoric acid aqueous solution （containing 0.05% triethylamine solution）（B） for gradient elution（0-5 min， 2%-3%A； 5-15 min， 3%-5%A； 15-65 min， 5%-30%A； 65-90 min， 30%-70%A）， the flow rate was 1.0 mL·min-1， the column temperature was 35 ℃， and the detection wavelength was 210， 260 nm. Traditional Chinese Medicine（TCM） Chromatographic Fingerprint Similarity Evaluation System （2012 edition） combined with cluster analysis， principal component analysis（PCA） and partial least squares-discriminant analysis（PLS-DA） were used to evaluate the quality differences between different batches of Yanghetang benchmark samples， and to find the main chemical components responsible for the quality differences. ResultHPLC fingerprint of Yanghetang benchmark sample was established， 13 common peaks were identified and attributed to each common peak， including peaks 2 and 8 from Rehmanniae Radix Praeparata， peaks 10 and 11 from Cinnamomi Cortex， peaks 1， 3-6 from fried Sinapis Semen， peak 13 from Ephedrae Herba， and peaks 7， 9， 12 from Glycyrrhizae Radix et Rhizoma. Eight of them were identified by comparing with control substance， which were 5-hydroxymethylfurfural（peak 2）， sinapine thiocyanate（peak 4）， glycyrrhizin（peak 7）， verbascoside（peak 8）， cinnamic acid（peak 10）， cinnamaldehyde（peak 11）， glycyrrhizic acid（peak 12） and ephedrine hydrochloride（peak 13）. The similarities of the HPLC fingerprints of 15 batches of Yanghetang benchmark samples with the control fingerprint were all greater than 0.80. The three chemometric methods could classify the samples into two categories. Eight differential components were screened out， among which 5-hydroxymethylfurfural， sinapine thiocyanate， verbascoside and ephedrine hydrochloride were identified. ConclusionThe established fingerprint analysis method is accurate， stable and reproducible， which basically reflects the overall chemical composition of Yanghetang benchmark sample， and can provide a basis for establishment of quality standards for compound preparations of this famous classical formula.
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OBJECTIVE@#Pseudostellaria heterophylla has been paid more attention in recent years, mainly as a medicine food homology plant. The content determination of P. heterophylla is not specified in the Chinese Pharmacopoeia (version 2020). The environmental conditions in different production areas could exert an influence on the quality of P. heterophylla. The purpose of this study is to discriminate P. heterophylla collected from different geographical origins of China.@*METHODS@#In this study, the content of polysaccharide in 28 batches of P. heterophylla was determined using phenol-sulfuric acid. HPLC fingerprints were established under optimised HPLC-PDA methods. Subsequently, the similarity analysis (SA) and the quantification of heterophyllin B were analyzed. The metabolites of P. heterophylla were identified and evaluated using UHPLC-Q Exactive HF orbitrap MS system. Principal component analysis (PCA), partial least squares discriminant analysis (PLS-DA), hierarchical cluster analysis (HCA) and orthogonal PLS-DA (OPLS-DA) were performed based on all peak areas.@*RESULTS@#The polysaccharide content in Guizhou and Jiangsu was higher than that of other production areas, which varied significant from different origins. While the content of heterophyllin B in Anhui and Jiangsu was high. The correlation coefficients of HPLC fingerprints for 28 batches samples ranged from 0.877 to 0.990, and the characteristic map can be used to identify and evaluate the quality of P. heterophylla. The samples from Fujian, Guizhou, Jiangsu provinces can be relatively separated using multivariate statistical analysis including PCA, PLS-DA, HCA, OPLS-DA, indicating that their metabolic compositions were significantly different. Ultimately, a total of 15 metabolites which were filtrated by a VIP-value > 1 and a P-value < 0.05 associated with the separation of different origins were identified.@*CONCLUSION@#HPLC fingerprint was established to evaluate the quality and authenticity of P. heterophylla. The present work showed that the difference of geographic distributions had an influence on the internal chemical compositions. A sensitive and rapid untargeted metabolomics approach by UHPLC-Q Exactive HF orbitrap MS was utilized to evaluate P. heterophylla from different origins in China for the first time. Overall, this study provides insights to metabolomics of P. heterophylla and supplies important reference values for the development of functional foods.
