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OBJECTIVE： To compare low-polarity volatile constituents in supercritical CO2 extract from the roots and stem of Ilex asprella and its effects on the proliferation of IEC-6 in vitro， and to provide reference for making full use of wild resources of I. asprella and expanding its medicinal parts. METHODS： The low-polarity volatile constituents were extracted from the root and stem of I. asprella with supercritical fluid CO2 extraction（SFE-CO2）. The chemical constituents were analyzed by GC-MS. IEC-6 cells were treated with different concentrations of supercritical CO2 extracts （0， 1， 5， 10， 20， 40， 60， 80， 100 μg/mL） from roots or stems of I. asprella. MTT assay was used to detect the relative viability， and cell proliferation curve was drawn and EC50 of each extract were calculated. RESULTS： Sixty-two and forty-six low-polarity volatile constituents were identified from supercritical CO2 extract in the roots and stem of I. asprella with GC-MS； there were 24 common constituents totally， mainly including pelargonic acid（14.18％ and 6.14％），octanoic acid（10.59％ and 4.35％），hexanoic acid（8.63％ and 10.86％），paeonol（7.79％ and 6.00％），2-methyl-3-phenyl-propanal（6.3％ and 0.58％），acetic acid（1.72％ and 33.77％） in root and stem， respectively. The results of cell culture in vitro showed that when the concentration of supercritical CO2 extract from the roots and stems of I. asprella was lower （≤60 μg/mL）， it could significantly promote the proliferation of IEC-6 cells and their EC50 were 16.35， 20.20 μg/mL， respectively； when the concentration of the extract was higher （≥80 μg/mL）， it showed cytotoxicity and inhibited the proliferation of IEC-6 cells. CONCLUSIONS： There are similar species of volatile constituents in roots and stems of I. asprella and similar in vitro bioactivity of the supercritical CO2 extracts to IEC-6 cells. The short-chain fatty acids may be the active ingredient to promote cell proliferation， while paeonol may be the cytotoxic active ingredient.
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Objective: To develop an effective and rapid method for the preparation of 23-acetate alisol B from Alisma orientalis. Methods: The SFE-CO2 extract from A. orientalis was injected into high speed counter current chromatography (HSCCC) directly, and eluted with difierent solvent systems. The crystalline purity was detected by HPLC. The structure of the target compound was identified by UV, IR, MS, and NMR. Results: The solvent system composed of n-hexane-ethylacetate- methanol-water (3∶2∶3∶2) was the best. The lower phase was used as the mobile phase and performed at a flow rate of 2 m/min, while the apparatus rotated at 800 r/min, and detected at 254 nm. The prepared alisol B 23-acetate was identified with infrared spectrometry (IR), mass spectrometry (MS), and nuclear magnetic resonance (NMR) detection, and its purity was 99.8% analyzed by HPLC. Conclusion: The established method is relatively simple, fast, and suitable for the fast isolation and separation of alisol B 23-acetate.
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Objective To investigate the extracting technology of the Northeast tussah pupa oil and analyze the composition of the oil. Methods The Northeast tussah pupa were crushed and dried at 60℃. The oil was extracted from the Northeast tussah pupa powder with super critical fluid extraction technology-CO2 (SFE-CO2) at the extracting temperature as 45 ℃,pressure as 50 MPa and operating time as 6 hours according to the results of homogeneous design. The composition of the oil was detected by gas chromatography (GC).Results The extracting rate of the oil from the Northeast tussah pupa powder was 17.93% (w/w)and the percent of compositions of the oil were C15:0 fatty acid 37.03%,hexadecanoic acid 5.63%,C17:0 fatty acid 32.81%,octadecanoic acid 1.79%,leic acid 3.75%,octadecadienoic acid 11.98% and α-1inoleic acid 7.00%. Conclusion The technology of SFE-CO2 can be used in extraction of Northeast tussah pupa with High extraction efficiency.
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OBJECTIVE: To analyze the chemical components of volatile oil from Artemisia mongolica by GC/MS, and to investigate their antimicrobial activities. METHODS: The volatile oils were extracted from Artemisia mongolica by SFE-CO2 technique, their chemical components were analyzed by GC/MS, and their antimicrobial activities were tested by agar plate diffusion method. RESULTS: Twenty-eight compounds were separated from the crude essential oils and 23 compounds were identified. The bacteriostatic experiment results indicated that this volatile oil has strong inhibitory effects on Staphyloccocus albus, Shigella flexneri and Bacillus paratyphosus B, whereas it had no remarkable effect on Staphyloccocus aureus. CONCLUSION: The experiment provides a scientific basis for further development and utilization of Artemisia mongolica.
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OBJECTIVE:To study the supercritical CO2 fluid extraction(SFE-CO2)technology of Olibanum.METHODS:The optimum extraction technology was obtained through orthogonal test with the content of acetic octylester determined by GC and taken as index for the evaluation of the technology.RESULTS:The optimal conditions were as follows:pressure 25 MPa,temperature 60℃ and extraction time 3h.CONCLUSION:The process of SFE-CO2 is suitable for Olibanum extraction.
