Separation Of Chemical Components Research Articles

Research Progress in the Separation of Chemical Components from Essential Oils by High-Speed Countercurrent Chromatography

Essential oils (EOs) are vital secondary metabolites in plants. They have garnered substantial attention owing to their distinct flavors and desirable attributes, including potent antioxidant, antibacterial, and antitumor properties. Nevertheless, the active constituents of EOs exhibit intricate chemical structures, and conventional separation techniques are inadequate for purifying the individual chemical components from EOs. High-speed countercurrent chromatography, based on the principles of a hydrodynamic equilibrium system, has emerged as a liquid–liquid chromatographic separation method renowned for its ability to handle substantial single injection volumes and the absence of irreversible adsorption. Consequently, in recent years, this technique has been widely employed in the isolation and refinement of natural products. In this review, a comprehensive analysis is conducted, contrasting the merits and demerits of high-speed countercurrent chromatography with conventional separation methods. The solvent systems, elution modes, commonly employed detectors, and practical applications are reviewed in the context of high-speed countercurrent chromatography for essential oil separation and purification. Furthermore, this review offers a glimpse into the potential prospects of applying this technique, with the intention of serving as a valuable reference for the use of high-speed countercurrent chromatography in the purification of EOs.

An online preparative high-performance liquid chromatography system with enrichment and purification modes for the efficient and systematic separation of Panax notoginseng saponins

In this study, an online preparative high-performance liquid chromatography (prep-HPLC) system based on the combination of the enrichment and purification modes for the efficient and systematic separation of Panax notoginseng saponins (PNS) was achieved. Five separation columns were used for the first and second separation of target components, eighteen trap columns were used to capture the effluents from the first separation or loading the trapped sample effluents, and a two-position eight-port valve was used to switch between the first and second separations. The conditions for the first and second separation of PNS were simulated and optimized with the online prep-HPLC system. Then, the PNS were separated using optimized chromatographic conditions. Notably, 14 monomer compounds with >90% purity (11 compounds with purity >97%) were simultaneously isolated from PNS using the above self-developed device, and their chemical structures were identified. Moreover, the separation time was less than 33.0 h. After 6 repeated enrichment and purification, the weight of each compound obtained was more than 5.0 mg, with compound 2 weighing over 900 mg. In brief, the self-developed prep-HPLC system, which integrated enrichment and purification, is suitable for the efficient and systematic separation of PNS and has broad application prospects, especially for the separation of complex chemical components in natural products.

Antifungal Effects and Active Components of Ligusticum chuanxiong

The separation of chemical components from wild plants to develop new pesticides is a hot topic in current research. To evaluate the antimicrobial effects of metabolites of Ligusticum chuanxiong (CX), we systematically studied the antimicrobial activity of extracts of CX, and the active compounds were isolated, purified and structurally identified. The results of toxicity measurement showed that the extracts of CX had good biological activities against Botrytis cinerea, Sclerotinia sclerotiorum, Alternaria alternata and Pythium aphanidermatum, and the value of EC50 were 130.95, 242.36, 332.73 and 307.29 mg/L, respectively. The results of in vivo determination showed that under the concentration of 1000 mg/L, the control effect of CX extract on Blumeria graminis was more than 40%, and the control effect on Botrytis cinerea was 100%. The antifungal active components of CX were identified as Senkyunolide A and Ligustilide by mass spectrometry and nuclear magnetic resonance. The MIC (minimum inhibitory concentration) value of Senkyunolide A and Ligustilide against Fusarium graminearum were 7.81 and 62.25 mg/L, respectively. As a new botanical fungicide with a brightly exploitative prospect, CX extract has potential research value in the prevention and control of plant diseases.

Phenolic Compounds of Rumex L: Aerial Part Fractions and Essential Oil Results of In vitro Screening for Antimicrobial Activity

The aim of the present study to clarify the phytochemical constituents of Rumex plants, extraction, separation and structural identification of chemical components, provide theoretical support and scientific basis for its traditional use, further expand the application scope of traditional medicinal plant resources in Uzbekistan, and develop its potential value. Three known anthraquinone derivatives has been isolated from the chloroform fraction extract of Rumex pamiricus roots and two known compounds were separated from the ethyl acetate fraction extract of Rumex conglomeratus roots. Their structures were elucidated by extensive spectroscopic evidence and chemical methods. Qualitative analyses of major phenolics by TLC analysis were also evaluated. The ester oil from the aerial parts of Rumex confertus and Rumex pamiricus, the gasoline, chloroform, ethyl acetate and butanol extracts of Rumex pamiricus aerial part and alcohol extract of Rumex pamiricus roots were tested in vitro for antimicrobial activity.
 This study aimed to determine the in vitro antimicrobial activity of the medicinal plants traditionally used in Uzbekistan against the microbial strains associated with infectious diseases.

