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1.
J Sep Sci ; 43(13): 2646-2656, 2020 Jul.
Article in English | MEDLINE | ID: mdl-32250541

ABSTRACT

A green and efficient strategy was established and optimized for target-oriented extraction, enrichment and separation of cadinene sesquiterpenoids from Eupatorium adenophorum Spreng., using the combination of supercritical fluid extraction, molecular distillation, and industrial preparative chromatography for the first time. The extraction conditions of supercritical fluid extraction were initially optimized by orthogonal experimental design. Under the optimum conditions, the contents of 9-oxo-10,11-dehydroageraphorone and 10Hß-9-oxo-ageraphorone, which were 55.00% and 6.01%, respectively, were much higher than conventional extraction methods. Then, the molecular distillation enrichment method was established and investigated by response surface methodology technology, which showed strong specificity for enriching target compounds and removing impurities from crude extracts. Under the optimum conditions of molecular distillation, total contents of cadinene sesquiterpenoids were increased to 89.19%. Finally, a total of 146 mg of 9-oxo-10,11-dehydroageraphorone and 29 mg of 10Hß-9-oxo-ageraphorone were easily obtained by industrial preparative chromatography, from 200 mg of distillation fraction, with purities over 99%. The contents of target components were analyzed by HPLC, and structures of them were identified by high-resolution MS, 1 H-NMR, and 13 C-NMR spectroscopy. These results indicate that it is a simple, effective, and eco-friendly strategy, which is easily converted into industrial scale.


Subject(s)
Ageratina/chemistry , Sesquiterpenes/isolation & purification , Sesquiterpenes/chemistry
2.
Zhong Yao Cai ; 38(4): 827-30, 2015 Apr.
Article in Chinese | MEDLINE | ID: mdl-26672353

ABSTRACT

OBJECTIVE: To study the supercritical CO2 fluids extraction (SFE) method to extract the components from Taxus yunnanensis. METHODS: Medicinal meterials were extracted by supercritical CO2, and then purified by industrial chromatography. Using the extraction yield of 10-DAB as the index,single factor test was carried out to investigate the effect of co-solvent, extraction time, extraction pressure, extraction temperature, pressure and temperature of separation kettle I. Then orthogonal experiment was used to optimize the best extraction condition. RESULTS: The suitable extraction condition was as follows: the ratio of co-solvent (80% ethanol) amount and the madicinal materials was 3: 1, Separation kettle I pressure was 14 MPa, separation kettle I temperature was 40 °C, extraction pressure was 25 MPa, extraction temperature was 60 T and extraction time was 90 min. The extract was separated by industrial chromatographic and then crystallized. CONCLUSION: The supercritical CO2 extraction and purification process of 10-DAB were simple and feasible.


Subject(s)
Plant Leaves/chemistry , Taxoids/isolation & purification , Taxus/chemistry , Chromatography, Supercritical Fluid , Ethanol , Pressure , Solvents , Temperature
3.
Zhong Yao Cai ; 36(3): 475-8, 2013 Mar.
Article in Chinese | MEDLINE | ID: mdl-24010333

ABSTRACT

OBJECTIVE: To research the optimal extraction process of supercritical CO2 extraction and analyze the component of the oil extracted from Aesculus wilsonii seed. METHODS: Using the yield of Aesculus wilsonii seed oil as the index, optimized supercritical CO2 extraction parameter by orthogonal experiment methodology and analysed the compounds of Aesculus wilsonii seed oil by GC-MS. RESULTS: The optimal parameters of the supercritical CO2 extraction of the oil extracted from Aesculus wilsoniit seed were determined: the extraction pressure was 28 MPa and the temperature was 38 degrees C, the separation I pressure was 12 MPa and the temperature was 40 degrees C, the separation II pressure was 5 MPa and the temperature was 40 degrees C, the extraction time was 110 min. The average extraction rate of Aesculus wilsonii seed oil was 1.264%. 26 kinds of compounds were identified by GC-MS in Aesculus wilsonii seed oil extracted by supercritical CO2. The main components were fatty acids. CONCLUSION: Comparing with the petroleum ether extraction, the supercritical CO2 extraction has higher extraction rate, shorter extraction time, more clarity oil. The kinds of fatty acids with high amounts in Aesculus wilsonii seed oil is identical in general, the kinds of fatty acids with low amounts in Aesculus wilsonii seed oil have differences.


Subject(s)
Aesculus/chemistry , Chromatography, Supercritical Fluid , Fatty Acids/analysis , Plant Oils/isolation & purification , Seeds/chemistry , Carbon Dioxide , Ethers/chemistry , Gas Chromatography-Mass Spectrometry , Plant Oils/chemistry , Pressure , Solvents/chemistry , Temperature
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