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Abstract Piper sarmentosum is a herbaceous shrub with numerous pharmacological benefits. However, the presence of two toxic phenylpropanoids (α- and β-asarone) limits the medicinal usage of the plant. In this study, the extraction of three asarone isomers, namely α-, β-, and -asarone was optimised using supercritical carbon dioxide extraction (SC-CO2) combined with Box-Behnken experimental design. Comparison of asarone contents in different conventional solvent extracts of P. sarmentosum leaves prior to and after SC-CO2 extraction was performed. The SC-CO2 method successfully maximised the extraction of α-, β-, and ɣ-asarone at P = 81.16 bar, T = 50.11°C, and t = 80.90 min, yielding 13.91% α-asarone, 3.43% β-asarone, and 14.95% ɣ-asarone. The SC-CO2 residue of the leaves re-extracted with conventional solvents showed a significant decrease of asarone ranging from 45% to 100% (p<0.001) compared to their counterparts without SC-CO2 treatment. α-, β-, and ɣ-asarone were completely removed in the ethanol extract of the residue. These findings suggested that the optimised SC-CO2 extraction parameters may serve as a quick treatment step for the selective removal of asarone from P. sarmentosum to develop safer extracts for the food and nutraceutical industries applications.
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Abstract This study aims to find the best conditions for the extraction of Zingiber officinale essential oil using the supercritical fluid extraction (SFE), steam distillation (SD) and hydrodistillation (HD) techniques, regarding the maximum oil yield. For the HD technique is evaluated the best ratio between plant mass and water volume and for SFE and SD the pressure condition was investigated. Principal Component Analysis (PCA) was used to evaluate the similarity between the composition of the essential oil in different pressures and extraction methods. The experimental extraction curve was plotted and three different mathematical models were used to fit the data for SD and SFE methods, obtaining the relevant mass transfer parameters. The essential oil compounds were identified by gas chromatography coupled with mass spectrometry (GC-MS), being α-zingiberene the main component with different contents (from 11.9 to 28.9%). The best condition for the SFE was 100 bar, 40 °C (0.0508 goil/gplant) with 19.34% of α-zingiberene; for the SD, 3 bar (133 °C) (0.00616 goil/gplant) with 28.9% of α-zingiberene; and HD, the volume of 750 mL (0.006988 goil/gplant) with 15.70% of α-zingiberene, all measured on a dry basis.
Subject(s)
Oils, Volatile/isolation & purification , Zingiber officinale/chemistry , Distillation , Chromatography, Supercritical Fluid , Gas Chromatography-Mass Spectrometry , Models, TheoreticalABSTRACT
OBJECTIVE：To establish and optimize a extraction method of Fructus Gleditsiae Abnormallis ，and to analyze and identify chemical components of the extract simultaneously. METHODS ：Fructus Gleditsiae Abnormallis was extracted with CO 2 supercritical fluid extraction （SFE）method. Based on single factor tests ，using extraction yield as index ，extraction temperature ， extraction pressure and extraction time as investigation factors ，SFE technology was optimized with orthogonal test ，and validation test was performed. Chemical components in the extract were identified by GC-MS. Relative percentage of each component was calculated with area normalization method. RESULTS ：The optimal SFE extraction technology of Fructus Gleditsiae Abnormallis was extraction temperature of 60 ℃，extraction pressure of 300 MPa and pression time of 15 min. Average extraction of 3 times of validation tests was 1.73％（RSD＝1.78％，n＝3）. The 48 components in the extracts of Fructus Gleditsiae Abnormallis were identified，which accounted for 98.31％ of the total amount of the extracts. The extracts of Fructus Gleditisae Abnormalis mainly included organic acids ，accounting for 36.99％，followed by alkaloids ，accounting for 12.59％ in total. Main components were palmitic acid （16.62％），oleic acid （14.12％），N-aminotetrahydropyrrole（9.79％），2，6-dimethyloctane-1，7-dien-3-ol（5.95％）， tetrahydropyran（3.83％），vanillin（3.39％），etc. CONCLUSIONS ：SFE method of Fructus Gleditisae Abnormalis is established successfully，and the extract is mainly organic acids.
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Objective To clarify the influence of the extraction process on its active ingredients by comparing the volatile oils of Rhizoma Chuanxiong obtained under different processes. Methods The volatile oil of Rhizoma Chuanxiong was extracted by supercritical CO2 extraction (SFE) and steam distillation. The main chemical components and relative contents were identified by gas chromatography-mass spectrometry (GC-MS). Results A total of 18 common components were identified in the volatile oil samples of Chuanxiong from the two methods. In steam distillation samples, main components included phthalides (61%), monoterpenoids (25%) and sesquiterpenes (10%). In SFE samples, phthalides (97%) were major components, followed by monoterpenoids (1%),sesquiterpenes (0.4%) and other minor components. Conclusion The steam distillation retains highly volatile components in Rhizoma chuanxiong such as monoterpenoids and sesquiterpenes. For SFE approach, the phthalides were extracted more efficiently compared with other components. The effect of the extraction process on the active ingredients should be fully considered in obtained products of Rhizoma chuanxiong since the difference in constituents may result in varied effects.
