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In order to better control the quality of Flos Puerariae(FP),qualitative and quantitative analyses were initially performed by using chemical fingerprint and chemometrics methods in this study.First,the fingerprint of FP was developed by HPLC and the chemical markers were screened out by similarity analysis(SA),hierarchical clustering analysis(HCA),principal components analysis(PCA),and orthogonal partial least squares discriminant analysis(OPLS-DA).Next,the chemical constituents in FP were profiled and identified by HPLC coupled to Fourier transform ion cyclotron resonance mass spectrometry(HPLC-FT-ICR MS).Then,the characteristic constituents in FP were quantitatively analyzed by HPLC.As a result,31 common peaks were assigned in the fingerprint and 6 of them were considered as qualitative markers.A total of 35 chemical constituents were detected by HPLC-FT-ICR MS and 16 of them were unambiguously identified by comparing retention time,UV absorption wavelength,accurate mass,and MS/MS data with those of reference standards.Subsequently,the contents of glycitin,genistin,tectoridin,glycitein,genistein,and tectorigenin in 13 batches of FP were detected,ranging from 0.4438 to 11.06 mg/g,0.955 to 1.726 mg/g,9.81 to 57.22 mg/g,3.349 to 41.60 mg/g,0.3576 to 0.989 mg/g,and 2.126 to 9.99 mg/g,respectively.In conclusion,fingerprint analysis in combination with chemometrics methods could discover chemical markers for improving the quality control standard of FP.It is expected that the strategy applied in this study will be valuable for further quality control of other traditional Chinese medicines.
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In this paper, we aim to control and evaluate the quality of Liuwei Dihuang Concentrated Pill by using the model of fingerprint technique and "component structure" theory. Agilent 5 TC-C_(18) column(4.6 mm×250 mm,5 μm) was used, with 0.1% formic acid solution-acetonitrile as mobile phase at a flow rate of 1.0 mL·min~(-1). The column temperature was 30 ℃, with detection wavelength of 242 nm and the sample volume of 10 μL. The characteristic fingerprint of Liuwei Dihuang Concentrated Pill was established by high performance liquid chromatography(HPLC) for its quality control. Seventeen common peaks were identified, and the similarity was 0.550-0.997 in 29 batches of samples, indicating that the quality difference among batches of Liuwei Dihuang Concentrated Pills was significant. The structural characteristics of the Moutan Cortex components in Liuwei Dihuang Concentrated Pills were characterized. On this basis, combined with the structural characteristics of genuine components of Moutan Cortex, the structural characteristics of components in Liuwei Dihuang Concentrated Pills were further analyzed. The results showed that there were significant differences in the contents and quantity ratios of 9 representative components(components) of Moutan Cortex in Liuwei Dihuang Concentrated Pills from different manufacturers, indicating internal quality differences among different batches of products. The fingerprint technique and the "component structure" theory established by the above research provide an analytical method and a research foundation for the quality evaluation of Liuwei Dihuang Concentrated Pills.
Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Quality ControlABSTRACT
Objective: To optimize the infiltration process of Astragalus (Astragalus membranaceus var. mongholicus) medicinal materials by Box-Behnken response surface method. Methods: Based on the HPLC-DAD-ELSD and response surface design method, the qualified rate of decoction pieces, the content of index components and bending inspection were used as comprehensive inspection indicators, and the three factors of infiltration were selected for response surface experimental design to optimize the infiltration process of Astragalus medicinal materials parameter. Results: The best infiltration process was as following: infiltration temperature was 20 ℃, with water addition of 1:0.988 for 6 h. Under this process, the qualified rate of Astragalus pieces was 95.81%, the content of calycosin-7-glucoside was 0.072%, and the content of astragaloside IV was 0.276 %. Combining fingerprint analysis and heat map analysis, the material basis of A. membranaceus var. mongholicus changed during the infiltration process. The infiltration parameters should be strictly controlled during the infiltration process to ensure uniform quality of the pieces. Conclusion: The optimized Astragalus medicinal material infiltration process is stable and feasible with good reproducibility, which can provide a reference for the mass production process development of Astragalus medicinal slices.
