Online extraction-high performance liquid chromatography-diode array detector-quadrupole time-of-flight tandem mass spectrometry for rapid flavonoid profiling of Fructus aurantii immaturus.
Abstract Chemical profiling of natural products by high performance liquid chromatography (HPLC) was critical for understanding of their clinical bioactivities, and sample pretreatment steps have been considered as a bottleneck for analysis. Currently, concerted efforts have been made to develop sample pretreatment methods with high efficiency, low solvent and time consumptions. Here, a simple and efficient online extraction (OLE) strategy coupled with HPLC–diode array detector–quadrupole time-of-flight tandem mass spectrometry (HPLC–DAD–QTOF-MS/MS) was developed for rapid chemical profiling. For OLE strategy, guard column inserted with ground sample (2 mg) instead of sample loop was connected with manual injection valve, in which components were directly extracted and transferred to HPLC–DAD–QTOF-MS/MS system only by mobile phase without any extra time, solvent, instrument and operation. By comparison with offline heat-reflux extraction for Fructus aurantii immaturus (Zhishi), OLE strategy presented higher extraction efficiency perhaps because of the high pressure and gradient elution mode. A total of eighteen flavonoids were detected according to their retention times, UV spectra, exact mass, and fragmentation ions in MS/MS spectra, and compound 9, natsudaidain-3-O-glucoside, was discovered in Zhishi for the first time. It is concluded that the developed OLE–HPLC–DAD–QTOF-MS/MS system offers new perspectives for rapid chemical profiling of natural products.
#1Li Duan(CPU: China Pharmaceutical University)H-Index: 11
#2Li-Li Dou(CPU: China Pharmaceutical University)H-Index: 8
Last. E-Hu Liu(CPU: China Pharmaceutical University)H-Index: 30
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Citrus polymethoxyflavones (PMFs) have been of increasing interest due to their extensive biological activities. In the present study, a total of eight PMFs were isolated from the peel of Citrus reticulata ‘Chachi’ (CRC). They were individually identified as 5-hydroxy-6,7,8,4′-tetramethoxyflavone (1), 5,6,7,3′,4′-pentamethoxyflavanone (2), 5-hydroxy-6,7,8,3′,4′-pentamethoxyflavone (3), 3,5,6,7,8,3′,4′- heptamethoxyflavone (4), 5,6,7,8,3′,4′-hexamethoxyflavone (5), 5,6,7,8,4′-pentamethoxyflavone ...
Last. Yu-Jie Fu(NEFU: Northeast Forestry University)H-Index: 61
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Abstract Nowadays, green extraction of bioactive compounds from medicinal plants has gained increasing attention. As green solvent, deep eutectic solvent (DES) have been highly rated to replace toxic organic solvents in extraction process. In present study, to simultaneous extraction five main bioactive compounds from fig leaves, DES was tailor-made. The tailor-made DES composed of a 3:3:3 molar ratio of glycerol, xylitol and D-(−)-Fructose showed enhanced extraction yields for five target compo...
#1De Ji(Nanjing University of Chinese Medicine)H-Index: 1
#2Ziyan Huang(Nanjing University of Chinese Medicine)H-Index: 4
Last. Tu-lin Lu(Nanjing University of Chinese Medicine)H-Index: 1
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Abstract The rhizome of Anemarrhena asphodeloides Bge. is commonly used as an herbal medicine in China. In this study, ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS) was used, in both negative and positive ion modes, to comprehensively analyze the chemical constituents of A. asphodeloides. From the intact precursor ions, MS/MS fragmentation information, and previous reports, we identified 89 compounds. These compounds include...
Last. Yongjiang Wu(ZJU: Zhejiang University)H-Index: 22
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Abstract Yangxinshi Tablet (YXST) is a Chinese patent medicine commonly used to treat cardiovascular diseases. However, its detailed chemical basis and mechanisms of action have not been clarified. In this study, high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry (HPLC–ESI-Q-TOF-MS) was applied for comprehensive analysis of the chemical constituents in YXST. A total of 127 compounds, including 19 phenolic acids, 12 alkaloids, 5...
Abstract An analytical method for the analysis of 16 pharmaceuticals and personal care products in compost from sewage sludge is successfully validated. Ultrasound assisted extraction with a mixture of acetonitrile:ethyl acetate (1:1, v/v) containing 10% (v/v) of acetic acid was carried out. Two cycles of extraction of 10 min were applied. A clean-up of the extracts using salt-assisted liquid–liquid extraction (SALLE) was also included. Experimental design was used for the optimization of the ma...