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Based on ITS sequences, the molecular identification of Cordyceps cicadae and Tolypocladium dujiaolongae was carried out, and high-performance liquid chromatography(HPLC) fingerprint combined with chemical pattern recognition method was established to differentiate C. cicadae from its adulterant T. dujiaolongae. The genomic DNA from 10 batches of C. cicadae and five batches of T. dujiaolongae was extracted, and ITS sequences were amplified by PCR and sequenced. The stable differential sites of these two species were compared and the phylogenetic tree was constructed via MEGA 7.0. HPLC was used to establish the fingerprints of C. cicadae and T. dujiaolongae, and similarity evaluation, cluster analysis(CA), principal component analysis(PCA), and partial least squares discriminant analysis(PLS-DA) were applied to investigate the chemical pattern recognition. The result showed that the sources of these two species were different, and there were 115 stable differential sites in ITS sequences of C. cicadae and T. dujiao-longae. The phylogenetic tree could distinguish them effectively. HPLC fingerprints of 18 batches of C. cicadae and 5 batches of T. dujiaolongae were established. The results of CA, PCA, and PLS-DA were consistent, which could distinguish them well, indicating that there were great differences in chemical components between C. cicadae and T. dujiaolongae. The results of PLS-DA showed that six components such as uridine, guanosine, adenosine, and N~6-(2-hydroxyethyl) adenosine were the main differential markers of the two species. ITS sequences and HPLC fingerprint combined with the chemical pattern recognition method can serve as the identification and differentiation methods for C. cicadae and T. dujiaolongae.
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Cromatografía Líquida de Alta Presión/métodos , Cordyceps/genética , Hypocreales , FilogeniaRESUMEN
Objective:To establish a method of measuring the contents of gallic acid, brevifolin, corilagin, geraniin, ellagic acid and rutin in Phyllanthus urinaria L. simultaneously with fingerprint study for analysis. Methods:Phyllanthus urinaria L. was extracted by ultrasound with 50% methanol. Chromatographic separation was performed on a Phenonmenex Luna C18 (4.6 mm×250 mm, 5 μm). The mobile phase consisted of acetonitrile (A) and 0.1% phosphoric acid aqueous solution (B) with gradient elution. The flow rate was 1.0 ml/min. The column temperature was 25 ℃, and the injection volume was 10 μl. The detection wavelength was 270 nm. HPLC fingerprints of Phyllanthus urinaria L. from different habitats was established. PCA and OPLS-DA were used to analyze the differences in chemical components of different habitats. Results:Gallic acid, brevifolin, corilagin, geraniin, ellagic acid and rutin showed good linearity at 0.042 8-0.641 6, 0.033 4-0.501 4, 0.142 2-2.133 1, 0.383 1-5.746 5, 0.063 1-0.946 2 and 0.019 2-0.287 8 μg, respectively. The average recovery rate of them was 103.65%, 96.39%, 101.85%, 95.04%, 98.79% and 98.33%, respectively. The HPLC fingerprints of different habitats contained 14 characteristic common peaks, and six compounds characteristic peaks were identified. PCA analysis showed that the chemical components of Phyllanthus urinaria L. from different habitats were different. Geraniin, ellagic acid and corilagin were screened by OPLS-DA. Conclusions:The method is efficient, accurate and sensitive, which can be used to measure the six components in Phyllanthus urinaria L.. The established HPLC fingerprint of different habitats combined with the measrurement method of six components can be used for the quality control and evaluation of Phyllanthus urinaria L..
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Objective:To establish a method for quality evaluation of Myristica fragrans Houtt. Methods:The common peak was determined with Dehydroisoeugenol as the reference peak, and the HPLC fingerprint of Myristica fragrans was established; then the common peaks were analyzed by High Resolution Liquid Chromatography-mass Spectrometry (HPLC-MS). The chemical components of the common peaks were identified through the calculation and data retrieval of the primary and secondary mass spectra of the characteristic peaks. Results:The HPLC fingerprint of Myristica fragrans was established, and the similarity degree of the 10 batches of samples was above 0.9 and 11 common peaks were established. According to the results of HPLC-MS, the components of 11 common peaks were identified as follow: Methyl eugenol (peak 1), Licarin A (peak 2), Myristol (peak 3), OdoratisolA (peak 4), 2-(3,4-Dimethoxyphenyl) butynoic acid (peak 5), Malabaricon D (peak 6), 5'-Methoxydehydroisoeugenol (peak 7), Dehydroisoeugenol (peak 8), Malabaricone C (peak 9), 4-Methoxy-6-{(2S,3S)-7-methoxy-3-methyl-5-[(1E)-1-propen-1-yl]-2,3-dihydro-1- benzofuran-2-yl}-1,3-benzodioxole (peak 10) and Licarin B (peak 11). Conclusions:The quality of Myristica fragrans could be evaluate with HPLC fingerprint method. HPLC-MS was used to analyze the chemical composition of complex components, which will provide reference for the identification and analysis of chemical components of the extracts and preparations of Traditional Chinese Medicine.
