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Ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS) was used to establish the chromatography fingerprint for aerial parts of Angelica sinenis(AAS) from 10 different places. Acetyl-phenyl-hydrazine(APH) was used to duplicate the mouse model of blood deficiency. Then partial least squares regression was used to investigate the spectrum-effect relationship between the relative contents and the data of enriching blood pharmacodynamics efficacy. The results showed that the three groups of high, medium and low doses of AAS had certain enriching blood activities(P<0.05), and the high dose group had the best effect(P<0.01). The contribution degree of the AAS to enriching blood activities of each common peaks were determined by PLS regression coefficient. Among them, 7 common peaks, including P17(unknown), P18(unknown), P19(unknown), P28(alisol B 23-acetate or its isomer), N5(luteolin), N11(1-caffeoylquinicacid,1-O-caffeoylquinic acid) and N14(unknown), contributed significantly to the effect of enriching blood activities. This paper dealed with the investigation on the spectrum-effect relationship between enriching blood activities and LC-MS chromatography fingerprint of AAS, and determination of the effective compositions of AAS with enriching blood activities. It provided theoretical foundation for the comprehensive development and utilization of AAS.
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Animals , Mice , Angelica , Chemistry , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Pharmacology , Mass Spectrometry , Medicine, Chinese Traditional , Plant Components, Aerial , ChemistryABSTRACT
Objective In this paper, HPLC-DAD-ELSD technique was used to establish the chromatography fingerprint of Ilex kudingcha. Methods Shimadzu C18 column (250 mm × 4.6 mm, 5 μm) was used. Acetonitrile-water as the mobile phase; The flow speed was 1.0 mL/min. The detection wavelength was 210 nm and the column temperature was 35 ℃. Results The chromatography fingerprint of Ilex kudingcha from 10 different origins was established. In the chromatography fingerprint with HPLC-DAD of Ilex kudingcha, 18 common peaks were damarcated and the similarities of Ilex kudingcha were between 0.911-0.970, and the chromatography fingerprint with HPLC-ELSD of Ilex kudingcha, 11 common peaks were damarcated and the similarities of Ilex kudingcha were between 0.914-0.962. Chlorogenic acid, kaempferol-3-O-β-D-rhamnoside, isorhamnetin-3-O-β- D-rhamnoside, kudinoside C, kudinoside A, kudinoside E, kudinoside D were confired by LC-MS and binding control. Conclusion The method of precision, reproducibility, stability is accurate, which can be used as the evaluation of the quality of Ilex kudingcha.
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Objective: To establish the chromatography fingerprint of Polygoni Cuspidati Rhizoma et Radix with hyphenated technique of HPLC-DAD-ELSD and to evaluate Polygoni Cuspidati Rhizoma et Radix from 10 different origins. Methods: Luna C18 (2) column (250 mm × 4.6 mm, 5 μm) was used. Mobile phase was acetonitrile-H2O; Flow speed was 1.0 mL/min; Temperature of column was set at 35℃; Detective wavelength was at 254 nm; Injection volume was 10 μL. The temperature of drift tube was 109℃ and the flow speed was 3.0 L/min. Results: The chromatography fingerprint of Polygoni Cuspidati Rhizoma et Radix from 10 different origins was established. In the chromatography fingerprint with HPLC-DAD of Polygoni Cuspidati Rhizoma et Radix, 19 common peaks were demarcated and the similarities of Polygoni Cuspidati Rhizoma et Radix were between 0.938-0.993. In the chromatography fingerprint with HPLC-ELSD of Polygoni Cuspidati Rhizoma et Radix, 14 common peaks were demarcated and the similarities of Polygoni Cuspidati Rhizoma et Radix were between 0.905-0.999. Polydatin, resveratrol, emodin-8-O-β-D-glucoside, physcion-8-O-β-D-glucoside, emodin, and physcion were identified. Conclusion: The method is accurate and stable, which can be used as the evidence for the quality evaluation of Polygoni Cuspidati Rhizoma et Radix.
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Objective: To establish the chromatography fingerprint of Schisandra chinensis Chewable Tablets (SCCT) with HPLC-DAD and to evaluate SCCT from 10 different batches. Methods: Luna C18 column (250 mm×4.6 mm, 5 μm) was used, mobile phase was acetonitrile-0.05% phosphate, flow speed was 1.0 mL/min, temperature of column was set at 35℃, detected wavelength was at 220 nm, and injection volume was 20 μL. Results: The chromatography fingerprint of SCCT from 10 different batches was established. In the chromatography fingerprint with HPLC-DAD of SCCT, 39 common peaks were demarcated and the similarities of SCCT were between 0.914-0.999. Schizandrin, schisandrol B, schisantherin A, schisandrin B, schisandrin C, salvianic acid A sodium, salvianolic acid B, cryptotanshinone, tanshinone IIA, 3, 4-dihydroxyhenzaldehyde, luteoloside, and buddleoside were identified. Conclusion: The method is accurate, reliable and with good reproducibility, and can be used as the evidence for the quality evaluation of SCCT.
