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ObjectiveTo establish the quality standard for Fraxini Cortex（Fraxinus chinensis） dispensing granules based on standard decoction， and to provide a basis for the quality control of this dispensing granules. MethodHigh performance liquid chromatography（HPLC） specific chromatograms of 15 batches of Fraxini Cortex（F. chinensis） standard decoctions and 3 batches of Fraxini Cortex（F. chinensis） dispensing granules were established with the mobile phase of 0.1% phosphoric acid aqueous solution（A）-acetonitrile（B） for gradient elution（0-10 min， 12%-15%B； 10-30 min， 15%-32%B） and the detection wavelength of 220 nm. And similarity evaluation， cluster analysis and principal component analysis（PCA） were also carried out. HPLC quantitative analysis of multi-components by single marker（QAMS） was established to determine the contents of the main components in the standard decoctions and dispensing granules. The contents of the corresponding components in Fraxini Cortex（F. chinensis） decoction pieces were also detected， and the transfer rates from decoction pieces to standard decoctions and dispensing granules were calculated. ResultThe similarities between specific chromatograms of 15 batches of Fraxini Cortex（F. chinensis） standard decoctions and 3 batches of Fraxini Cortex（F. chinensis） dispensing granules were all>0.9， and 7 common peaks were identified. The results of cluster analysis and PCA showed that there was some differences in the composition of different batches of standard decoctions， but did not show aggregation of origin. As the standard decoctions， the extract rate was 6.18%-11.62%， the contents of esculin， syringin， fraxin， esculetin， fraxetin， calceolarioside B were 44.92-103.51， 1.36-11.87， 33.26-90.73， 4.63-29.75， 2.40-16.86， 2.49-17.35 mg·g-1， and the transfer rates from decoction pieces to standard decoction were 25.21%-42.54%， 52.57%-88.84%， 43.43%-79.45%， 49.15%-88.27%， 49.22%-72.69%， 27.66%-47.67%， respectively. The extract rates of Fraxini Cortex（F. chinensis） dispensing granules were 10.4%-10.7%， the transfer rates of the above six components from decoction pieces to dispensing granules were 42.76%-43.17%， 80.01%-80.90%， 59.59%-59.88%， 51.35%-52.67%， 60.50%-60.93%， 37.98%-38.37%， respectively， which were generally consistent with the transfer rates from decoction pieces to standard decoctions. ConclusionThe established quality control standard of Fraxini Cortex（F. chinensis） dispensing granules based on standard decoctions is reasonable and reliable， which can provide reference for the quality control and process research of this dispensing granules.
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Objective: To establish the method for the specific chromatograms analysis of steamed Panax notoginseng Powder and determine the content of eight components, combined with clustering analysis and partial least square discriminant analysis (PLS-DA), with aim to provide reference for the quality control of steamed Panax notoginseng Powder. Methods: HPLC with Agilent ZORBAX SB-C18 column (250 mm × 4.6 mm, 5 μm) was used, the mobile phase was acetonitrile (B)-water (A) in a gradient elution mode, the detection wavelength was set at 203 nm, the flow rate was 1.0 mL/min, the column temperature was 40 ℃, and sample size 10 ìL. HPLC characteristic spectrum of steamed Panax notoginseng Powder was established, and quantitative determination methods of eight index components, ginsenoside 20 (S)-Rh1, 20 (R)-Rh1, Rk3, Rh4, 20 (S)-Rg3, 20 (R)-Rg3, Rk1 and Rg5, were investigated, its content in 63 batches of samples were determined. Results: The specific chromatograms of steamed Panax notoginseng Powder effective parts were established and 19 common peaks were designated. Among them, eight rare saponins including ginsenoside 20 (S)-Rh1, 20 (R)-Rh1, Rk3, Rh4, 20 (S)-Rg3, 20 (R)-Rg3, Rk1 and Rg5 all showed good linear relationship within the ranges of 0.999 9, 0.999 5, 0.999 4, 0.999 3, 0.999 1, 0.999 3, 0.999 1, and 0.999 3, respectively. The average recovery was 95%—105%, with the RSD value less than 2%. Moreover, the 63 batches of samples were divided into two groups: brown red and light yellow, and the quality of brown red group was obviously better than that of pale yellow group. Conclusion: The quality of the steamed Panax notoginseng Powder is related to the color and lustre. This method is accurate, sensitive and reproducible, which can provide reference for the quality evaluation of steamed Panax notoginseng Powder.