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This study aims to establish a combinative method based on fingerprint,assay of multi-component and chemometrics for quality evaluation of Magnoliae Officinalis Cortex. Twenty batches of samples were determined by UPLC and a common mode of fingerprint was established. The similarities between fingerprints of 20 batches of samples were over 0. 90 and the common mode were evaluated. Eight components were identified as syringing, magnocurarine, magnoflorine, magnoloside B, magnoloside A, honokiol,magnolol,and piperitylmagnolol by comparison with reference substances and their content in samples were simultaneously determined.Based on the results,the fingerprint had good consistency between the same origin and minor diversity between the different sources.Piperitylmagnolol and peak 13 could be used as a distinction with the different sources. According to content of 8 components,Fisher discriminant analysis model was established and different source sample was classified pursuant to the discriminant fraction. It is indicated that simultaneous quantification of multi components coupled with chemometrics analysis could be a well-acceptable strategy to identify and evaluate the quality of Magnoliae Officinalis Cortex.
Subject(s)
Chromatography, High Pressure Liquid , Discriminant Analysis , Drugs, Chinese Herbal , Reference Standards , Magnolia , Chemistry , Phytochemicals , Reference Standards , Quality ControlABSTRACT
Objective: To observe the effect of different processing methods on the quality of Codonopsis Radix and provide data reference for the reasonable processing in the producing areas. Methods: An analytical strategy that combined quantitative and HPLC fingerprint analysis with chemometrics was developed for the quality evaluation of Codonopsis Radix. Lobetyolin, polysaccharide, sucrose, glucose, and fructose were detected simultaneously in Codonopsis Radix samples treated with different processing methods including dryer-drying, sun-drying, shade-drying, sulfur fumigation, and kneading, etc. Results: The results showed that different processing methods had an obvious impact on the quality of Codonopsis Radix. Sun-drying or shade-drying was recommended, and sulfur fumigation should be avoided. And dryer-drying at 40 °C−50 °C was suggested to meet the requirement for large scale processing. In addition, based on the content of polysaccharide, glucose, and fructose, it was advised to knead for three times. As for lobetyolin and sucrose, kneading should be avoided. Conclusions: Our findings demonstrated that processing method had a big impact on the quality of Codonopsis Radix. Based on the results, the appropriate processing methods directed at different requirements were recommended. The study could lay a foundation for the reasonable processing of Codonopsis Radix in producing areas.
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Objective To study the dry extract rate, determination and transfer rate of maker compounds, and fingerprint of standard decoction of ginger juice Magnoliae Officinalis Cortex (GJMOC) and provide a reference for the preparation and quality assessment of its dispensing granules by establishing 16 batches of standard decoction of GJMOC. Methods A total of 16 batches of GJMOC standard decoctions were prepared following literature requirements. The quantitative analysis method of magnolol and honokiol was according to Chinese Pharmacopoeia (2015 edition). The transfer rate of total magnolol and honokiol and extraction rate were calculated. the pH value was determined and HPLC fingerprint was established under a flow rate of 1 mL/min and eluted with a mobile phase of acetonitrile (A)-0.1% phosphoric acid solution (B) in a gradient mode (0-15 min, 12%-16% A; 15-30 min, 16%-28% A; 30-42 min, 28%-74% A; 42-55 min, 74%-80% A). The column temperature was set at 40℃ and the detection wavelength was 294 nm. Results By measuring the of 16 batches of standard decoction, the transfer rate of the sum of magnolol and honokiol ranged from 6.5% to 12.0%, the extraction rate was at a range of 3.41% to 7.14% and pH value was 4.63 to 5.43. The Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine (2012A) was used to analyze and compare the fingerprints, and seven common peaks were determined and four were identified including magnoloside B (peak 1), magnoloside A (peak 2), honokiol (peak 6), and magnolol (peak 7). The similarity among 16 batches of standard decoction of GJMOC was evaluated, and the similarity was all greater than 0.69. Moreover, this study established an HPLC fingerprint analysis method of GJMOC standard decoction. Conclusion The preparation method established in this study is stable and feasible, and the analysis method shows good precision, stability, and repeatability in fingerprint analysis and it is suitable for evaluating the quality of standard decoction of GJMOC.