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ObjectiveTo investigate the intestinal absorption characteristics of multi-index components in Danggui Buxuetang with drug absorption simulating system （DASS） established by everted intestinal sac model. MethodThe intestinal absorption solution at different time points after administration of Danggui Buxuetang was collected and detected by high performance liquid chromatography （HPLC）， acetonitrile （A）-0.2% glacial acetic acid solution （B） was used as the mobile phase for gradient elution （0-16 min， 15%-23%A； 16-20 min， 23%-28%A； 20-25 min， 28%-30%A； 25-30 min， 30%A； 30-35 min， 30%-65%A； 35-45 min， 65%-95%A）， the detection wavelength was 302 nm. HPLC fingerprint of intestinal absorption solution was established and the common peak was calibrated， and the relative cumulative absorption rate of each index component was calculated. The relative cumulative absorption curves of components were fitted with various mathematical models by DDSolver 1.0 to explore the absorption law of different components. ResultThe absorption process of C2 （calycosin-7-glucoside） and C6 in Danggui Buxuetang was in line with zero-order equation， C9 was best fitted by Weibull equation， and the remaining 7 components were in line with Makoid-Banakar equation. C1 with C2， C3， C5， C7 and C10， C2 with C5 and C7， C3 with C4， C5， C7 and C10， C4 with C6 and C10， C5 with C7， C6 with C10， C7 with C10， C8 with C9 were absorbed simultaneously during the absorption process. With the prolongation of time， the overall cumulative absorption rate of Danggui Buxuetang increased. At 120 min， the overall cumulative absorption rate of Danggui Buxuetang exceeded 38%， and reached 49.14% at 180 min. ConclusionTen ingredients in Danggui Buxuetang are absorbed in the jejunum， but absorption law of various components is different， which shows that the intestinal absorption of compound preparations of traditional Chinese medicine （TCM） has multiple characteristics. Intestinal absorption study of TCM compound preparations with chemical composition as the index can reveal some of its absorption law， but it is not complete.
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ObjectiveTo establish an integrated method of fingerprint qualitative， multi-component quantitative analysis and chemometrics， and to evaluate the quality attributes and differences of Aurantii Fructus from different production areas and origins. MethodAnalysis was performed on COSMOSIL 5C18-MS-Ⅱ column （4.6 mm×250 mm， 5 μm） with the mobile phase of acetonitrile-0.2% phosphoric acid solution for gradient elution （0-4 min， 19%A； 4-5 min， 19%-21%A； 5-18 min， 21%A； 18-19 min， 21%-28%A； 19-27 min， 28%A； 27-28 min， 28%-40%A； 28-36 min， 40%A； 36-37 min， 40%-50%A； 37-42 min， 50%-60%A； 42-46 min， 60%-95%A； 46-55 min， 95%-100%A）， the flow rate was 1 mL·min-1， the column temperature was 30 ℃， the detection wavelength was set at 320 nm， and the injection volume was 10 μL. High performance liquid chromatography （HPLC） fingerprints of Aurantii Fructus from different production areas and origins were established. Then， the quality of 26 batches of samples was evaluated by cluster analysis （CA）， principal component analysis （PCA） and orthogonal partial least squares discriminant analysis （OPLS-DA）. A method for the determination of 12 components was developed and verified， and a thermal map-based CA of Aurantii Fructus from different production areas and origins was carried out based on the content difference of samples. ResultThe fingerprint and determination methods were well verified. The similarity of HPLC fingerprint of 12 batches of Aurantii Fructus was 0.85-0.996， 20 common peaks were calibrated and 14 of them were assigned. The resolution and linear relationship of 12 components in quantitative analysis were good. The recovery rates were 99.2%-101.0% with RSD≤2.0%. The results of CA， PCA and OPLS-DA indicated that the differentiation of Aurantii Fructus in different production areas was great， and there were differences among different cultivars. ConclusionThe qualitative analysis of fingerprint and quantitative analysis of multiple indexes based on the same chromatographic analysis conditions are convenient， accurate and reliable， and combined with chemometrics， the identification and quality analysis of Aurantii Fructus from different production areas and origins can be realized， which can provide reference for quality control and evaluation of Aurantii Fructus.