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Objective: To establish HPLC specific chromatograms of Puerariae Lobatae Radix(PLR) and Puerariae Thomsonii Radix(PTR), and make a distinction about their species and different habitats of PLR by chemical pattern recognition, provide reliable methods for scientific evaluation and effective control of their quality. Method: HPLC was employed to determine the contents of chemical ingredients in 23 batches of PLR and PTR.The similarity analyzed with "Similarity Evaluation System for Chromatographic Fingerprint of Chinese Materia Medica"(version of 2004A), then a common pattern was established.Based on its chemical fingerprint information, the quality of PLR and PTR was comprehensively analyzed by three kinds of chemical pattern recognition methods. Result: In addition to sample S22(from Shaanxi province), the similarities of 23 batches of samples were more than 0.9, which showed that similarity of PLR and PTR was good, this method can not differentiate them.Principal component analysis(PCA) could only identify PLR and PTR, but partial least squares-discriminant analysis(PLS-DA) could distinguish PLR from PTR and the producing areas of PLR with model interpretation of 96.4% and prediction of 74.6%.The result of hierarchical cluster analysis(HCA) was consistent with PLS-DA. Conclusion: Chemical pattern recognition method can make a distinction between PLR and PTR, as well as different habitats of PLR;it is suitable for quality control of their medicinal materials.
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Objective: To compare the effect of four kinds of decocting containers on the content of sinapine and the HPLC specific chromatograms of Sinapis Semen decoction,so as to optimize decocting container for the development of classical formulas. Method: Selecting four kinds of decoction vessels,named traditional casserole,ceramic pot,round-bottom flask and stainless-steel pot as the research object,the content of sinapine in Sinapis Semen decoction and its HPLC specific chromatograms were used as indexes to investigate the influence of different decoction vessels on the decoction.Similarity evaluation of specific chromatograms was performed by the "Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine"(edition of 2004A). Result: The contents of sinapine in the decoction prepared by traditional casserole,ceramic pot,round-bottom flask and stainless-steel pot were 0.04%,0.07%,0.84% and 0.97%,respectively.Compared with specific chromatograms of the decoction prepared by traditional casserole,the similarities of specific chromatograms of the decoction prepared by ceramic pot,round-bottom flask and stainless-steel pot were 0.98,0.82 and 0.68,respectively.Compared with specific chromatograms of the decoction prepared by ceramic pot,the similarities of specific chromatograms of the decoction prepared by round-bottom flask and stainless-steel pot were 0.79 and 0.62,respectively.Compared with specific chromatograms of the decoction prepared by round-bottom flask,the similarity of specific chromatograms of the decoction prepared by stainless-steel pot was 0.97. Conclusion: The content of sinapine and HPLC specific chromatograms of Sinapis Semen decoction obtained from different decocting containers are quite different.
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HPLC specific chromatograms of Poria were established, and the concentrations of 10 triterpenoids(16α-hydroxydehydrotrametenolic acid, poricoic acid B, dehydrotumulosic acid, poricoic acid A, polyporenic acid C, poricoic acid AM, 3-O-acetyl-16α-hydroxydehydrotrametenolic acid, dehydropachymic acid, pachymic acid, and dehydrotrametenolic acid) were simultaneously determined. Chromatographic analysis was conducted on a Welch Ultimate XB C_(18) column(4.6 mm × 250 mm,5 μm). Acetonitrile solution(contain 3% tetrahydrofuran)(A) and 0.1% formic acid aqueous solution(B) were used as the mobile phase with gradient elution at a flow rate of 1.0 mL·min~(-1). The column temperature was 30 ℃ and the injection volume was 20 μL. The experimental data were analyzed by the SPSS 22.0 and GraphPad Prism 7.0. The established triterpenoids fingerprints were specific, and the 10 components were well separated and showed good linearity(r≥0.999 6) within the concentration ranges tested. The mean recoveries were between 98.53%-103.8%(RSD 1.7%-2.7%). The method was specific and repeatable, and could be used for identification and quality evaluation of Poria. The results showed that the contents of 10 triterpenoids were positively correlated with each other. The contents of 10 triterpenoids of samples collected from producing areas were higher than that collected from markets. The total contents of 10 triterpenoids of samples collected from Hubei and Yunnan province were slightly higher than that from Anhui province, but the contents of samples from Anhui province were varied in smaller ranges.
Subject(s)
China , Chromatography, High Pressure Liquid , Materia Medica , Poria , ChemistryABSTRACT
Objective: To establish the HPLC specific chromatograms of the ethyl acetate layer in ten batches of effective parts of Filifolium sibiricum and to determine the contents of five components. Methods: The analysis of effective parts of F. sibiricum was performed on a Thermo AcclaimTM120 C18 column (250 mm × 4.6 mm, 5 μm) with acetonitrile (B)-PBS (A) (0.1 mol/L sodium dihydrogen phosphate-2% glacial acetic acid, 1∶1) as the mobile phase in a gradient elution mode, the detection wavelength was set at 360 nm, the flow rate was 0.8 mL/min, and the column temperature was 35 ℃. Results: The specific chromatograms of F. sibiricum effective parts were established and ten common peaks were designated. Among them, five components including isorientin, isovitexin, isoquercitrin, luteoloside and isorhamnetin-3-O-β-D-glucose all showed good linear relationship within the ranges of 0.018—0.108, 0.066 8—0.400 8, 0.088—0.528, 0.118 4—0.710 4 and 0.017 6—0.105 6 μg, respectively. The average recovery was 98.67%, 97.93%, 98.95%, 99.81%, and 97.33% with the RSD value at 1.10%, 0.93%, 1.10%, 0.62%, and 1.48%, respectively. Moreover, the similarity of the eight batches of samples was above 0.9 in the ten batches of medicinal herbs, the similarity of the two batches of which was 0.688 and 0.695, indicating that its content was lower and the difference was greater. In addition, there were significant differences in the content of five components in each harvest time. The content of flavonoids in medicinal herbs was higher with high flower percentage. It was suggested that the content of flavonoids in F. sibiricum was related to the flower percentage of harvest period. Conclusion: The HPLC specific chromatograms of the F. sibiricum effective parts were established and the common characteristic peaks were determined, which could be used for quality control of the F. sibiricum.