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Abstract A precise and accurate method for the identification and authentication of Phyllanthus niruri L. from P. debilis Klein ex Willd. and P. urinaria L., Phyllanthaceae, was developed using high-performance liquid chromatography. Chromatographic fingerprint analysis was combined with simultaneous quantification of phyllanthin and hypophyllanthin for the developed method. Phyllanthin and hypophyllanthin were successfully separated and quantified under this proposed method. The highest amount of phyllanthin and hypophyllanthin was found in P. niruri compared to P. debilis and P. urinaria. Fingerprint chromatogram of the three Phyllanthus species showed distinct profiles that these may be used to identify and authenticate each Phyllanthus species, which improved by marker compounds present in each species. The combination of chromatographic fingerprint analysis and discriminant analysis was successfully discriminated all three species, including P. niruri adulterated with P. debilis or P. urinaria. The method can be used for the identification and authentication of P. niruri from related species, such as P. debilis and P. urinaria.
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ABSTRACT This paper aimed to evaluate the quality of hawthorn leaves and Guang hawthorn leaves by an UPLC-MS method from two aspects, fingerprint analysis and multi-ingredient quantification. Chromatographic separation was carried out on an UPLC system, the standardized characteristic fingerprints was established by Similarity Evaluation System for chromatographic fingerprinting of traditional Chinese medicine and cluster analysis. Eight components were simultaneously determined by mass spectrometry in multiple reaction-monitoring mode. The method was validated in terms of linearity (R2 > 0.9971), intraday and interday precision (RSD < 2.0%), repeatability (RSD < 2.3%), stability (RSD < 2.5%) and recovery (96.2-103.8%). The developed method was successfully applied to the quality evaluation between hawthorn leaves and Guang hawthorn leaves, and there were differences in the component and the content, hawthorn leaves and Guang hawthorn leaves cannot substitute each other in clinical medication.
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Ultra-performance liquid chromatography-evaporative light scattering detection (UPLC-ELSD) fingerprint analysis method was established for quality control of Guci tablets. Chromatographic separation was performed on Waters Acquity UPLC BEH C₁₈ column (2.1 mm×100 mm, 1.7 μm) at 30 °C of column temperature. Acetonitrile-0.1% formic acid solution was adopted as mobile phase for gradient elution. The flow rate was set at 0.3 mL·min⁻¹, and the injection volume was 3 μL. Detection was carried out on an ELSD with a nitrogen pressure of 0.28 MPa, drift tube temperature of 60 °C, and gain of 400. A total of 39 batches of samples produced by six manufacturers were measured by using the above method and the data were analyzed by ChemPattern software. The peak present in more than 75% of the samples was defined as a common peak, and 30 common peaks were determined. Among them, 19 peaks were identified by rapid resolution liquid chromatography/tandem mass spectrometry (RRLC-MS/MS) method, 16 of which were confirmed by reference substances. The similarity of the tested samples was 0.47-0.98, suggesting that the quality of the samples from different manufacturers varied greatly. Furthermore, principal component analysis (PCA) and hierarchical analysis (HCA) were performed to clarify the main different components in samples. The results indicated that there might be some feeding problems about Paeoniae Radix Alba, Notoginseng Radix et Rhizoma, and Clematidis Radix et Rhizoma in a few manufacturers. This study provided some evidences for the overall quality control of Guci tablets, as well as its quality standard improvements.