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There are two source plants for the traditional Chinese medicine Murrayae Folium et Cacumen (MFC) in Chinese Pharmacopoeia, i.e. Murraya exotica L. and M. paniculata (L.) Jack. Herein, a chemical comparison of M. exotica and M. paniculata by high performance liquid chromatography (HPLC) fingerprint analysis coupled with chemometrics and network pharmacology was performed. The main peaks in the fingerprints were identified by liquid chromatography coupled with ion trap/time-of-flight mass spectrometry (LC-IT-TOF-MS) and authenticated by references. The chemometrics results showed that the HPLC fingerprints of these two species were clearly divided into two categories using hierarchical cluster analysis (HCA) and principal component analysis (PCA), and a total of 13 significantly differentiated markers were screened out by orthogonal partial least squares-discriminant analysis (OPLS-DA). However, the following network pharmacology analysis showed that these discriminated markers were found to act via many common targets and metabolic pathways, indicating the possibly similar pharmacological effects and mechanisms for M. exotica and M. paniculata. The above results provide valuable evidence for the equivalent use of these two plants in clinical settings. Moreover, the chromatographic fingerprint analysis coupled with chemometrics and network pharmacology supplies an efficient approach for the comparative analysis of multi-source TCMs like MFC.
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To obtain the chemical profile of Tibetan medicinal plant ″Bangga″, the present study established the HPLC fingerprint of ″Bangga″ and inferred common chemical constituents of its two original plants, Aconitum tanguticum and A. naviculare by LC-MS. The HPLC analysis was performed on a Kromasil 100 C_8 column(4.6 mm×250 mm, 5 μm) with acetonitrile(A)-0.1% formic acid in water(B) as mobile phase in a gradient elution mode. Besides, the flow rate was set at 1 mL·min~(-1) and the column temperature was 35 ℃. The detection wavelength was set at 255 nm and the injection volume was 10 μL. Seventeen batches of ″Bangga″ samples were analyzed and the HPLC fingerprint was established under the above conditions. Similarity evaluation was performed using Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine(2012). As a result, 16 common peaks were selec-ted and the similarity values of 17 batches of ″Bangga″ were in the range of 0.702-0.966. Furthermore, one batch of A. tanguticum and one batch of A. naviculare were analyzed by LC-MS/MS and 74 common compounds were inferred, including 10 phenolic acids, 26 flavonoids, and 38 alkaloids. The established method, with good separation and strong specificity, is simple and feasible, and can be used for the quality control of ″Bangga″ and identification of its two original plants. A. tanguticum and A. naviculare are similar in chemical composition and component content, but are quite different in the content of flavonoids.
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Cromatografía Líquida de Alta Presión , Cromatografía Liquida , Medicamentos Herbarios Chinos , Plantas Medicinales , Espectrometría de Masas en Tándem , TibetRESUMEN
Objective: The chemical finger printing-based methods for evaluating TCMs quality can report partial of TCMs quality without linking to effective constituents. In this study, a mathematical model was established for the quality evaluation of total saponins of Panax japonicus (TSPJ), a folk medicine in China and Japan for treating diseases, through coupling the dynamic changes of chemical constitutions with corresponding activities. Methods: High-performance liquid chromatography (HPLC) fingerprints were applied to establish the chromatographic database of TSPJ. The associated hypolipidemic activity database was determined by TG assay using HepG2 cell model. Correlation analyses of two databases were performed by partial least squares (PLS) for calculating regression coefficients, and the interval value of YZL value (the ratio of positive and negative peak-to-peak area coefficient) closely related to hypolipidemic activity was refined by the formula of Norminv function to value the quality of TSPJ. Results: In this study, the chromatographic data of 16 common peaks were obtained from 20 batches of TSPJ. After the estimate by this mathematical evaluation model, seven peaks were positively correlated with hypolipidemic activity, and nine peaks were negatively correlated with hypolipidemic activity. When the YZL value was less than 0.7861, the quality of sample was inferior, while YZL value was more than 6.6992, and the quality of samples was superior. The quality of another ten batches of TSPJ was further assessed to verify this method. Conclusion: These results indicated that the established model could be usefully applied to evaluate the quality of TSPJ in the hypolipidemic activity.