Separation and anti-inflammatory evaluation of phytochemical constituents from Pleurospermum candollei (Apiaceae) by high-speed countercurrent chromatography with continuous sample load.

Pleurospermum (Apiaceae) species possess a wide range of biological properties viz. analgesic, anti-inflammatory, antimalarial, and so on. Pleurospermum candollei (DC.) Benth. Ex C. B. Clark. is reported to cure diarrhea, gastric, respiratory, stomach, abdominal, joint, and back pain problems. In addition, it is also used for both male and female infertility. The present study deals with an efficient technique using high-speed countercurrent chromatography for separation of chemical components from the methanol extract of P. candollei. Notably, nine main compounds namely luteolin 7-O-glucoside (1), oxypeucedanin hydrate (2), pabulenol (3), bergapten (4), heptadecanoic acid (5), (E)-isoelemicin (6), trans-asarone (7), α-linolenic acid (8), and isoimperatorin (9) were very efficiently separated and isolated in pure form. Multiple injections were applied followed by two off-line recycling high-speed countercurrent chromatography. The inhibitory effect of nitric oxide production of all compounds was tested in the presence of 200ng/mL lipopolysaccharide in RAW264.7 mice macrophage cells. The results demonstrated that compounds 7 and 8 effectively inhibited nitric oxide production, with IC50 values of 28.44 and 53.18μM, respectively. This study thus validates the traditional claim of using P. candollei. Taken together, these findings will be useful in future research to find a potential candidate with anti-inflammatory properties.

Study on Separation and Purification of Chemical Components of Dichloromethane from Pine Needle Extract

To study the chemical composition of the extract of cedar pine needle methylene chloride. Methods: The paper used silica gel and Sephadex LH-20 column chromatography to separate and purify, and carried out structural identification based on physical and chemical properties and spectral data. At the same time, gallic acid was preliminarily separated by high-performance liquid chromatography (HPLC), the separation conditions of gallic acid were determined, and the content change of gallic acid after tannin was acid-decomposed was determined, proving that the extract may contain decomposable hydrolysis Tannin or compound tannin. Results: Five compounds were isolated from the dichloromethane extract of cedar pine needles, which were identified as: ferulic acid (1), osthol (2), β-phenylacrylic acid (3), paeonol (4), Magnolol (5). Conclusion: All compounds except Compound 5 were isolated from this plant for the first time.

A novel online preparative high-performance liquid chromatography system with the multiple trap columns-valve switch technique for the rapid and efficient isolation of main flavonoids from Epimedium koreanum Nakai.

In this work, a new online preparative high-performance liquid chromatography was developed for the fast and efficient separation of complex chemical mixtures from natural products. This system integrates two chromatographic systems into an online automatic separation system using the technique of multiple trap columns with valve switching. The sample was first separated into 18 subfractions in the online preparative high-performance liquid chromatography, and the sample eluents were then diluted and captured online on 18 trap columns by the multiple trap columns technique, respectively. Each subfraction retained on the trap column was transferred online to the separation column for the second separation. Finally, the target compounds were purified by appropriate separation conditions and multiple heart-cutting strategies. Importantly, the system was successfully used to separate 18 high-purity flavonoids from the crude extract of Epimedium koreanum Nakai online in one step. The entire separation time was approximately 20 h, and the structures were characterized by the high-performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry and nuclear magnetic resonance. This online preparative high-performance liquid chromatography system represents an efficient and rapid separation system that has the potential for a wide array of applications in the separation of complex chemical components from natural products.

Magnetic molecularly imprinted polymer combined with high performance liquid chromatography for selective extraction and determination of the metabolic content of quercetin in rat plasma

In this study, a novel magnetic solid phase extraction adsorbent was prepared, namely Fe3O4@SiO2 as the carrier, quercetin as the template molecule, acrylamide (AM) as the functional monomer, ethylene glycol dimethacrylamide (EGDMA) as the crosslinker, 2,2′-azobisisobutyronitrile (AIBN) as the initiator to prepare magnetic molecularly imprinted polymer (MMIPs) with specific adsorption of quercetin by surface molecular imprinting technique. MMIPs were characterized by Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and transmission electron microscope (TEM). The binding properties of MMIPs were evaluated by isothermal adsorption, kinetic adsorption and selective adsorption experiments. The results showed that the saturated adsorption capacity and adsorption time were 17.9 μmol/g and 20 min, respectively, and showed high selectivity for quercetin. Under optimized conditions, the limit of detection (LOD) and limit of quantitation (LOQ) were 55.327 ng/mL and 184.413 ng/mL, respectively. The recovery and RSD were 85.34–95.67% and 3.36–6.59, respectively. We successfully combined magnetic solid phase extraction with high performance liquid chromatography (MSPE-HPLC-UV) for the enrichment, separation and detection of quercetin in rat plasma. The results showed that the peak and half-life of quercetin in plasma were 1.5 h (32.310 μg/mL) and 3 h, respectively. The method was simple, rapid and efficient, and could be applied to the separation and detection of quercetin in complex matrices, and also provides a basis for the separation and identification of other natural chemical components.