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Artemisiae Argyi Folium, the dried leaves of Artemisia argyi, has been widely used in traditional Chinese and folk medicines for treatment of hemorrhage, pain, and skin itch. Phytochemical studies indicated that volatile oil, organic acid and flavonoids were the main bioactive components in Artemisiae Argyi Folium. Compared to the volatile compounds, the research of nonvolatile compounds in Artemisiae Argyi Folium are limited. In the present study, an accurate and reliable fingerprint approach was developed using HPLC for quality control of Artemisiae Argyi Folium. A total of 10 common peaks were marked，and the similarity of all the Artemisiae Argyi Folium samples was above 0.940. The established fingerprint method could be used for quality control of Artemisiae Argyi Folium. Furthermore, an HPLC method was applied for simultaneous determination of seven bioactive compounds including five organic acids and two flavonoids in Artemisiae Argyi Folium and Artemisiae Lavandulaefoliae Folium samples. Moreover, chemometrics methods such as hierarchical clustering analysis and principal component analysis were performed to compare and discriminate the Artemisiae Argyi Folium and Artemisiae Lavandulaefoliae Folium based on the quantitative data of analytes. The results indicated that simultaneous quantification of multicomponents coupled with chemometrics analysis could be a well-acceptable strategy to identify and evaluate the quality of Artemisiae Argyi Folium.
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Taraxaci Herba was derived from the dried Herba of Taraxacum mongolicum, T. borealisinense and several species from the Taraxacum genus. Taraxaci Herba has been widely used in traditional Chinese and folk medicines. According to the different growth and cultivation pattern, Taraxaci Herba could be divided into two species, wild Taraxaci Herba and cultivated Taraxaci Herba. In the present study, an accurate and reliable fingerprint approach was developed using high performance liquid chromatography(HPLC) for quality control of Taraxaci Herba. A total of 9 common peaks were marked, and the similarity of all the Taraxaci Herba samples was above 0.960. The established fingerprint method could be used for quality control of Taraxaci Herba. Furthermore, an HPLC method was established for simultaneous determination of six bioactive compounds, including monocaffeoyl tartaric acid, chlorogenic acid, caffeic acid, cichoric acid, 4,5-dicaffeoylquinic acid and luteolin in wild Taraxaci Herba and cultivated Taraxaci Herba. Moreover,chemometrics analysis such as principal component analysis and orthogonal partial least squares discriminant analysis were performed to compare and discriminate the wild samples and cultivated samples based on the quantitative data. The chemometrics results indicated that 4,5-dicaffeoylquinic acid and luteolin were significant to effectively discriminate the wild Taraxaci Herba and cultivated Taraxaci Herba samples, and these two compounds could be recognized as chemical markers for quality evaluation of wild Taraxaci Herba and cultivated Taraxaci Herba. The fingerprint analysis and quantitative analysis of multi-components could be a well-acceptable strategy for evaluation the quality of Taraxaci Herba.
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Objective: To establish a method of fingerprint analysis and determination of index compounds on commercial Polygala tenuifolia by ultra performance liquid chromatography, and to evaluate the quality of P. tenuifolia with different commodity specification grades. Methods: UPLC was used to establish different commodity specification grade of P. tenuifolia and determine the contents of ten indicative compounds including sibiricose A5, sibiricose A6, lancerin, sibiricoxanthone B, glomeratose A, 7-O-methyl mangiferin, polygalaxanthone III, 3,6′-disinapoyl sucrose, tenuifoliside A, and tenuifoliside C, and establish comprehensive quality evaluation function at the same time. Results: The methods for fingerprint analysis and compound determination were in agreement with methodological requirements. A total of 37 peaks were selected as the common peaks, of which 22 peaks were identified, and the similarities were between 0.927 and 0.971. There are differences at different degrees in the contents of ten indicative compounds. The comprehensive quality evaluation function showed that the overall quality of Datong was better than that of Zhongtong; The overall quality of wild P. tenuifolia was better than that of cultivated. Conclusion: The validated UPLC fingerprint analysis and compound determination methods were successfully used in the quality control of P. tenuifolia.
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In order to reveal the properties of polar metabolome in inflammatory cells, we selected LPS-induced RAW264.7 inflammatory cell models as the carrier for the research of metabolic fingerprint analysis. In this study, an ultra performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF/MS)-based metabolomics protocol was optimized for the extraction of polar metabolites from RAW264.7 cell line. Then orthogonal partial least squares discriminant analysis (OPLS-DA) was used to process the metabolic data, and finally, a total of 17 metabolites were selected and identified. The results showed that MeOH-CHCl3-H2O (8∶1∶1) was chosen as the optimal extraction solvent to achieve higher number of chromatographic peaks, with the best relative extraction efficiency and stability. Comparing with the normal cells, the inflammatory cells presented an abnormal metabolism in protein, carbohydrate, nucleotide and phospholipids. In this study, a UPLC-Q-TOF/MS-based metabolomics protocol for the polar metabolites from RAW264.7 cell line was developed, which may provide important information for the study of mechanism of inflammation and the anti-inflammatory drugs.