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Objective:The correlation between the appearance color of cooked rhubarb samples and the components characterized by high performance liquid chromatography （HPLC） fingerprint was studied to reveal the quality transfer law in the steaming process of processed products with rice-wine. Method:The visual analyzer was used to analyze the change of the appearance color of cooked rhubarb sample powder at different processing time， the common components and their relative peak areas of processed products with rice-wine were identified by HPLC fingerprint， as well as multivariate statistics and Pearson correlation analysis were used to cluster， discriminate and analyze the appearance color and the component variables in HPLC fingerprint. Result:During the processing of cooked rhubarb， the <italic>a</italic><sup>*</sup> （red-green value） of sample powder had no obvious change， but the <italic>L</italic><sup>*</sup> （lightness value）， <italic>b</italic><sup>*</sup><italic> </italic>（yellow-blue value） and <italic>E</italic><sup>*</sup><italic>ab </italic>（total chromaticity value） showed a decreasing trend， and the appearance color changed from bright to dark， from yellow to brown. A total of 46 chromatographic peaks in the fingerprint were identified at 254 nm and 280 nm， and 18 of them were identified by comparison with reference standards. The change trend of <italic>L</italic><sup>*</sup>，<italic> b</italic><sup>*</sup><italic> </italic>and <italic>E</italic><sup>*</sup><italic>ab </italic>were positively correlated with the contents of tannins （catechin， epicatechin and ethyl gallate）， stilbene glycoside （<italic>trans</italic>-3，5，4′-trihydroxystyryl-4′-<italic>O</italic>-<italic>β</italic>-<italic>D</italic>-glucoside）， phenylbutanone glycoside of 4′-hydroxyphenyl-2-butanone-4′-<italic>O</italic>-<italic>β</italic>-<italic>D</italic>-［2ʺ-<italic>O</italic>-gallic-6ʺ-<italic>O</italic>-（4ʺ-hydroxy）-cinnamoyl）-glucoside， conjugated anthraquinones （aloe emodin-8-<italic>O</italic>-glucoside， rhein-8-<italic>O</italic>-glucoside， emodin-8-<italic>O</italic>-glucoside） and <italic>ω</italic>-hydroxyemodin （<italic>P</italic><0.05， <italic>P</italic><0.01）， and negatively correlated with the contents of free anthraquinones （emodin， aloe emodin and physcion）. Compared with 254 nm， the similarities of chromatographic peaks at 280 nm was more obvious， and the number of detected common peaks was more， which could reflect more subtle differences in chemical composition. Conclusion:Tannins， stilbene glycosides and phenylbutanone glycosides are strongly correlated with <italic>L</italic><sup>*</sup>， while anthraquinones are strongly correlated with <italic>b</italic><sup>*</sup>， the decrease of <italic>E</italic><sup>*</sup><italic>ab</italic> is mainly related to the increase of free anthraquinone content and the decrease of catechins， <italic>ω</italic>-hydroxyemodin， stilbene glycosides， conjugated anthraquinone and phenylbutanone glycosides. The change of appearance color index of process samples can reflect the change trend of the contents of medicinal components in cooked rhubarb to some extent.
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Objective:To establish the high performance liquid chromatography （HPLC） fingerprint of Citri Sarcodactylis Fructus， and to search for makers to characterize the quality difference of Citri Sarcodactylis Fructus from different origins coupled with chemometrics. Method:The analysis was performed on a Thermo Hypersil GOLD C<sub>18</sub> column （4.6 mm×250 mm， 5 μm） with mobile phase consisted of acetonitrile-0.05% phosphoric acid solution for gradient elution， and the detection wavelength was set at 254 nm. A total of 31 batches of samples were analyzed to establish the HPLC fingerprint of Citri Sarcodactylis Fructus. Similarity evaluation was performed by Traditional Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System （2012 edition） to confirm the common peaks， which were identified by comparison of reference substances. On the basis， chemometrics methods were used to analyze and evaluate the quality of Citri Sarcodactylis Fructus from different origins. At the same time， 3 batches of 5 species of decoction pieces from the genus <italic>Citrus</italic> in the family Rutaceae， including Citri Sarcodactylis Fructus， Aurantii Fructus Immaturus， Aurantii Fructus， Citri Reticulatae Pericarpium Viride and Citri Reticulatae Pericarpium， were randomly collected for evaluating the effectiveness and reliability of the established HPLC fingerprint of Citri Sarcodactylis Fructus. Result:HPLC fingerprint of Citri Sarcodactylis Fructus was established and 22 common peaks were identified. And seven common peaks among them were identified as 6，7-dimethoxycoumarin， diosmin， hesperidin， byakangelicin， 5，7-dimethoxycoumarin， bergapten and oxypeucedanin. Except for 2 batches of samples， the similarities of fingerprints between other 29 batches of samples were >0.9. The 31 batches of Citri Sarcodactylis Fructus were basically divided into 3 groups by cluster analysis and principal component analysis， which were consistent with the classification of three different producing areas. Eight differential markers were screened by orthogonal partial least squares discriminant analysis and four of them （5，7-dimethoxycoumarin， bergapten， 6，7-dimethoxycoumarin and diosmin） were identified by reference substances. Similarity evaluation of 5 species of decoction pieces from genus <italic>Citrus</italic> in the family Rutaceae was carried out by taking the reference fingerprint of Citri Sarcodactylis Fructus as treference chromatogram， similarity of Citri Sarcodactylis Fructus decoction pieces was 0.892-0.977， and the similarities of the other 4 kinds of decoction pieces were 0.215-0.517. Conclusion:The established fingerprint method is reasonable， effective and accurate for quality control of Citri Sarcodactylis Fructus， the characterization information is more comprehensive combined with chemometrics.