Isolation and Characterization of Flavonoids from Black Glutinous Rice (Oryza Sativa L. Var Glutinosa)

This study aims to isolate and characterize the isolated flavonoid compounds from glutinous rice (Oryza Sativa L. Var Glutinosa). The method that used was maserasi with methanol solvent, multilevel fractionation with n-hexane and ethyl acetate. The separation of chemical components using column chromatography and tested its purity by melting point test and TLC. Characterization of isolated flavonoids using color reagents (H2SO4, NaOH, Mg-HCl), KKt-2A, UV-Vis and FT-IR. The powder (amorphous) flavonoid isolation results have a melting point of 236.5-237.8 oC. Flavonoid powder added H2SO4 produces a yellow color, with NaOH producing a violet color, and Mg-HCl produces a red color. KKt-2A with a BAA developer has Rf 0.49 and 15% acetic acid having Rf 0.09. The UV-Vis spectrum shows maximum absorption at 532 nm wavelength. The results of powder analysis (amorphous) flavonoid using FT-IR showed absorption at wave number 3.330,40 cm-1, 2838,96 cm-1, 1,656,23 cm-1, 1,421,85 cm-1, 1,112,25 cm-1, 1,019,27 cm-1 and 697,76 cm-1. According to those data it can be concluded that flavonoids that isolated have the form of powder (amorphous) which belong to anthocyanin group that have o-diOH on ring B and have a conjugated double bond.Keywords- Black Sticky Rice, Flavonoid, Fractionation, FT-IR, Maserasi, UV-Vis.

Effect of Alcohols on Simultaneous Bio-oil Upgrading and Separation of High Value-added Chemicals

This paper studied the effect of alcohols on simultaneous esterification and alkylation reactions designed for the upgrading of bio-oil, and the separation of upgraded oil. The upgrading of bio-oil was performed in an autoclave with Amberlyst-36 as the catalyst, and methanol, ethanol, and n-butanol as the alcoholic solvents. The separation of various chemical components, such as unreacted solvents, water phase, extraction phase, and high value-added chemicals, in the upgraded oil were realized via distillation, at 80–90 °C (at 0.01 MPa) vacuum distillation and an extraction process. The results showed that, the simultaneous esterification and alkylation reactions for the upgrading of bio-oil not only restrained the acetylation reaction of aldehydes, which increased the relative contents of stable ethers, but also enhanced the oil soluble components of the upgraded bio-oil. After separation, the high value-added chemical, namely methyl-α-d-glucopyranoside, was obtained with 5.39 wt.% yield and a relative content of 88.9% (sugar phase). The results from this work also showed that this novel method was quite a promising technique for upgrading bio-oil together with the separation of the high value-added chemical.

Study on the separation of chemical components and hypoglycemic activity of Scrophularia ningpoensis Hemsl

This paper investigated the action of hydrophilic constituents from Scrophularia ningpoensis Hemsl. on glucose-lowering effect metabolism in Hep G2 cells.The crude extract by diacolating with 70% ethanol was redissolved in water and was loaded on a glass column containing D101 macroporous resin, and was separated by silica gel column and HSCCC to obtain compounds.The structures of compounds were identified by ~1H and 13C-NMR spectroscopic data, and cell assay was performed by MTT and Kit methods in high glucose model.Compounds were identified as acteoside ( 1) , prim-O-glucosylcimifugin ( 2) , aucubin ( 3) , harpagide ( 4) , D- ( +) -sucrose ( 5) , cinnamic acid ( 6) , harpagoside ( 7) , angroside C ( 8) and twenty-seven alkane ( 9) .Antihyperglycemic activity of each compounds in 0.1 ~ 2.5 μg/m L concentration range was selected, and glucose consumption ability of harpagoside was the highest. Twenty-seven alkane was isolated from the genus of Scrophularia ningpoensis Hemsl.for the first time.Antihyperglycemic activity of compound 7 of Scrophularia ningpoensis would be potentialand rich resources for drug development.