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A novel method combining ultra-high performance liquid chromatography (UHPLC) fingerprint and simultaneous quantitative analysis of eight phenolic components was developed and validated for quality evaluation of Tetrastigma hemsleyanum leaves. For fingerprint analysis, 15 peaks were selected as the common peaks to evaluate the similarities among 41 batches of T. hemsleyanum leaves collected from different regions. Additionally, simultaneous quantification of eight markers, including neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, isoorientin, orientin, vitexin-2-O-rhamnoside,vitexin and isovitexin, was performed and the obtained data demonstrated that our method has achieved desired linearity, precision and accuracy. Clustering statistical analysis was further application in T. hemsleyanum leaves from different regions. The results indicated that new approach conbine ultra-high performance liquid chromatography (UHPLC) fingerprint and simultaneous quantitative analysis of eight phenolic components was applicable in quality control of T. hemsleyanum leaves.
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Objectives: To obtain the variety of Erigeron breviscapus with high yield, high content of active constituents, and stable agronomic characteristics. Methods: The group bulk selection breeding and individual selection breeding methods were applied respectively, and two varieties were evaluated partially by DUS testing and the fingerprint was analysed by AFLP markers. Results: The variety "Airuijie No. 1" had the yield of 3780 kg/hm2, the scutellarin content of 1.84%, and the total caffeic acid esters content of 1.79%; For the other variety "Airuijie No. 17", the yield was 3075 kg/hm2, the content of scutellarin was 1.71%, and the content of total caffeic acid esters was 1.50%. Compared with the wild local E. breviscapus after one-year acclimatization, the two new varieties showed better economic traits with higher uniformity, more stability, and unique AFLP fingerprint. Conclusion: The two varieties of E. breviscapus have high value of application and popularization.
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Quality assessment of traditional herbal medicines is of benefit not only in research but also in practice. The method of quality assessment of the Thai traditional medicine, Ayurved Siriraj Prasachandaeng, was established by using High Performance Thin Layer Chromatography (HPTLC) and High Performance Liquid Chromatography (HPLC). In HPTLC, the chromatographic fingerprints were developed; the color and the relative retardation factor (rRf) of bands were compared with those of reference markers. Likewise, relative retention time (rRt), and applied information content (f) were evaluated in HPLC fingerprints. Reference markers, gallic acid, caffeic acid, p-coumaric acid, ferulic acid, vanillic acid and kojic acid were used as qualitative markers in HPTLC whereas gallic acid, caffeic acid and vanillic acid were used as qualitative and quantitative markers in HPLC. Similarity of the chromatographic pattern among batches was determined by the presence of stated mathematic parameters in the range of 80 to 125 percent of the average. The HPTLC and HPLC fingerprints of three batches of Ayurved Siriraj Prasachandaeng showed similar chromatographic patterns. Such similarity showed that the productions of different batches in the recipe were consistent. Moreover, it revealed that some markers found in the recipe certainly came from various medicinal herbal components of their own recipes. In conclusion, the combination of rRf from HPTLC, and rRt and f from HPLC is the suitable method for identification and quality control of different batches of Ayurved Siriraj Prasachandaeng.
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A large amount of data generated in the study of chromatographic fingerprint of Chinese herbal medicines. Criteria selection was one of main considerations while the fingerprint analysis was conducted. Based on the published reports, several criteria of chromatographic fingerprint analysis were reviewed in this paper, including the basic parameters, criteria of peaks isolated, reproducibility of chromatogram and related criteria,criteria of optimization, criteria of stability as well as multi-phase multi-information fingerprint chromatograms, etc..