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Objective To study the optimum parameters of the supercritical CO2 fluid extraction of Polyrhachis vicina Roger and chemical constituents of ant oil. Methods The experiments were designed with the uniform design. Three factors are extraction pressure, temperature and time. GC-MS was applied for analyzising. Results The optimum condition was obtained:the extraction pressure is 36 MPa, the temperature of extraction is 40 ℃ and extraction time is 50min. 45 components were identified from 60 chromatographic peaks. The main chemical constituents were (Z)-9-octadecenoicacid (48.278%), hexadecanoicacid (17.574%), (Z)-9-hexadecenoi (4.912%), cholesterol (2.957%). There are some linear paraffin in ant oil. Conclusion This method can extract the ant oil from Polyrhachis vicina Roger quickly and efficiently. This experiment provide foundation for exploitation and utilization of ant resource.
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Objective To study the optimum parameters of the supercritical CO2 fluid extraction of roasted Rhizoma Atractylodis Macrocephalae and roasted Fructus aurantii immaturus,and chemical constituents of extractive matters. Methods The experiment was performed with orthogonal design. Four factors were extractive pressure,temperature,extractive time and the flow rate of CO2. GC-MS was applied for analyzing. Results The optimum condition were obtained:the extractive pressure was 33 MPa,the temperature of extraction was 40 ℃,the extractive time was 60 minutes and the flow rate of CO2 was 27 L/h. The main chemical constituents was gamma-Elemene. Conclusion The method applied to obtain the extractive matters from roasted Rhizoma Atractylodis Macrocephalae and roasted Fructus aurantii immaturus was quickly and efficiently with satisfactory results. It provides foundation for exploration.
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Objective To study the different extraction methods for the content of tanshinoneⅡA in water decocted Radix Salviae Miltiorrhiza, in order to develop comprehensive utilization of Salvia miltiorrhiza. Method Tanshinone ⅡA was extracted by supercritical carbon dioxide fluid and compared with ultrasonic extraction. Result When the extraction pressure was 35 MPa, extraction temperature was 40 ℃, extraction time was 2 h and entrainer (ethanol) was 100 %, the yields of the tanshinone ⅡA was up to 3.87 mg, while the ultrasonic extraction was 2.89 mg. Conclusion TanshinoneⅡA extracted by supercritical carbon dioxide fluid was better than ultrasonic extraction and had higher purity. The comprehensive utilization of Salvia miltiorrhiza is available.
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Objective To investigate the ex tr action technique for seperating the active components in the root of Salvia mi ltiorrhizae bunge by supercritical fluid, and to analyze the extracted product s by HPLC-MS n . Methods The extraction condition s were established as follows: 950ml?L -1ethanol as the first entrainer, t he pressure of 20.0 MPa, temperature at 45 ℃, and extracting time 1 h; then 100 mL?L -1 ethanol was selected as the second entrainer, pressur e was 30.0 MPa, temperature was 65 ℃, and extracting time was 3 h. Results Compared with traditional refluxing extraction and ultrasonic extraction, supercritical fluid extraction was better and more effect ive. Conclusion Supercritical extraction is simple, highly selec tive and efficient in extracting the active components in Salvia miltiorrhizae bunge.
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OBJECTIVE:To extract and analyze the compositions of fatty oil of Semen Pharbtidis METHODS:The fatty oil was extracted with CO2 supercritical fluid The content and compositions were determined by gravimetric analysis and GC-MS respectively RESULTS:The oil content of Semen Pharbtidis was 34 78% Among the fatty acids,linoleic acid,oleic acid and palmitic acid were dominant The unsaturated fatty acids accounted for 88 70% of the total fatty acids,and the major saturated fatty acid was palmitic acid CONCLUSION:The oil of Semen Pharbtidis is of high-quality,and the analysis results provide a scientific basis for exploitation and utilization of the oil of Semen Pharbtidis
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The volatile compounds obtained by SFE-CO2 (supercritical fluid extraction utilizing CO2) from the barks of Aniba canelilla (H. B. K.) Mez. (Lauraceae) were analyzed by HRGC-FID (high resolution gas chromatography - flame ionization detector) and HRGC-MS (high resolution gas chromatography -mass spectrometry). Phenylpropanoids and lower amounts of sesquiterpenoids, representing ca. 97 percent of the total oil, were identified. The main compound, 2-phenylnitroethane, corresponds to 71,12 percent of the total oil.
Os constituintes químicos voláteis das cascas de Aniba canelilla (H. B. K.) Mez. (Lauraceae), obtidos por SFE-CO2 (extração com fluido supercrítico utilizando CO2), foram analisados por HRGC-FID (cromatografia gasosa de alta resolução com detector de ionização de chama) e HRGC-MS cromatografia gasosa de alta resolução acoplada à espectrometria de massas). Foram identificados fenilpropanóides e sesquiterpenos, estes últimos em pequenas quantidades, representando cerca de 97 por cento da composição total da fração volátil. O principal componente, 2-fenilnitroetano, corresponde a 71,12 por cento do extrato obtido por SFE.