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The present study is to compare specific chromatograms and main acitive components between wild and cultivated rhizomes of Paris polyphylla var. yunnanensis by HPLC. HPLC analysis was performed on a Waters XSelect HSS T3 C₁₈ clumn (4.6 mm×250 mm, 5 μm), with a mobile phase consisting of acetonitrile (A)-water (B) at a flow rate of 1 mL•min⁻¹ (0-50 min,30%-50%A;50-80 min,50% A,80-85 min,50%-30%A;85-100 min,30% A). The detection wavelength was 203 nm and the column temperature was controlled at 30 ℃, and the injection volume was 10 μL. HPLC specific chromatograms of wild and cultivated rhizomes of P. polyphylla var. yunnanensis were established and nine steroidal saponins were simultaneously determined by the above method. The mean contents of paris saponin Ⅶ, paris saponin H and total average contents of four pennogenyl saponins in Rhizomes of wild samples were significantly higher than those of cultivated ones. However, this result is opposite from the average content of paris saponin Ⅰ and total average contents of five dioscins in the wild and cultivated samples. Because the significant differences occurred for the specific chromatograms and main active components between the wild and cultivated P. polyphylla var. yunnanensis, much more pharmacological and clinical researches are therefore necessary.
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This study is to establish the HPLC specific chromatogram and determine four main nucleosides of wild and cultivated Cordyceps sinensis. Uridine, inosine, guanosine and adenosine were selected as reference substance. HPLC analysis was performed on a Waters XSelect HSS T3 C₁₈ (4.6 mm×250 mm, 5 μm), with a mobile phase consisting of water(A)-acetonitrile (B) at a flow rate of 0.6 mL•min⁻¹ (0-5 min,0% B;5-15 min,0%-10% B, 15-30 min,10%-20% B, 30-33 min, 20%-50% B, 33-35 min, 50%-0% B, 35-40 min, 0% B). The detection wavelength was 260 nm and the column temperature was controlled at 30 ℃, and the injection volume was 5 μL. HPLC specific chromatogram of wild and cultivated C. sinensis was established and four main nucleosides were simultaneously determined by the above method. Specific chromatograms and contents of four main nucleosides showed no significant differences between cultivated and wild C. sinensis. These results can provide scientific evidences for further development and utilization of cultivated C. sinensis.
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To establish and analyze the HPLC specific chromatograms of Xingnaojing injection manufactured by different factories. The separation was performed on a Thermo BDS Hypersil C₁₈ column (4.6 mm×250 mm, 5 μm), with the mobile phase consisting of acetonitrile-0.02% formic acid aqueous solution for gradient elution. The flow rate was 1.0 mL•min⁻¹, and the column temperature was 35 ℃. The detection wavelength was set at 254 nm, and the sample size was 20 μL. Eleven chromatographic peaks were identified as characteristic peaks of HPLC specific chromatograms of Xingnaojing injection, after analyzing 29 batches of Xingnaojing injection samples. Compared with the reference substances, seven of them were identified as eucarvone, camphor, curcumenone, curcumenol, curdione, curzerenone and germacrone, respectively. HPLC specific chromatograms of Xingnaojing injection manufactured by three factories could be easily classified into three categories after investigation with computer-aided similarity evaluation system combined with principal component analysis. The established HPLC specific chromatograms provide a basis for scientific evaluation and effective control of the quality of Xingnaojing injection.
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Objective: To establish the method for the specific chromatograms analysis of Crocus sativus, so as to distinguish the active constituents between saffron and gardenia. Methods: HPLC with ZorBax XDB-C18 column was used, the mobile phase was a linear gradient of methanol containing 0.5% acetic acid and water containing 0.5% acetic acid in 45 min, the detection wavelength was set at 254 nm and the flow-rate was 1.0 mL/min. Results: Multi batches of samples were analyzed to establish the specific chromatograms. Eight marked peaks were separated. The methodological evaluation showed that the method had a good repeatability. The active constituents between saffron and gardenia could be significantly distinguished by this method. Conclusion: The method is simple, rapid, and accurate with good reproducibility and can be used for the quality control and identification of C. sativus.