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This study established high-performance liquid chromatography(HPLC) fingerprints of Chinese medicines derived from Apocynum venetum and Poacynum pictum in Xinjiang and explored their composition differences with the combination of content determination, similarity analysis, cluster analysis and principal component analysis. The HPLC conditions included Phenomenex Kinetex C_(18) column(4.6 mm ×100 mm, 2.6 μm), acetonitrile-0.01% trifluoroacetic acid aqueous solution as mobile phase, gradient elution, flow rate of 0.6 mL·min~(-1), detection wavelength of 281 nm and column temperature of 25 ℃. The content of chlorogenic acid, quercetin-3-O-sophoroside, rutin, hyperin, isoquercitrin, trifolin and astragalin was determined in 31 batches of medicinal materials, and fingerprint research and chemometric analysis were performed with Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine(Version 2004 A) and SPSS 21.0. In the Chinese Pharmacopoeia 2020, the quality of Apocyni Veneti Folium is controlled by character identification, microscopic identification, thin layer chromatography identification and quantitative determination of hyperin. There were 21 common peaks of A. venetum and P. pictum in the HPLC fingerprints, 5 of which were identified as chlorogenic acid, hyperin, isoquercitrin, trifolin and astragalin, with their content also determined. Except for 3 batches of medicinal materials, the similarity of other 28 batches was higher than 0.83, indicating good similarity. Two categories were formed in the cluster analysis based on content determination, which showed that some differences existed in similarities between different regions of Xinjiang. The medicinal materials were ranked by quality with principal component analysis, and the results indicated that the top 15 all came from northern Xinjiang. The quality difference of A. venetum and P. pictum had a correlation with the place of origin. This study provides a reference for the analysis and evaluation of A. venetum and P. pictum from different habitats and the selection of introduction and cultivation areas.
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Apocynum , China , Cromatografía Líquida de Alta Presión , Medicamentos Herbarios Chinos , Medicina Tradicional ChinaRESUMEN
Objective: To provide a scientific basis for the quality control of YuanZhi San capsule(YZSC). Methods: Fourier transform infrared spectroscopy(FTIR)combined with second derivative spectra was used to analyze the chemical components of YZSC;high performance liquid chromatography(HPLC)was used to establish the fingerprints of different batches of YZSC, the quality assessment of YZSC was carried out by similarity evaluation, cluster analysis(CA), principal component analysis(PCA)and orthogonal partial least squares discriminant analysis(OPLS-DA). Results: The main components of YZSC were carbohydrate, flavonoids, alkaloids, organic acids and saponins. There were 41 common peaks in the fingerprint, seven peaks were identified using reference substance, they were 3, 6'-disinapoylsucrose, ferulic acid, jatrorrhizine hydrochloride, palmatine chloride, berberine, quercetin and β-asarone. The similarity of 10 batches of samples was higher than 0.99. The CA and PCA analysis indicated that there were differences in different batches of YZSC, and they were mainly divided into two categories. By the OPLS-DA, 10 main chemical constituents were found to be the cause of the quality differences in the batches, and the peaks of berberine, 3, 6'-disinapoylsucrose, palmatine chloride, β-asarone, and jatrorrhizine hydrochloride were recognized by comparison with the reference substances. Conclusion: The chemical pattern recognition technology based on the FTIR and HPLC analysis might be used for the quality evaluation of YZSC.
