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OBJECTIVE To opti mize the supercritical CO 2 extraction technology of volatile oil from Blumea balsamifera ，and compare the components of the volatile oil from B. balsamifera obtained by supercritical CO 2 extraction and steam distillation. METHODS The volatile oil of B. balsamifera was extracted by supercritical CO 2 extraction. Using extraction rate of volatile oil as index，extraction temperature ，extraction pressure and extraction time as factors ，based on single-factor experiment ，orthogonal experiment was used to optimize the supercritical CO 2 extraction technology. Gas chromatography-mass spectrometry was used to identify the components of volatile oil from B. balsamifera . Peak area normalization was used to calculate the relative contents of each component. Taking the volatile oil obtained by steam distillation as a reference ，the extraction rates ，components and contents of volatile oil by the two methods were compared. RESULTS The optimal supercritical CO 2 extraction technology of volatile oil from B. balsamifera included extraction pressure of 30 MPa，extraction temperature of 50 ℃ and extracting for 50 min. After 3 times of validation tests ，average extraction rate of volatile oil was 4.64％（RSD＝0.54％，n＝3）. Thirty-nine components such as tritriacontane，stigmasterol，squalene were identified in the volatile oil of B. balsamifera obtained by supercritical CO 2 extraction； and 51 components such as triacontane ，ledol，humulene epoxide Ⅰ were identified by steam distillation. The extraction rate of volatile oil from B. balsamifera obtained by 2 methods were 4.64％ and 0.99％. A total of 26 common components were obtained ， such as xanthoxylin ，L-borneol，β-caryophyllene. Except for xanthoxyline （34.829％ by supercritical CO 2 extraction，30.676％ by steam distillation method ）and phytol （2.401％ by supercritical CO 2 extraction，1.273％ by steam distillation ），the relative contents of the components of volatile oil obtained by supercritical CO 2 extraction were lower than those of steam distillation. CONCLUSIONS The optimal supercritical CO 2 extraction technology is stable and feasible ；the components and contents of volatile oil obtained by two methods varies greatly ，and main compounds are aldehydes and ketones ，alkenes，alcohols and other components.
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Objective: To optimize the supercritical CO2 extraction process of active ingredients from Magnoliae Officinalis Cortex (MOC) and explore the antioxidant activity of the extracts. Methods: The content of magnolol and honokiol of the supercritical CO2 extracts of MOC was determined by HPLC, and the extraction process was optimized by orthogonal experiment. The antioxidant activities of the extracts were determined by MTT. Results: The optimum extraction pressure of magnolol was 25 MPa, the extraction temperature was 55 ℃, the amount of CO2 was 30 kg, and the optimum extraction parameters mentioned above of honokiol were 15 MPa, 50 ℃, and 25 kg, respectively. Conclusion: Under the optimum extraction conditions, magnolol and honokiol have high extraction efficiency, good repeatability, stability and feasibility, and the extract have good antioxidant activity.
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To define the extraction process, main components and antioxidative and antimicrobial activities of volatile oil from fenugreek(Trigonella foenum-graecum) leaves and its active substance basis. Response surface methodology was used for optimum supercritical CO_2 extraction conditions of essential oil from fenugreek leaves. The main components of volatile oil were analyzed by GC-MS, its antioxidant activity was evaluated by measuring the scavenging ability of 1,1-diphenyl-2-picrylhydrazyl(DPPH) and 2, 2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid, ABTS) free radical, and the antimicrobial effect of volatile oil was evaluated by K-B paper AGAR diffusion method. The results showed that the optimal extraction temperature was 50 ℃, the extraction time was 89 min, and the extraction pressure was 35 MPa. Under the conditions, the optimum extracting yield of volatile oil was 1.72%,which was about 1.5 times higher than that of the conventional steam distillation. A total of 52 compounds were found based on reference substance retention time and GC-MS fragmentation information or the existing literatures, and the major compounds were oleic acid(9.65%), carveol(9.41%), n-hexadecanoic acid(9.1%), linoleic acid(6.95%), methyl linolenate(5.4%), petroselinic acid(5.3%), testosterone(3.4%), sotolon(1.75%). The volatile oil of fenugreek showed moderate antioxidant activities in DPPH assay(IC_(50) value of 0.473 mg·mL~(-1)) and ABTS test(IC_(50) value of 0.107 mg·mL~(-1)). The oil had a stronger antimicrobial activity in vitro. MIC of the volatile oil ranged from 0.375 to 1.5 mg·mL~(-1). The results showed that the optimized volatile oil extraction process was stable, and the extraction yield was high. Fenugreek leaves contained a variety of volatile components, with obvious antioxidant and antibacterial activities. This study provides a certain theoretical basis for the comprehensive development and utilization of fenugreek.