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Objective To investigate fingerprint analysis and quantification of Rhizoma Drynaria. Methods HPLC fingerprints were carried out at 30° on a Zirchrom C18 column (4.6 mm×200 mm, 5 µm). The mobile phase was methanol (A) and phosphoric acid aqueous solution (pH3.6, B). Gradient programmer was performed in linear gradient The chromatogram was monitored at a wavelength of 283 nm throughout the experiment and the chromatographic peaks were obtained, ranging from 200 nm to 400 nm. The injection volume was 10 µl. Then quantitative analyses were carried out at 30$ on a Kromasil C18 column (250 mm×4.6 mm,5 µm). Results In fingerprint analysis, plant materials from 16 regions were analyzed under the optimized HPLC conditions and 12 peaks were selected as characteristic peaks Compared with the reference standards, 6 major chromatographic peaks were characterized and identified, with sum of peaks area over 70% according to area normalization method. Additionally, the similarity analysis and HCA analysis were performed and the results got mutual authentication In quantitative analysis, the four compounds showed good regression (r>0.9995) within test ranges and the recovery of the method was in the range of 97.9%-103.7%. Conclusion The results revealed that the method of reference chromatographic fingerprints combined with multiple compounds determination could be used as an efficient strategy for systematic quality evaluation of Rhizoma Drynariae.
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Objective To investigate fingerprint analysis and quantification of Rhizoma Drynaria. Methods HPLC fingerprints were carried out at 30℃on a Zirchrom C18 column (4.6 mm×200 mm, 5μm). The mobile phase was methanol (A) and phosphoric acid aqueous solution (pH3.6, B). Gradient programmer was performed in linear gradient. The chromatogram was monitored at a wavelength of 283 nm throughout the experiment and the chromatographic peaks were obtained, ranging from 200 nm to 400 nm. The injection volume was 10μl. Then quantitative analyses were carried out at 30℃on a Kromasil C18 column (250 mm×4.6 mm,5μm). Results In fingerprint analysis, plant materials from 16 regions were analyzed under the optimized HPLC conditions and 12 peaks were selected as characteristic peaks. Compared with the reference standards, 6 major chromatographic peaks were characterized and identified, with sum of peaks area over 70% according to area normalization method. Additionally, the similarity analysis and HCA analysis were performed and the results got mutual authentication. In quantitative analysis, the four compounds showed good regression(r>0.9995) within test ranges and the recovery of the method was in the range of 97.9%-103.7%. Conclusion The results revealed that the method of reference chromatographic fingerprints combined with multiple compounds determination could be used as an efficient strategy for systematic quality evaluation of Rhizoma Drynariae.
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Objective To establish high performance liquid chromatograph ( HPLC ) fingerprint of liqi xiaoying tablets,and to provide reference for quality control of the herbal medication. Methods The chromatography conditions consisted of Aichrom Bond-AQ C18(250 mmí4. 6 mm,5 μm) column with mobile phase of acetonitrile-0. 1% phosphoric acid ( gradient elution) , column temperature of 30 ℃, flow rate of 1 mL · min-1 , injection volume of 20 μL, and UV detection wavelength of 226 nm. Results HPLC fingerprint was established with 13 common peaks,4 of which were identified. The similarity of the HPLC fingerprints of liqi xiaoying tablets from 10 batches was greater than 0. 95. Conclusion The method is accurate, reliable, and can reflect complete information for the quality of liqi xiaoying tablets.
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Traditional Chinese medicines (TCMs) are in great demand all over the world, especially in the developing world, for primary health care due to their superior merits such as low cost, minimal side effects, better cultural acceptability, and compatibility with humans. However, Chinese medicines consist of several herbs which may contain tens, hundreds, or even thousands of constituents. How these constituents interact with each other, and what the special active ones are, may be the biggest bottleneck for the modernization and globalization of TCMs. Valid methods to evaluate the quality of TCMs are therefore essential and should be promoted and be developed further through advanced separation and chromatography techniques. This paper reviews the strategies used to control the quality of TCMs in a progressive perspective, from selecting single or several ingredients as the evaluation marker, to using different kinds of chromatography fingerprint methods. In summary, the analysis and quality control of TCMs are developing in a more effective and comprehensive manner to better address the inherent holistic nature of TCMs.