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Flavonoids are widely found in medicinal plants, which have important medical properties. Flavonoids were proved to have many pharmacological activities, such as anti-oxidation, antitumor, antimutation, anti-inflammatory, antibacterial and anti-aging. The extraction of flavonoids is the crucial link in their clinical applications. In recent years, many emerging Chinese medicine extraction methods have also been widely used in the extraction of flavonoids. This paper reviews the current application of new methods for flavonoid extraction, in order to provide references for the extraction, development and utilization of flavonoids. These new extraction methods include supercritical fluid extraction (SFE), ultrasonic assisted extraction (UAE), microwave assisted extraction (MAE), pressurized liquid extraction (PLE), pulsed electric field (PEF) assisted extraction, enzyme assisted extraction (EAE), green solvent extraction, steam explosion assisted extraction, dynamic high pressure microfluidization (DHPM) assisted extraction, etc.
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Objective To establish a rapid and effective supercritical fluid extraction (SFE) and rapid resolution liquid chromatography method coupled with diode-array detector (RRLC-DAD) to quantify the chromones in a species. Methods The effects of four parameters including ethanol concentration (50%–90%), pressure (25–45 MPa), temperature (40–60 oC), and time (30–90 min) on the chromones yields, namely prim-O-glucosylcimifugin, cimifugin, 5-O-methylvisammioside, and sec-O-gluco-sylhamaudol, were investigated using SFE system with orthogonal array design (OAD). Furthermore, the extracts were analyzed using rapid resolution liquid chromatography coupled with diode-array detector (RRLC-DAD) system to confirm the results. Results Under the optimized conditions, i. e., 35 MPa of pressure, 60 °C of temperature, 70% ethanol, and 60 min of time, the yields of prim-O-glucosylcimifugin, cimifugin, 5-O-methylvisammioside, sec-O-glucosylhamaudol, and total chromones were 3.514, 0.132, 6.242, 0.342, and 10.231 mg/g, respectively. In comparison with ultrasonic assisted extraction (UAE), SFE was able to yield a 20.7% increase in the total chromones from Saposhnikoviae Radix. Conclusion SFE is an alternative and promising method to extract chromones from this species, and the established RRLC-DAD method could serve as a rapid and effective method for the identification of chromones from Saposhnikoviae Radix.
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OBJECTIVE: To isolate the chemical constituents and screen out the activity index of Dendrobium officinale, and establish a reliable method for isolation and determination. METHODS: A supercritical fluid extraction (SFE) combined with simulated moving bed (SMB) chromatography method was established for the chemical composition extraction of D. officinale. RESULTS: Under the optimal SFE condition 46 g crude extract and 30 mg naringenin could be obtained from 1 kg of dried D. officinale. Naringenin and peak X could be fully extracted and isolation by the optimal supercritical fluid simulated moving bed (SF-SMB) operation. The content of naringenin increased from 1 199 mg to 2 400 mg in 1 kg of crude extract and the percentage content of peak X increased from 4.99% to 20.44%. The pure peak X was isolation by SMB and identified as 2, 6 -dimethoxy-4-(2-propen-1-yl)-phenol using GC-MS, 1H-NMR, and IR. CONCLUSION: The technology of SFE combined with SMB is stable and excellent for extraction and isolation of the active ingredients from D. officinale, and it provides a new idea for the industrial extraction.
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This study was aimed to optimize the extraction (CO2 supercritical extraction) process and purification (ethanol washing and decontaminating) process of total fatty acid in Brassica campestris pollen. With the extraction yield of total fatty acid as index, CO2 supercritical extraction of total fatty acid in B. campestris polle was optimized by central composite design-response surface methodology. Ethanol washing and decontaminating was done for the extract through orthogonal design with content of total fatty acid (linolenic acid amide, linolenic acid glyceride, linolenic acid and palmitic acid) as the indexes. The optimum parameters of CO2 supercritical extraction technology were as follows: extraction pressure of 35 MPa, extraction temperature of 60 ℃and extraction time of 3 h. When extract of supercritical fluid was purified by 50 times of 80% ethanol for 1.5 h, the content of total fatty acid can reach 60%. In addition, this process was stable and steady, provided reliable basis for production.