Selective isolation of components from natural volatile oil by countercurrent chromatography with cyclodextrins as selective reagent

Selective separation of chemical components from seven kinds of volatile oil by countercurrent chromatography with three types of cyclodextrins as selective reagent was investigated in this work. Preparative separation of chemical components from volatile oil is generally quite challenging due to their extremely complexity of the composition. A biphasic solvent system n-hexane-0.10molL−1 cyclodextrin (1:1, v/v) was selected for separation of components from volatile oil and three types of cyclodextrins were investigated, including β-cyclodexrin, methyl-β-cyclodexrin and hydroxypropyl-β-cyclodexrin. All kinds of volatile oils are from seven kinds of traditional Chinese herb. Results showed that some chemical components could be well separated with high purity from each kind of volatile oil using different type of cyclodextrin as selective reagent. For example, germacrone and curcumenone could be selectively separated from volatile oil of Curcumae Rhizoma with methyl-β-cyclodexrin and hydroxypropyl-β-cyclodexrin as selector respectively, and other five components were selectively separated from volatile oil of Chuanxiong Rhizoma, Myristicae Semen, Aucklandiae Radix and Angelicae Sinensis Radix by countercurrent chromatography with different cyclodexrin as selective reagent. Separation mechanism for separation of components from volatile oil by countercurrent chromatography with cyclodextrin as selective reagent was proposed. Peak resolution of the present separation method could be greatly influenced by the chemical compositions of volatile oil.

Separation of coal liquid distillate by dimethyl sulfoxide

Efficient separation of different chemical components in liquid hydrocarbons from direct coal liquefaction is a meaningful process. This paper aims to separate the 150–180°C coal liquid distillate into three fractions: aromatics, alkanes, and phenolics. The coal liquid distillate is composed mostly of hundreds of single-ring compounds and is not easy to study directly. Therefore, a model of the distillate on a molar ratio was defined as 1t-butylbenzene (TBB): 1t-butylcyclohexane (TBC): 1 phenol. And dimethyl sulfoxide (DMSO) was selected as the solvent to separate them from each other. The model compounds' vapor–liquid equilibrium shows that DMSO's effectiveness is obvious. In TBB-TBC-phenol ternary system, DMSO can entrain TBB into the light fraction and keep phenol in the heavy fraction, while TBC is in the middle fraction, which isn't affected. DMSOs' influence was studied and divided as follow: the hydrogen bond terminator between TBB and phenol, an entrainer for TBB, and an extractant for phenol. Finally the 150–180°C coal liquid distillate is separated via batch distillation into three fractions: 150–160°C fraction (containing 79.17wt.% aromatics and 20.25wt.% alkanes), 160–185°C fraction (containing 81.30wt.% alkanes and 17.69wt.% aromatics) and a bottom product (containing 27.95wt.% phenolics and 72.05wt.% DMSO).

On-line visualization of multicolor chemical images with stimulated Raman scattering spectral microscopy.

We demonstrate multicolor, on-line visualization in label-free biomedical microscopy based on stimulated Raman scattering (SRS). Fast data acquisition of SRS spectral images and subsequent image generation are achieved. The loading vectors for the blind separation of chemical components are predetermined by multivariate analysis at a certain field of view (FOV) and are applied to execute on-line visualization of chemical images at other FOVs. We also show that the response time can be shortened by reducing the number of spectral data points. This on-line visualization system is expected to increase the usability of the Raman imaging system and the analytical throughput for screening.

Electrochemical synthesis and functionality evaluation of silver nanostructured layers

The functionality of silver nanostructures prepared by means of electrochemical deposition of silver into the pores of anodic alumina oxide (AAO) template was examined in correlation to electrodeposition conditions. The optical activity as well as the chemical separation ability of prepared nanostructured films was studied. The surface enhanced Raman spectroscopy (SERS) performance was evaluated by the signals of rhodamine 6G, 4‐aminothiophenol and 2,7‐dichlorfluorescein. Nanostructured silver substrates showed moderate surface enhancement for Raman scattering from adsorbed molecules with the magnitude of about 26.9. Moreover, a novel separation/pre‐concentration function of the silver nanowire structures was indicated. The identification and position detection of the model compounds were realised with SERS. The separation of single chemical components from the two‐component mixture over the examined silver nanostructured films was sufficiently approved. The results obtained demonstrated the potential of the prepared substrate as a SERS detection and separation probe for further implementation to any instrumentation. Copyright © 2014 John Wiley & Sons, Ltd.