Subject(s)
Chemistry Techniques, Analytical , Methods , Drugs, Chinese Herbal , Chemistry , Reference Standards , Medicine, Chinese Traditional , Reference Standards , Plants, Medicinal , Chemistry , Quality ControlABSTRACT
AIM:To establish some HPLC-digitized fingerprint spectrum(HPLC-DFPS)in Liuwei Dihuang Dripping Pill preparation and to apply it to identification of medicinal materials.METHODS:Based on loganin and paeonoside contents adopted as qualitative and quantitative factors,relative retention value as creteria,RPHPLC was carried out on inensil ODS:column,mobile phase consisted of methanol-water(0.2% formyl acid),detection wavelength was set at 240 nm.RESULTS:Using above optimum chromatograph conditions,HPLC-DFPS of relative medicinal materials andLiwei Dihuang Dripping Pillpreparation were established.By comparison a group of characteristic peaks could be used to identify medicinal materials.CONCLUSION:This result indicates that it is practical to use HPLC-DFPS for identification of Liawei Dihuang Dripping Pill.
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Objective Chromatography fingerprint of Radix Codonopsis of different age from Shanxi province was studied to provide the reference for the science appraisal of intrinsic quality of Radix codonopsis. Method A RP-HPLC method was applied on GraceSmart-RP18 (250 mm?4.6 mm, 5 ?m) column with acetonitrile-0.1% acetic acid gradient elution as mobile phase, and the flow-rate was 0.6 mL/min. The detection wavelength was at 268 nm and the column temperature was at 30 ℃. Result Chromatography fingerprint of Radix Codonopsis can demonstrate obviously the difference and the similarity of Radix Codonopsis of different age. The RSD were lower than 3% in the precision, stability and the repetitiveness trial, and the codonopsis pilosula alkyne glucoside can be used as the reference to identify the active composition of Radix Codonopsis. Conclusion The method was simple, reproducible and reliable. The integrity of fingerprint can be used to supply the reference for the quality control of Radix Codonopsis from Shanxi provice.
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AIM:To establish some HPLC-digitized fingerprint spectrum(HPLC-DFPS)in Liuwei Dihuang Dripping Pill preparation and to apply it to identification of medicinal materials.METHODS:Based on loganin and paeonoside contents adopted as qualitative and quantitative factors,relative retention value as creteria,RP-HPLC was carried out on inertsil ODS:column,mobile phase consisted of methanol-water(0.2% formyl acid),detection wavelength was set at 240 nm.RESULTS:Using above optimum chromatograph conditions,HPLC-DFPS of relative medicinal materials and "Liwei Dihuang Dripping Pill" preparation were established.By comparison a group of characteristic peaks could be used to identify medicinal materials.CONCLUSION:This result indicates that it is practical to use HPLC-DFPS for identification of Liuwei Dihuang Dripping Pill.
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AIM:To establish the chromatography fingerprint of the constituents of Melia toosendan Sieb from different areas in order to provide a base for the identification of its quality. METHODS: A gradient separated method was applied. Column:Inertsil ODS-3 C_ 18 ,mobile phase:acetonitrile-water,detection wavelength:270 nm,flow rate:1.0 mL/min,column temperature:25 ℃. RESULTS: To establish the chromatography fingerprint of the constituents of Melia toosendan Sieb., make the technical parameters for its quality controlling,and mark 39 main peaks as its characteristic fingerprint. CONCLUSION: The distribution of constituents of Melia toosendan Sieb differ a little from different areas, but the propotion of the constituents differ greatly, with the Melia toosendan Sieb.from the same area , the distribution and propotion differ a little. This method is reproducible, simple and easy, and can be use to provide a base for the quality control of Melia toosendan Sieb.
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AIM To establish chromatography fingerprint of Radix Codonopsis. METHODS HPLC was applyed on a Hypersil ODS column with water-methanol gradient elution, flow-rate of 0.8 ml?min -1 . Determination of content of atractylenodie Ⅲ adopted ELSD and PAD with methanol-water(67∶ 33), flow-rate of 1.0 ml?min -1 , column temperature at 30?C , ELSD:carried-gas flow-rate of 2.2 L?min -1 , drift-tuber temperature was 80?C ;PAD:wavelength was 220 nm. RESULTS 25 common peaks were picked up, their similarity among 10 batchs of samples was more than 98.12 % based on marker composition(Atractylenolide Ⅲ). CONCLUSION The chromatography fingerprint of Baitiao Radix Codonopsis could be used as their characteristic chromatography fingerprint of hydrophobic fraction.