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To optimize the solvent system of high-speed counter-current chromatography (HSCCC) for diterpenoidtanshinone separation and define it's antitumor activity in vitro. Total diterpenoidtanshinone was made by CO2 supercritical fluid extraction (SFE), UPLC was applied to determining the peak area of tanshinone IIA and cryptotanshinone in different solvents up or under phase, and the partition coefficient K values of them were calculated. CKK-8 was used to observe the inhibitory effects of diterpenoidtanshinone on human liver cancer (QGY-7703), lung cancer (PC9, A549), gastric cancer (MKN-45, HGC-27), colon cancer (HCT116), myeloma (U266, RPMI8226), and breast cancer (MCF-7). The best solvent system for HSCCC was petroleum ether-ethyl acetate-methanol-aqua (12∶8∶ 13∶7). The yield of diterpenoidtanshinone was 8.65%. Diterpenoidtanshinone has good effect of antitumor in vitro especially on human PC9 cell. The selected solvent system is suitable for diterpenoidtanshinone separation by HSCCC, and the established HSCCC method is reliable and easy for operating. Diterpenoidtanshinone has good antitumor effect in vitro.
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Plants differ in metabolism during their life cycle. In species used as phytotherapics, these changes determine the quality and effectiveness of the product. The aim of this study to evaluate the differences of chemical extracts obtained with supercritical CO2 from young and adult leaves of Zanthoxylum tingoassuiba St.-Hil., Rutaceae, a species used in the folk medicine in Brazil. The chemical composition of the extracts was elucidated by spectroscopic analysis and comparison with literature data. The results showed difference in the composition of the leaves from Z. tingoassuiba and allowed the determination of parameters for the extraction of α-bisabolol and furanocoumarins in this vegetal matrix.
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OBJECTIVE:To facilitate the application of Asarum forbesii Maxim. in the fields of medicine and fine chemicals. METHODS:The essential oil was extracted from Asarum forbesii Maxim. by supercritical fluid extraction (SFE), and the chemical constituents of essential oil were analyzed by GC-MS. RESULTS:22 constituents were identified, dominating the list were 1,2-Benzenedicarboxylic acid (mass fraction:20.47%), Eugenol methyl ether (15.37%),(Z)-9-Oleic acid(13.21%), 9,12-Octadecadienoic acid (Z, Z) (12.53%),Elemicin (11.05%), n-Hexadecanoic acid (7.59), Octadecanoic acid (4.36%). CONCLUSION:The method used on essential oil extraction serves as references for the further exploitation and utilization of Asarum forbesii Maxim..
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OBJECTIVE: To analyze the chemical compositions of the essential oils of Eupatorium fortunei extracted by CO2-supercritical-fluid-extraction(SFE-CO2) vs.steam distillation extraction(SD).METHODS: The essential oils of the E.fortunei were extracted by SD vs.SFE-CO2.The chemical components were separated and analyzed by GC-MS.RESULTS: 31 compounds were identified in the essential oils of E.fortunei extracted by SFE-CO2,accounting for 75.97% of the peak area of the total ion-current chromatogram,with 2-propenoic acid-3-(4-methoxyphenyl)-ethyl ester showing the highest proportion(40.50%).21 compounds were identified in the essential oils of E.fortunei extracted by SD,accounting for 51.70% of the peak area of the total ion-current chromatogram,with caryophyllene showing the highest proportion(10.35%).13 components were mutual in both extraction methods.The contents of the components varied greatly.CONCLUSION: SFE-CO2 is more stable and reliable and reproducible than SD,and it is more applicable for the extraction of the essential oils from Chinese herbal medicine.
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OBJECTIVE:To extract volatile rose oil by the supercritical fluid extraction technology.METHODS:The optimum extraction technology condition was investigated by orthogonal experiment with extraction rate as the evaluation in?dex,and with the pressure,temperature of extraction and the flow of CO 2 as investigation factors(3levels of each were cho?sen).RESULTS:The optimum technology condition was the following:the extraction pressure was25MPa,the temperature was50℃and the flux of CO 2 was600L/h.CONCLUSION:The established method has the following merits:high extraction rate,fast speed,simple technics,pollution-free,pure extraction etc.
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OBJECTIVE: To study the optimum supercritical- fluid extraction technique for Xiangjiang Granula essential oil. METHODS: The orthogonal test was adopted to optimize the extraction process using the content of Ligustilide and the yield rate of essential oil as indicators, and 95% ethanol as co- solvents. The content of Ligustilide was determined by HPLC, using Phenomenex Luna C18( 250nm? 4. 6nm, 5? m) as column and methanol- 0. 5% glacial acetic acid( 30∶ 70) as mobile phase, with the detection wavelength set at 280 nm. RESULTS: The optimal extraction conditions were: temperature at 50℃ , pressure at 45MPa, extraction time for 3h, and 95% ethanol as co- solvents. The Ligustilide had a good linearty relationship between 5. 1～ 25. 5? g? mL- 1( r=0. 999 8) . CONCLUSIONS: This technique is easy, convenient and workable, and can provide theoretical support for production.