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Object To study the technology of supercritical CO_2 extraction of effective components from Dragon's Blood which has the inhibiting function on ?-glucosidase. Methods The influence of the extraction pressure, temperature, time and fluid velocity on surplus extraction rate and the improvement of inhibition was mainly discussed. Results The optimal experimental parameters were 15 MPa extraction pressure, 45 ℃ extraction temperature, 30 kg/h fluid velocity and 2 h extraction time. Conclusion The results show that SFE-CO_2 can enormously increase the surplus extraction rate and the inhibitory activities on ?-glucosidase.
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Objective To study the technology of supercritical fluid CO_2 extraction(SFE CO_2) on urosolic acid from Cornus officinalis.Methods The effects of pressure,temperature,time,CO_2 flow rate types,and volume of entrainer on the urosolic acid extracts were studied. The optium conditions for SFE CO_2 was determined.The technology of SFE CO_2 was compared with that of traditional solvent extraction.Results The optium extraction conditions were as follows: pressure 35.0 MPa,temperature 318 K,absolute ethyl alcohol entrainer,content 4%,time 3 h and flow rate of CO_2 8 kg/h.Conclusion SFE CO_2 excels the traditional solvent extraction in yield,safety and efficiency.
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Objective To find out the optimal supercritical CO2 fluid extr ac tion prosess for Tetrahydropalmatine. Methods The extraction process was optimiz ed by orthogonal design with the yield of Tetrahydropalmatine as markers. Three factors including extraction pressure, temperature and the volume of entrainer were observed. Results The optimal condition of supercritical CO2 fluid extrac tion process was: under the pressure of 15Mpa at 40 ℃ , 1.5 fold of 95 % EtO H with Corydalis yanhusuo W.T.Wang as the entrainer. Conclusion The optimal supe rcritical process is feasible, with the advantage of low temperature and energy consumption, short time, high production and no organic residua.
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Objective To compare the effects of SFE - CO2 extraction and steam- distillation extraction for the extraction of volatile constituents from Huoxiang Zhengqi prescription. Methods The recovery rate of the volatile constituents and GC- MS method were used to compare the two different extraction methods. Result The recovery rate of volatile constituents was 0.45 % when extracted by steam distillation for 5 hours and 2.40 % by SFE - CO2 extraction for 3 hours. A large amount of peaks were detected in the SFE - CO2 extraction, while few compounds could be detected in the steam distillation extract 15 minutes later. Conclusion SFE - CO2 extraction method is a better method for the extraction of volatile constituents from Huoxiang Zhengqi prescription,with higher recovery rate, obtaining more ingredients and costing less time compared with those by steam distillation extract method.
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AIM: To compare the ligustilide content in Siwu Decoction and its ingredient herb. METHODS: To extract with SFE-CO 2 and to determine ligustilide with HPLC. RESULTS: Of the content of ligustilide, the highest in single herb, next in the mixture of Angelicae Sinensis Radix and Lignstic Rhizoma, the lowest in Siwu Decoction. CONCLUSION: When Angelicane Sinensis Radix and Lignstic Rhizoma were in compound preparation, the content of ligustilide became lower obviously.
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AIM: To optimize the extraction process of Myrrha by SFE-CO 2. METHODS: Orthogonal design was applied and GC was used to determine the contents of ?-Elemene in order to optimize the process. RESULTS: The optimized conditions were as follows: pressure 25 MPa, temperature 45 ?C and extraction time 4 h. CONCLUSION: The method of SFE-CO 2 is rapid, convenient in comparison with conventional methods.
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AIM: To Study the chemical constituents of volatile oil in Herminium bulleyi(Rolfe) Tang et Wang,ethnic drug from Miao Nationality. METHODS: The volatile oil of Herminium bulleyi was extracted by CO_2-supercritical fluid extraction method and steam distillation method,and their chemical constituents were analyzed and identified by GC-MS. RESULTS: SFE-CO_2 extraction gained 32 known constituents and steam distillation 33 ones.Volatile oil yield by SFE-CO_2 was three times that by steam distillation. CONCLUSION: The effect of SFE-CO_2 extraction on yield of volatile oil has obvious benefits both easy and quick.Cetylic acid content in volatile oil by SFE-CO_2 extraction is as high as 52%.
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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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The tanshinone ⅡA,an effective component of Radix Salviae Miltiorrhizae(RSM)can be extracted up to 90% in alcohol,but mostly decomposed in the later concentrating and drying procedures.Although reducing-pressure concentrating processes can reduce the decomposi- tion in experiment,but it can not preserve effectively the tanshinone during the large scale production because of the extended time of tanshinone in dampness and heat.Supercritical carbon dioxide extraction(SFE-CO_2)of RSM can give crystalline substance and dark red modifier when the alcohol is used as modifier at extraction pressure of 10 Mpa and the tem- perature at 40℃.The SFE-CO_2 technology can get higher concentration of tanshinone and be used during preparation production directly.The SFE-CO_2 technology is superior to the alco- hol-extraction technology.