#1Qingping Gao(CSU: Central South University)H-Index: 1
#2Ruyi Ma(CSU: Central South University)H-Index: 1
Last. Haiyan Xiang(Southern Medical University)H-Index: 6
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Abstract Vine tea with strong antioxidant activity is commonly consumed as healthy tea/beverage. However, detailed information about its antioxidants is incomplete. Here, off-line hyphenation of heart-cutting high-speed countercurrent chromatography (HSCCC) with high performance liquid chromatography–diode array detector–quadrupole time-of-flight tandem mass spectrometry (HPLC–DAD–QTOF-MS/MS) were described for systematic profiling antioxidants in vine tea. At first, antioxidants were rapidly sc...
#1Nicole Bajcsik(TUK: Kaiserslautern University of Technology)H-Index: 1
#2Rudolf Pfab(TUM: Technische Universität München)H-Index: 9
Last. Jörg Pietsch(TUD: Dresden University of Technology)H-Index: 8
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Abstract A selective and sensitive analytical method for the simultaneous determination of cucurbitacin B, E, I and E-glucoside in plant material and body fluids by HPLC–MS was developed. After liquid–liquid extraction with dichlormethane, separation was achieved on a Phenomenex Luna Pentafluorophenyl Column (150 mm × 2 mm, 5 μm) using acetonitrile-water (90:10, v/v) as mobile phase system. Detection was performed using a 3200 Q Trap mass spectrometer (AB Sciex). For analysis Q1 Scans with negat...
#2H. N. M. Oliveira(UFRN: Federal University of Rio Grande do Norte)H-Index: 7
Last. Elisa de Sousa(UFRN: Federal University of Rio Grande do Norte)H-Index: 7
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Abstract In this study, Rumex Acetosa extracts were obtained from extraction techniques with supercritical fluid (SFE), Soxhlet and low pressure solvent extraction (LPSE). In the SFE, it was evaluated the effect of the process variables (temperature, solvent flow rate, pressure and cosolvent concentration) on the extraction kinetics, yield and extract solubility. In the Soxhlet extraction, it was evaluated the usage of ethanol, acetonitrile, isopropanol and tert -butyl alcohol, while in LPSE ext...
#1Pei Li(CPU: China Pharmaceutical University)H-Index: 2
#2Su-Ling Zeng(CPU: China Pharmaceutical University)H-Index: 11
Last. E-Hu Liu(CPU: China Pharmaceutical University)H-Index: 30
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Abstract To get a better understanding of the bioactive constituents in Aurantii Fructus Immaturus (AFI) and Aurantii Fructus (AF), in the present study, a comprehensive strategy integrating multiple chromatographic analysis and chemometrics methods was firstly proposed. Based on segmental monitoring, a high-performance liquid chromatography (HPLC)-variable wavelength detection method was established for simultaneous quantification of ten major flavonoids, and the quantitative data were further ...
Current methods employed for the analysis of the chemical composition of solid matrices (such as plant, animal, or human tissues; soil; etc.) often require many sample treatment steps, including an extraction step with exclusively dedicated solvents. This work describes an optimized analytical setup in which the extraction of a solid sample is directly coupled to its analysis by high-performance liquid chromatography. This approach avoids (i) the use of pumps and valves other than those comprisi...
#1Yan Cao(Beijing University of Chinese Medicine)H-Index: 5
#2Wenjing Liu(Beijing University of Chinese Medicine)H-Index: 9
Last. Yuelin Song(Beijing University of Chinese Medicine)H-Index: 23
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Abstract null null Extraction is responsible for transferring components from solid materials into solvent. Tedious extraction procedures are usually involved in liquid chromatography-based chemical analysis of herbal medicines (HMs), resulting in extensive consumptions of organic solvents, time, energy, and materials, as well as the significant chemical degradation risks for those labile compounds. Fortunately, an emerging online pressurized liquid extraction (OLE, also known as online liquid e...
#1Hua Guo(LNUTCM: Liaoning University of Traditional Chinese Medicine)
#2Yue-Hua Chen(LNUTCM: Liaoning University of Traditional Chinese Medicine)
Last. Hui Zhang(LNUTCM: Liaoning University of Traditional Chinese Medicine)H-Index: 2
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Abstract The lack of direct connection between traditional herbal medicines and multiple biological targets is a bottleneck in herbal research and quality evaluation. To solve this problem, a strategy for the discovery of active ingredients from function-similar herbal medicines based on multiple biological targets was proposed in this article. The technical route includes chromatographic separation, mass spectrometry analysis, enzymatic activity detection, pharmacophore analysis and molecular d...