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OBJECTIVE: To establish an HPLC chromatographic fingerprint analysis method for the quality evaluation of Baidianfeng capsule and study the differences of products from different manufacturers. METHODS: The chromatographic separation was performed on an XBridge@Shield RP18 column(4.6 mm×250 mm, 5 μm), with the mixture of methanol and 0.15% formic acid as mobile phases in gradient elution mode.The detection wave length was set at 300 nm, the flow rate was 1.0 mL•min-1 and the column temperature was maintained at 35 ℃. The similarity was evaluated with Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine (version 2008). Common peaks were identified by HPLC-MS through the comparison with the references and literature. RESULTS: The precision, repeatability and stability of the established method can meet the requirements of fingerprint chromatography analysis.There were 18 common peaks were identified in the HPLC fingerprint.The similarity of 10 batches of samples ranged from 0.723 to 0.900, indicating greater differences in the qualities among the samples. CONCLUSION: The developed method could provide the comprehensive information about the chemical components in Baidianfeng capsule in a rapid reliable and convenient manner.It could be used in quality evaluation of the drug. It provides scientific basis for improving its quality standard.
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OBJECTIVE: To carry out HPTLC and HPLC fingerprint analysis of 18 batches of Ganoderma samples using two kinds of reference substance of Ganoderma extract, G. lucidum Extract Reference Substance(CZERS) and G. sinense Extract Reference Substance(ZZERS). METHODS: HPTLC Fingerprint was used to analyze triterpene acids and sterols in Ganoderma with chloroform-acetonitrile-methanol-formic acid (13∶2∶0.5∶0.5, develop 3 times) and cyclohexane-ethyl acetate-methanol-formic acid (15∶5∶0.5∶0.5, develop 2 times) respectively. HPLC Fingerprint analysis was conducted using Kromasil 100-5 C18 column (4.6 mm×250 mm, 5 μm) kept at 25 ℃. Mobile phase A was acetonitrile and B was 0.02% phosphoric acid; gradient elution procedure was as follows: 0-40 min, 29%→33% A; 40-70 min, 33%→65%A; 70-105 min, 65%→100%A; 105-120 min, 100% A; flow rate was 1.0 mL•min-1. DAD detector was adopted with detection wavelength set at 244 nm. The injection volume was 10 μL. RESULTS: By using ERS and fingerprint analysis, G. lucidum, G. sessile and G. lucidum could be distinguished. The components of G. lucidum in different species and growth patterns were different. CONCLUSION: There are many varieties of G. lucidum, which can be divided into wild and artificial cultures, and the culture media of artificial culture are different, which leads to the difference of individual components of different G. lucidum. Fingerprint analysis based on ERS of specific varieties are more suitable for the overall quality control of G. lucidum.
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OBJECTIVE: To establish a chemical pattern recognition method for Panax notoginseng (P. notoginseng) and classify the main root, rhizome, and rootlet. METHODS: The fingerprints of P. notoginseng samples in three different parts were established based on HPLC method. The similarity was calculated by the Similarity Evaluation System of Chromatographic Fingerprints of Traditional Chinese Medicine (2012 edition). The pattern recognition were carried out by principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA). RESULTS: The HPLC fingerprint common pattern of 35 batches of P. notoginseng samples was established. Similarity values were in the range of 0.994 to 1.000, which indicated that similarity analysis could not classify them. The established PCA model could only identify the rhizome, besides PLS-DA can completely identify the three parts of P. notoginseng. Seven characteristic peaks, such as ginsenoside Rg1, ginsenosides Rb1 were screened as biomarkers. CONCLUSION: The combination of HPLC fingerprint and chemical pattern recognition could provide a comprehensive reference for the quality control and quality evaluation of P. notoginseng.
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OBJECTIVE: To establish a high performance liquid chromatography(HPLC) method for determining chromone components in Saposhnikoviae Radix, and compare the similarities and differences between bolting and non-bolting samples. METHODS: Agilent Ecilpse Plus C18 column(4.6 mm×250 mm,5 μm) was used for chromatographic analysis, water and methanol were used as mobile phase for gradient elution at a flow rate of 1 mL•min-1. Detection was conducted at 254 nm. The column temperature was maitained at 35 ℃ and the injection volume was 10 μL. RESULTS: There were 10 common peaks in the HPLC fingerprints of 8 batches of Saposhnikoviae Radix,with similarity above 0.94 in six batches of bolting and non-bolting samples and below 0.90 in two batches of second-stubble samples.The HPLC assay had good linearity for the four chromone components. The average recoveries for prim-O-glucosylcimifugin,cimicifugin, 5-O-methylvisamidol glycoside and sec-O-glu cosylhamaudol were 95.05%, 98.62%, 98.3% and 99.02%,and the RSDs of repeatability test were 1.60%, 1.77%, 1.24% and 3.09%, respectively. When comparing the bolting and non-bolting Saposhnikoviae Radix, the content of cimicifugin increased after bolting, the other three components and the total amount of the four chromone components did not have significant variation. CONCLUSION: The establishment of HPLC fingerprint combined with simultaneous determination of four chromone components provides a more comprehensive reference for the quality control and quality evaluation of Saposhnikoviae Radix. There are no obvious differences in chromone components between bolting and non-bolting Saposhnikoviae Radix, but there is significant difference between second-stubble and first-stubble Saposhnikoviae Radix.