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Antioxidants , Distillation , Oils, Volatile , Plant Leaves , TrigonellaABSTRACT
Objective:To analyze and compare the volatile oil components of pine needle of Pinus yunnanensis from different habitats. Method:The volatile oils of pine needle of P. yunnanensis from 12 different habitats were extracted by supercritical CO2 extraction （SFE-CO2），the components were analyzed by gas chromatography-mass spectrometry （GC-MS），and relative percentage of each component was determined by peak area normalization method，and SPSS 20.0 software was used for principal component analysis. Result:The 137 compounds were isolated from the volatile oil of pine needle of P. yunnanensis from 12 different producing areas，with 1 sample identified 57 species，2 samples identified 57 species，3 samples identified 54 species，4 samples identified 48 species，5 samples to identify 58 species，6 samples identified 60 species，7 samples identified 53 species，8 samples identified 55 species，9 samples identified 56 species，10 samples to identify 58 species，11 samples identified 54 species and 12 samples to identify 50 species，composed of hydrocarbon，acid，alcohol，ester，aldehyde，ketone，phenol，ether 8 compounds，including 11 common composition including alpha pinene，beta pinene，beta caryophyllene，7C，10C，16C-hexadecatrienoic acid and palmitic acid methyl ester，palmitic acid，phthalic acid dibutyl do acid，alcohol，stearic acid，mountain，wood tar acid. Conclusion:In this study，supercritical CO2 extraction （SFE-CO2） was used to extract the volatile oil of pine needle of P. yunnanensis from different habitats. It was found that the volatile oil of pine needle of P. yunnanensis was mainly composed of hydrocarbons，acids，esters and alcohols. And the content and species of volatile oil of pine needle of P. yunnanensis from different producing areas differ greatly which lay a foundation for the further development and utilization of pine needle of P. yunnanensis resources.
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Objective: To study the chemical constituents of Rabdosia rubescens. Methods: The chemical constituent of R. rubescens was separated and purified by using of various column chromatographic technologies (silica gel, MCI, and ODS column chromatography) as well as HPLC. Structures were elucidated by physicochemical characteristics and spectral data. Results: One new flavanoiel compound was isolated from supercritical fluid extract of R. rubescens, and it was elucidated as 3’-hydroxy-2’,4’- dimethoxy-flav-3-ene (1). Conclusion: Compound 1 is a new flavanoid, named as rubescenane A.
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OBJECTIVE： To study the chemical constituents of supercritical CO2 extract from Xinjiang Daucus carota seed（called “D. carota seed extract” for short）， and to preliminarily evaluate its antimicrobial and antioxident activity， so as to provide reference for the development and quality control of related products of the plant. METHODS： The non-polar volatile part of Xinjiang D. carota seed was extracted by supercritical CO2 extraction method. The chemical constituents of the extract were identified and quantified by GC-MS and standard spectral labrary. The relative percentage content of each component was calculated by peak area normalization method. The antibacterial activity of D. carota seed extract against Staphylococcus aureus，Escherichia coli and Candida albicans were investigated by trace broth dilution method and AGAR medium plate method. Its antioxidant activity was investigated by TLC-bioautography method. RESULTS： Twenty chemical constituents were identified from D. carota seed extract （the total relative percentage content was 98.76％）， mainly including β-bisabolene， α-asarone， α-pinene， β-caryophyllene， aspidinol， etc. D. carota seed extract has certain antimicrobial activity on S. aureus， E. coli and C. albicans. The minimum inhibitory concentrations were 0.039， 0.833， 0.625 mg/mL， and minimum bactericidal concentrations were 0.078， 1.667， 1.250 mg/mL， respectively. The extract has a certain scavenging ability to DPPH radical. CONCLUSIONS： D. carota seed extract obtained by supercritical CO2 extraction contains monoterpenes and sesquiterpenes， and possesses certain antibacterial and antioxidant activity.