Extraction and separation of nickel and cobalt from saprolite laterite ore by microwave-assisted hydrothermal leaching and chemical deposition

Extraction and separation of nickel and cobalt from saprolite laterite ore were studied by using a method of microwave-assisted hydrothermal leaching and chemical deposition. The effects of leaching temperature and time on the extraction efficiencies of Ni2+ and Co2+ were investigated in detail under microwave conditions. It is shown that the extraction efficiencies of Ni2+ and Co2+ from the ore pre-roasted at 300°C for 5 h were 89.19% and 61.89% when the leaching temperature and time were about 70°C and 60 min, respectively. For the separation process of Ni and Co, the separation of main chemical components was performed by adjusting the pH values of sulfuric leaching solutions using a NaOH solution based on the different pH values of precipitation for metal hydroxides. The final separation efficiencies of Ni and Co were 77.29% and 65.87%, respectively. Furthermore, the separation efficiencies of Fe of 95.36% and Mg of 92.2% were also achieved at the same time.

UHPLC-Q-TOF/MS in rapid separation and identification of chemical components in <I>Veratrum nigrum</I> L

UHPLC-Q-TOF/MS in rapid separation and identification of chemical components in <I>Veratrum nigrum</I> L

OC-163 Identification of inflammatory bowel disease (IBD) using field asymmetric ion mobility spectrometry (FAIMS)

IntroductionResident colonic bacteria, principally anaerobes and firmicutes, ferment undigested fibre. The resultant volatile organic compounds (VOCs) formed are dissolved in the faeces but also absorbed and excreted in the urine....

SUPERCRITICAL CARBON DIOXIDE FRACTIONATION OF PITHECELLOBIUM JIRINGAN JACK SEED COMPOSITIONS USING FAST GAS CHROMATOGRAPHY TIME OF FLIGHT MASS SPECTROMETRY

ABSTRACTThe volatile oil components of ground Pithecellobium jiringan seeds were fractionated using supercritical carbon dioxide (SC‐CO2) at 80C and 6,000 psi. The extract was collected every 20 min and the yield was successively extracted into five fractions; thus, the total extraction time was 100 min. The yields (volatile oils) were analyzed with fast gas chromatography/time of flight mass spectrometry (Fast GC‐MS‐TOF) and 55 components were identified. The major components were found to be fatty acids, ally sulfur, vitamin E, terpenoids, and flavonoid and alkaloid compounds. The major components were present at different percentages in each fraction, where some compounds were more dominant in fraction 1 and extracted in the first 20 min where others were more dominant in later fractions. However, the SC‐CO2 and GC‐MS‐TOF may be regarded as new analytical tools for the separation and identification of chemical components from P. jiringan jack seeds. Substances extracted from P. jiringan jack seeds could be evaluated for anti‐diabetic and anti‐hypertensive effects.PRACTICAL APPLICATIONSPithecellobium jiringan seed was commonly consumed by Malaysians as raw vegetables dishes as appetizer. Traditionally, the use of raw vegetables is recommended for the prevention of diseases and for health care purposes. The selection of P. jiringan seeds as a material used in the supercritical carbon dioxide extraction is due to significance reasons. There is no in‐depth study on their valuable compounds, even though the use of P. jiringan seeds employed in traditional medicines is widespread among the local rural communities, especially for treatment of hypertension and diabetes. Hence, research studies on the chemical constituents and biological activities of this plant are needed. Because it is used in human consumption, a safe extraction technique as supercritical fluid technology is most apt for this research.

HPLC-TOFMS in rapid separation and identification of chemical components in <I>Oldenlandia diffusa</I> and its injection preparations

Objective To rapidly separate and identify the chemical components in traditional Chinese herbal medicine of Oldenlandia diffusa and its injection preparations by high performance liquid chromatography-time of flight mass spectrometry(HPLC-TOFMS).Methods An Agilent Zorbax XDB-Cl8 column(250 mm×4.6 mm,5 μm) was used for separation and identification of chemical components in Oldenlandia diffusa,with a mobile phase of 0.3% acetic acid(A) and methanol(B) in gradient elution,0-30 min,30%-90%B.The flow rate was set at 1.0 ml/min and the injection volume was 10 μl.The time-of-flight mass spectrometer was equipped with an EIS ion source.The scanning mass range was between m/z 100-1 000.Results The traditional Chinese medicine of Oldenlandia diffusa and its injection preparation were on-line separated and characterized by HPLC-TOFMS,and 11 chemical compounds were identified in Oldenlandia diffusa,6 compounds in market injection preparation,and 2 compounds in the injection prepared by ourselves.Conclusion Chromatographic demonstration of chemical compounds in Oldenlandia diffusa in one run provides a foundation for the further studying the metabolism and mechanism of Oldenlandia diffusa and its injection preparations.