New treatment strategies for schistosomiasis should be evaluated, since resistant strains to the only available drug, Praziquantel, have already been described. Thus, we demonstrated antiparasitic effects of ethanolic extracts of Jatropha gossypiifolia and Piper arboreum on cercariae and adult worms of Schistosoma mansoni. The bioassays were performed at 0-10 000 μg mL-1 concentration for 0-72 h. Adult worms were stained with carmine to assess external and internal damage. The chemical screening...
Last. Chunjie Zhao(SPU: Shenyang Pharmaceutical University)H-Index: 6
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Sanhua decoction, a famous Chinese herbal formula has been widely used for the treatment of stroke. In our study, a rapid, swift and straightforward analytical method with the help of UHPLC-FT-ICR-MS/MS was successfully developed for the first time to separate and identify the chemical constituents of Sanhua decoction. Chromatography was performed on a Universal XB C18 column (150 mm × 2.1 mm, 1.8 μm) using a mobile phase containing 0.1% formic acid–water (A) and acetonitrile (B). A total of 137...
Abstract This work investigates the applicability of on-line extraction (OLE) directly coupled to liquid chromatography (LC) for the dynamic extraction of hydrophobic organic compounds from complex solid samples. The method operates within the existing apparatus of the LC by replacing the valve loop with an extraction vessel comprised of an empty guard column loaded with the sample. In this manner, extraction is accomplished by the mobile phase as it flows through the extraction vessel under hig...
Abstract Du-zhong brick tea (DBT), a new post-fermented functional tea, is marketed in China for its prevention of diseases from oxidative stress. However, antioxidant compounds in DBT are not clear. Here, a novel online extraction–HPLC–ferric reducing antioxidant power (OLE–HPLC–FRAP) has been developed to screen antioxidants in DBT. For OLE, guard column is packed with DBT (1.0 mg), then compounds are extracted directly by HPLC mobile phase for HPLC–FRAP analysis without sample pretreatment pr...
The quercetin molecularly imprinted polymer microspheres were prepared by reversible addition-fragmentation chain transfer free radical polymerization combined with precipitation method (RAFTPP) with the dibenzyl trithiocarbonate (DBTTC) as RAFT reagent and quercetin as template molecule. The effects of solvents and cross-linking agent on the morphology and size of polymers were investigated, and the polymers were preliminarily screened by scanning electron microscope. The adsorption experiment ...
#1Chaoying Tong(CSU: Central South University)H-Index: 9
#2Jinju Xu(CSU: Central South University)H-Index: 6
Last. Shuyun Shi(CSU: Central South University)H-Index: 35
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Rapid extraction, discrimination and quantification of isomers, especially for thermally unstable isomers, in complex natural products by direct MS are of great challenge due to the time-consuming sample pretreatment procedures, thermal instability, and identical mass behaviors. This work developed an online extraction-quadrupole time-of-flight tandem MS (OLE-QTOF-MS/MS) system for quantification of isomeric phenylethanoid glycosides (acteoside and isoacteoside; acteoside isomerizes to isoacteos...
Last. Alejandro Cifuentes(CSIC: Spanish National Research Council)H-Index: 78
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Abstract Recently, the high analytical power provided by the new HRMS instruments (working in the MS or MS/MS mode, stand alone or hyphenated with separation techniques) is making more feasible the characterization of plant secondary metabolites. In this regard, HRMS-based techniques are becoming the technique of choice, since they are capable of answering many questions regarding the analytical characterization of secondary metabolites, usually found in very complex matrices, including their st...
#1Chaoying Tong(CSU: Central South University)H-Index: 9
#2Xia Tong(CSU: Central South University)H-Index: 6
Last. Keke Guo(CSU: Central South University)H-Index: 6
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Abstract Rapid differentiation, characterization and quantification of isomers from complex mixtures by direct mass spectrometry (MS) remained an analytical challenge due to their similar or identical MS/MS spectra and matrix interferences. Here, we reported a novel online extraction–quadrupole time-of-flight tandem mass spectrometry (OLE–QTOF-MS/MS) system to rapid, efficient and sensitive analysis of interglycosidic linkage isomers (hesperidin and neohesperidin) in Citrus paradisi cv. Changsha...