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Objective To optimize the extraction conditions of Schisandra sphenanthera(SS)seed oil by supercritical CO2ex?traction and identify its components by GC-MS.Methods SS seed oil was used as tested material,response surface methodology was used to optimize the process of supercritical CO2extraction,and GS-MS method was used to analyse SS seed oil composition.Results A model of an equation was established,which could be used to optimize the process parameters of supercritical CO2extraction of SS seed oil. The optimum extraction parameters were as follows:the extraction pressure was 33 MPa,the extraction temperature was 53℃,the extraction time was 90 min,the CO2flow rate was 21.40 ml/min.In this condition,the extraction rate of SS seed oil was 7.97%.The SS seed oil was analyzed by GC-MS,and 23 compounds were identified.In these compounds,(1α,4a.β,8a.α)-1,2,3, 4,4a,5,6,8a-octahydro-7-methyl-4-methylene-1-(1-methylethenyl)-naphthalene,(-)-1,7-dimethyl-7-(4-methyl-3-pentenyl)-tricyc?lo[2.2.1.0(2,6)]heptane and(R)-2,4a,5,6,7,8-octahydro-3,5,5,9-tetramethyl-1H-(σ-phenyl)cycloheptene had the content of more than 10% and the contents were 27.78%,14.77% and 13.12% respectively.Conclusion This process has high extraction rate, fast speed and simple operation,and can be used for the extraction of SS seed oil.
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Objective: To optimize the extraction process of volatile oil from Fructus Litseae.Methods: Supercritical CO2 extraction (SFE-CO2) was used to extract volatile oil from Fructus Litseae, and the extraction process was optimized by a central composite design-response surface method (CCD-RSM).The kind and content of volatile oil extracted by SFE-CO2 and steam distillation (SD) were detected by gas chromatography-mass spectrometer (GC-MS).Results: The highest extraction rate of the total effective constituents was 66.26% when the optimum conditions were as follows: the extraction temperature was 44 ℃, the extraction pressure was 26 MPa, entrainer ethanol was 11 ml and the extraction time was 40 min.It was revealed that neral, geranial and limonene were the major constituents.Compared with that of SD, the kind of volatile oil extracted by SFE-CO2 was fewer while the content of citral extracted by SFE-CO2 was higher.Conclusion: The extraction process optimized by CCD-RSM provides reference for the extraction method and quality control of volatile oil from Fructus Litseae.
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Objective To optimize the supercritical carbon dioxide(SC-CO2)extraction of lipids from tempeh(TE-C)and further improve the lipid classes ratio. Methods The experimental parameters of SC-CO2 extraction including extraction temperature, pressure,and moisture content of tempeh were optimized using a Box-Behnken design combined with response surface methodology (RSM),according to the weighted extraction ratio of TE-C and lipid classes after the experimental results of single factors. Detailed chemical compositions of TE-C obtained by optimum conditions of SC-CO2 extraction were analyzed by high performance liquid chroma?tography with an evaporative light-scattering detector(HPLC-ELSD)and high performance liquid chromatography-atmospheric pres?sure chemical ionization mass spectrometry(HPLC-APCI-MS). Results TE-C was composed of three lipid classes:fatty acids(Ⅰ), diacylglycerols(Ⅱ)and triacylglycerols(Ⅲ). The optimum SC-CO2 extraction conditions of TE-C were 50℃extraction temperature, 25 MPa pressure,1.99%moisture content of tempeh and 1.5 hour extraction time. Conclusion The optimum value of RSM for SC-CO2 extraction was(5.97±0.15)g/100 g.
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AIM To optimize the supercritical CO2 extraction of sauchinone and to evaluate the in vitro antitumor activity of Saururi Herba supercritical extract.METHODS With extraction pressure,extraction temperature,extraction time,entrainer (ethanol) concentration and entrainer amount as influencing factors,together with extraction rate of sauchinone as an evaluation index,orthogonal test was used for optimizing the extraction.Then MTT was applied to determining the extract's inhibitory effect on human multidrug-resistant hepatocellular carcinoma cell line (7721/Adm).RESULTS The optimal conditions were determined to be 30 MPa for extraction pressure,50 ℃ for extraction temperature,2 h for extraction time,95％ for ethanol concentration,and one time for ethanol amount,the average extraction rate of sauchinone was 0.173％.The obtained extract significantly inhibited the proliferation of 7721/Adm cells (IC50 =50.08 μg/mL),demonstrating a stronger activity than that of ethanol extract (ICs0 =150.59 μg/mL).CONCLUSION This stable and feasible method is appropriate for sauchinone extraction,and the supercritical CO2 extract from Saururi Herba shows a strong in vitro antitumor activity.