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OBJECTIVE: To study the fingerprints of rhizomes of Paris polyphylla Smith var. polyphylla and Paris polyphylla Smith var. yunnanensis (Franch.) Hand. -Mazz from different origins in Dali and the differences of seven main steroidal saponins. METHODS: The fingerprints of rhizomes of Paris polyphylla var. polyphylla and Paris polyphylla var. yunnanensis from different origins in Dali were established by HPLC. The similarity of fingerprints and seven main steroidal saponins were compared and analyzed. RESULTS: There were 14 common peaks in the fingerprints of rhizomes of Paris polyphylla var. polyphylla from different origins in Dali, and the similarity of the fingerprints of the samples from different habitats except Jinhua Weishan and Longjie Weishan was greater than 0.9. There were 13 common peaks in the fingerprints of rhizomes of Paris polyphylla var. yunnanensis from different origins in Dali, and the similarity of the samples from different origins was greater than 0.92. There were 11 common peaks in the fingerprints of rhizomes of Paris polyphylla var. polyphylla and Paris polyphylla var. yunnanensis from different origins in Dali, and the similarity of the fingerprints was very low, between 0.057 and 0.225. Polyphyllin Ⅰ, polyphyllin Ⅱ, polyphyllin Ⅵ and polyphyllin Ⅶ are detected in the rhizomes of Paris polyphylla var. polyphylla and Paris polyphylla var. yunnanensis from different origins in Dali. The average peak areas of polyphyllin Ⅰ, polyphyllin Ⅱ, polyphyllin Ⅵ and polyphyllin Ⅶ in Paris polyphylla var. yunnanensis from different origins in Dali were higher than those of Paris polyphylla var. polyphylla. Polyphyllin H was detected in the rhizomes of Paris polyphylla var. yunnanensis from Leqiu Nanjian, Jinhua Weishan, Fengyu Eryuan, Dengchuan Eryuan, Hongyan Midu, Xiyi Heqing and the rhizomes of Paris polyphylla var. polyphylla from Wanqiao Dali, Fengyi Dali, Xiyi Heqing, Hongyan Midu and Leqiu Nanjian. Polyphyllin Ⅲ was detected in the rhizomes of Paris polyphylla var. polyphylla from the origins except Longjie Weishan. Polyphyllin Ⅴ was also detected in the rhizomes of Paris polyphylla var. polyphylla in Fengyu Eryuan and Xiyi Heqing. CONCLUSION: Polyphyllin Ⅰ, polyphyllin Ⅱ, polyphyllin Ⅵ and polyphyllin Ⅶ are detected in the rhizomes of Paris polyphylla var. polyphylla and Paris polyphylla var. yunnanensis from different origins in Dali. The similarity of the HPLC fingerprints of the rhizomes of Paris polyphylla var. polyphylla and Paris polyphylla var. yunnanensis is very low, and there are great differences in seven main steroidal saponins. The contents of polyphyllin Ⅰ, polyphyllin Ⅱ, polyphyllin Ⅵ and polyphyllin Ⅴ in Paris polyphylla var. yunnanensis are higher than those in Paris var. polyphylla.
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In this paper, angelica broken wall powder(ABWP) was taken as the research object, HPLC fingerprint combined with multi-component determination(ferulic acid, senkyunolide I, coniferyl ferulate, ligustilide and 3-butylidenephthalide), physical fingerprint(D_(90), particle size distribution range, particle size distribution width, bulk density, tap density, inter-particle porosity, Carr index, specific surface area, pore volume, angle of repose, Hausner ratio, loss on drying and hygroscopicity)were used to characterize the quality attribute of ABWP; similarity analysis, cluster analysis, principal component analysis and orthogonal partial least squares discriminant analysis were conducted to construct the quality evaluation method of holographic analysis based on traditional Chinese medicine QbD "4 H mode", in order to evaluate the quality of ABWP from different sources and find out differentiated indicators. The quality evaluation method could be used for scientific, comprehensive evaluation of the quality attribute of ABWP, and the quality consistency evaluation of cell-wall-broken powder of different sources or different processes.It provides new ideas for quality control and research of ultrafine granular powders of traditional Chinese medicine.