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To compare the chemical components and their contents of essential oil extracted from Radix Angelicae Sinensis by the methods of supercritical CO 2 fluid extraction (SFE-CO 2), normal pressure steam distillation (NPSD) and vacuum steam distillation (VSD). The combination of gas chromatography and mass spectrometry was applied to analyze the chemical components and their contents of essential oil extracted from Radix Angelicae Sinensis.The chemical components and their contents of essential oil extracted by the above three methods were different.[Conclusion]SFE-CO 2 is superior to VSD and NPSD in raising yield and shortening extractive time. It is a good method for the extraction of essential oils from Radix Angelicae Sinensis.
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Object To study the conditions for the extraction of active ingredients in Ligusticum chuanxiong Hort by supercritical fluid extraction (SFE) Methods Conditions for the extraction were studied by orthogonal experimental design as guided by the content of ferulic acid presented in the extract Results The optimum conditions for the yield of ferulic acid were thus established Conclusion The best SFE conditions were: temperature of the extraction pot was 70 ℃ under the pressure of 35 MPa, CO 2 as the modifier with the flow rate of 25 kg/h, the time for extraction was 2 5 h
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Objective To investigate the effect of Pericarpium Zanthoxyli (HJ) on guinea pigs trachea in vitro and its therapeutic mechanism. Methods The actions of HJ on the contraction of normal trachea and on the spasm of spasmodic tracheas caused by acetylcholine (Ach) and histamine phosphate (HIS), as well as the actions on intracellular Ca2+ - dependent contraction and extracellular Ca2+ - dependent contraction induced by HIS were observed. Results HJ could inhibit the guinea pigs trachea contraction , antagonize the contraction of trachea spasm induced by Ach and HIS , restrain the extracellular Ca2+ - dependent contraction induced by HIS in a dose- dependent manner. Conclusion HJ has an antiasthma effect.
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Objective To optimize the experimental condition for CO 2 supercritical fluid extraction(SFE)of volatile oil from Marchantia convoluta andto analyse the extract.Methods Orthogonaltestwas applied.SFEtechnology was usedto optimize the extractionconditionfor volatile oilfrom Marchantia convoluta and the solventextractionwas useda s the control.The extract was analyzed by GC-MS and HPLC.Results The optimal extraction conditions f or the volatile oil were:pressure at15MPa,heatingtemperatureat50℃,addingt hemodifier ofalcohol30mLtoextractfor2h,flowingratebeing10L /hand theabsorbefa-cient solution being alcohol .Twent y -three peaks were isolated and 19components were identified,accounting 82.61%.Conclusion SFEmethodhas theadvantages of shorterextractiontimeandhighextractionefficiencyas comparedwiththet radi-tionalsolventextraction.
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AIM: To identify and determine compounds in supercritical CO_2 extraction from Hypericum perforatum L. METHODS: The contents of flavones and hyperforin were determined by reverse phase HPLC.The condition in supercritical fluid extraction(SFE) was: extraction temperature at 40 ?C,extraction pressure at 20 MPa,separation temperature at 45 ?C,separation presure at 8 MPa,extraction time 1 h. RESULTS: There was no flavones and the content of hyperforin was 180.6 mg/g in the sample of SFE using neat CO_2.The flavones and hyperforin were found in SFE extract using ethanol as modifier and the contents of rutin,quercetin,hyperoside,hyperforin were 1.10 mg/g、1.84 mg/g、1.33 mg/g、26.19 mg/g,respectively. CONCLUSION: The concentration of hyperforin by SFE with neat CO_2 is significantly higher than that with modified supercritical CO_2 extraction. The method of SFE with neat CO_2 can be used to prepare extracts with high concentration hyperforin.
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AIM: To isolate,identify and screen active compounds of simplitied formula of Danggui Shaoyao Power(poria,Rhizoma Atracty-lodis Macrocephalae,and Radix Angeliae Sinensis). METHODS: Compounds in the fraction of CO_2 supercritical fluid extraction(SFE-CO_2) were isolated by silica gel chromatography and detected the protective effect on KCl-induced PC12 cell damage. RESULTS: Twelve compounds were obtained,and nine of them were identified as atractylenolide Ⅰ,Ⅱ,Ⅲ,biatractylenolide,levistolid A,pachymic acid,ferulic acid,?-sitosterol and ?-daucosterol,of which only atractylenolide Ⅲ can improve the cell viability significantly. CONCLUSION: Atractylenolide Ⅲ may be one of the active compounds of FBD in curing vascular dementia.