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OBJECTIVE:To extract and identify the volatile components of the roots of Polyalthia nemoralis,and to evaluate its biological activity in vitro. METHODS:Supercritical CO2 extraction (SFE-CO2) was performed to extract volatile compounds from the roots of P. nemoralis,and the volatile components were separated and determined by GC-MS. Human hepatic cancer Huh-7 cells were cultured with 0(blank control),5,10,20,30,40 and 50 μg(medicinal material)/ml extract for 24 h,and then MTT assay was used to detect the inhibitory effect of the extracts on cells. Relative cell viability and IC50 were calculated. The an-ti-bacterial activities of extract to Staphylococcus aureus,Methicillin-resistant Staphylococcus aureus,Enterococcus faecalis and oth-er strain were determined by Kirby-bauer method and broth dilution method. RESULTS:Forty compounds were identified from the SFE-CO2 extracts from the roots of P. nemoralis. The main constituents were(Z,Z,Z)-9,12,15-octa-decatrien-1-ol,glycerin,cinna-maldehyde,n-hexadecanoic acid and eugenol. Compared with blank control group,SFE-CO2 extracts from the roots of P. nemoralis 5 μg(medicinal material)/ml and above showed significant inhibitory effect on cell growth(P<0.05),and the inhibitory effect was strengthened as the concentration of extracts increased,IC50 values was 5.2 μg(medicinal material)/ml. However,the supercritical extract didn't showed antibacterial activity against three microorganisms in 2 kinds of antibacterial tests. CONCLUSIONS:SFE-CO2 and GC-MS method can effectively extract and identify volatile components of the roots of P. nemoralis,and supercritical extracts can inhibit the viability of cells but have no antibacterial activity.
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OBJECTIVE:To optimize the technology of supercritical CO2 extraction from Zingiberis rhizoma. METHODS:With the comprehensive score of the contents of 6-ginger phenol,8-ginger phenol and 10-ginger phenol and the extraction rate of the oil from Z. rhizoma as the index,uniform design method was adopted to investigate the effects of extraction pressure,extrac-tion temperature and extraction duration on the extraction result;verification tests were conducted. RESULTS:The optimal condi-tions were as follows as the extraction pressure of 25 MPa,extraction temperature of 30 ℃ and extraction duration of 2 h. In the verification tests,the average extraction rate of the oil from Z. rhizoma was 3.2%(n=3),and the comprehensive score was 1.874 2 (RSD=0.65%,n=3),with the relative deviation of 0.6% between the measured value and the predicted value. CONCLUSIONS:The optimal extraction technology is stable and feasible,with the advantages of low temperature,short duration.
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Objective:To research the effects of entrainer on extracting astragaloside from astragalus by supercritical CO2 . Meth-ods:The optimum extraction technology conditions were investigated by an L9 (34 ) orthogonal experiment with the extraction rate of as-tragaloside as the evaluation index and the addition way, variety, amount and flow rate of the entrainers as the investigation factors. The content of astragaloside was determined by HPLC. Results:The addition way of entrainer was the presoak treatment combined with the dynamic extraction mode, and the entrainer was 95 % alcohol with 300 ml of infusing volume and 10 ml·min-1 flowing volume. The best factors of supercritical fluid extraction were as follows:the extraction pressure was 35 MPa, the extraction temperature was 45℃, the outlet temperature was 55℃, the extracts were collected with 95% alcohol, and dynamic extraction time was 2 h. Under the above process conditions, the extraction rate of astragaloside was 0. 040 7%. Conclusion:The extraction of astragaloside from astragalus by supercritical CO2 extraction with the optimized process is significantly improved.
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OBJECTIVE: To optimize the extraction and inclusion processes of ginger oleoresin from Zingiberis Rhizoma Recens. METHODS: Supercritical carbon dioxide extraction was selected to extract ginger oleoresin from Zingiberis Rhizoma Recens. The extraction condition was optimized by orthogonal experiment. The inclusion method, the ratio of ginger oleoresin to β-cyclodextrin and inclusion time were studied as factors of inclusion process. RESULTS: The optimized extraction technology was as follows: extraction temperature was 50℃, extraction pressure was 25 MPa, separation pressure was 9 MPa and extraction time was 90 min. The optimal inclusion method was triturating inclusion, with the ratio of ginger oleoresin to β-cyclodextrin of 1:8 and inclusion time of 60 min. CONCLUSION: The optimized technology of extraction and inclusion is stable and feasible, and can be used for the extraction and inclusion of ginger oleoresin.
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Extraction process plays an important role in Chinese herbal medicine applications. Traditional extraction method has some disadvantages, such as long processing time, high solvent consumption and low efficiency. Thus, some new technologies and methods have been introduced in this paper, including ultrasonic extraction, microwave extraction, supercritical fluid extraction. On the basis of advantages and disadvantages of traditional Soxhlet extrac-tion, this paper mainly described the principles, characteristics, influencing parameters and applications.
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Objective:To compare the steam distillation( SD) and supercritical CO2 ( SFE-CO2 ) method in the extraction of vola-tile constituents from such 3 traditional Chinese drugs as cnidium monnieri, radix sileris and atractylodes lancea in compound Kuhuang prescription. Methods:Essential oil was extracted from the 3 traditional Chinese drugs by SD and SFE-CO2 method, respectively. The components were identified by GC-MS, and their relative contents were calculated with peak area normalization method. Results:To-tally 36 components were isolated and identified using SD extraction and 31 components were identified using SFE-CO2 extraction, a-mong them, 22 components were the same and their relative molecular weight mainly concentrated within 200-230. Conclusion: SFE-CO2 method can extract effective components from the 3 traditional Chinese drugs in compound Kuhuang prescription with higher selec-tivity, which is the more suitable extraction method for essential oil from the prescription.
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The chemical constituents of fistular onion stalk obtained by supercritical CO2 extraction were separated and purified by silica gel and sephadex LH-20 gel column chromatography and the preparative TLC method and four flavonoids were obtained.On the basis of the spectral data,they were structurally identified as(+)-catechin,(-)-epicatechin,astragalin,and 3-O-β-D(2-O-β-D-glucopyranosyl)-glucopyranosides of kaempferol.
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Objective To optimize the extraction process by determing the volatile oil yield of steam distillation and supercritical CO2 extraction from flowers of Elaeagnus angustifolia L..Methods Orthogonal test was carried out to compare two extraction effects between steam distillation and supercritical CO2 extraction by detecting the extraction ratio from flowers of Elaeagnus angustifolia L..Results Steam distillation time on volatile oil extraction has the greatest impaction,and the best condition of supercritical CO2 extraction was extraction pressure of 20 MPa,extraction temperature of 40 ℃,and flux of CO2 is 10 L/h.Conclusion Compared with steam distillation,supercritical CO2 extraction spends less time,has higher efficiency and less harm to the materiel after extracting.It adapts to batch process and is convenient for subsequent extraction technology.
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OBJECTIVE:To analyze the chemical components extracted with supercritical CO2(SFE-CO2)from Eucalyptus tereticornis.METHODS: Volatile oil was extracted from E.tereticornis with SFE-CO2.The chemical component analyzed by GC-MS and its proportion was determined by normalization method.RESULTS: 28 compounds which account for 88.13% of the total peak area were separated and identified.The main components of volatile oil were eucalyptol (33.99%),borneol(8.88%),?-pinene (5.39%),caryophyllene (4.51%),(+)-4-carene (4.19%).CONCLUSION:This study can be served as a scientific basis for the further exploitation and utilization of E.tereticornis.
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Object To establish a high efficient and reliable method for extraction and analysis of the diterpenoids in Pteris semipinnata L. Methods Supercritical CO 2 fluid modified with alcohol was used to extract the diterpenoids in P. semipinnata, the extracting conditions were optimized by orthogonal design method, and the modifying solvent was investigated through total ions chromatograghy normalization. A quadrupole mass spectrometer coupled with atmospheric pressure chemical ionization interface was employed as a detector for HPLC, the -1 ion was used as selective ion for the detecting of ent 11 ? hydroxy 15 oxo kaur 16 en 19 olic acid (5F) in selective ion monitoring (SIM) mode. The peak area of SIM and tolal ion chromatogram (TIC) were used for quantitative determination. As an example of its application, this method was used to determinate the content of 5F as antitumor diterpenoids in P. semipinnata. Results The optimized conditions for supercritical CO 2 fluid extraction are 25 MPa, 60 ℃, 15% methanol, flow rate 3 0 mL/min; analytical column was Diamonsil ODS (150 mm?4 6 mm, 5 ?m); the mobile phase of HPLC was CH 3CN 2 mmol/L NH 4AC (35∶65), flow rate 1 0 mL/min, injection volume 5 ?L; the standard curve showed good linearity over the range of 0 05-2 5 ?g; the limit of detection is 0 4 ng; the recovery is 97 8% (n=3). Conclusion This method is highly efficient, sensitive, and selective, which can be applied to study the antitumor drug of diterpenoids in P. semipinnata and to establish the drug standard.