CN103045371A - Preparation method for purifying essential oil and ursolic acid from wild ledum palustre in great khingan - Google Patents

Preparation method for purifying essential oil and ursolic acid from wild ledum palustre in great khingan Download PDF

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Publication number
CN103045371A
CN103045371A CN2012105955378A CN201210595537A CN103045371A CN 103045371 A CN103045371 A CN 103045371A CN 2012105955378 A CN2012105955378 A CN 2012105955378A CN 201210595537 A CN201210595537 A CN 201210595537A CN 103045371 A CN103045371 A CN 103045371A
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essential oil
ursolic acid
extraction
carbon dioxide
distillation
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CN103045371B (en
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张亚红
姚德坤
姚德利
万莉
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GREAT XINGAN MOUNTAINS LINGEBEI ORGANIC FOOD CO Ltd
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GREAT XINGAN MOUNTAINS LINGEBEI ORGANIC FOOD CO Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention belongs to the field of natural organic chemistry, and discloses a method. The method has the advantages that 1, a supercritical CO2 extraction technology is adopted; a system is sealed in an extraction process; destroy of small-molecule volatile oil is avoided; the whole essential oil extraction process is conducted at an approximate room temperature; the activity loss is very little; 2, a molecular distillation technology is adopted for purifying essential oil; an operating temperature is far below a boiling temperature of a substance at atmospheric pressure; in addition, the heating time is very short; the substance cannot be destroyed; the separation and purification degree and the yield of the essential oil are high; and 3, ultrasonic extraction is conducted, so that the heating time of effective components is shortened; the bioactivity is high; a silica gel column chromatography purification technology can ensure that the purity of ursolic acid is further increased; the operation is simple and easy; and the production cost is lowered greatly. With the adoption of the method, the extraction time is shortened greatly; an extraction speed is increased; in addition, a purification effect is obvious; contents of the effective components are high; the essential oil and ursolic acid can be obtained simultaneously; the relative content of the essential oil reaches 77.4%; and the purity of ursolic acid is increased to 98.73%.

Description

A kind of in the wild Du Xiang in Daxing'an Mountainrange the preparation method of purification essential oil and ursolic acid
Technical field:
The invention belongs to the natural organic chemistry field, relate to a kind of method of extracting Du's volatile oil and ursolic acid in the wild Du Xiang in Daxing'an Mountainrange, particularly relate to and a kind ofly utilize supercritical carbon dioxide extraction and join with the molecular distillation technique lotus root, ultrasonic extraction, the method for column chromatography again obtain respectively the method for essential oil, two kinds of compositions of ursolic acid.
Background technology:
Du Xiang is that Ericaceae Du Xiang belongs to evergreen dwarf shrub, up to more than 50 centimetres, and multi-branched, branch is thinner, and the food value of leaf is slightly thick, and is close and alternate has intense flavors, narrow linearity, long 2-4 centimetre, wide 1.5-3 millimeter.The anti-the moon of Du Xiang, and happiness water is wet, and less demanding to soil, often be born in river valley or sphagnum bog ground, grow in flakes group.This kind mainly is distributed in temperate zone, the Northern Hemisphere or cool temperature zone area, is distributed in northeast in China, concentrates and is distributed in Daxinganling District larch forest and tamarack white birch theropencedrymion, and resource is very abundant.
Du Xiang different sites chemical ingredients kind content has difference, and China starts late to the research of this wild plant resource of Du Xiang, to the research that only limits at present the volatile component of obtaining with steam distillation.From present result of study, Ledum palustre L. var. dilatatum Wahl.oil can be used for perfume industry.
Domesticly generally extract essential oil with steam distillation, exist the service temperature height, heat-sensitive materials easily decomposes, the shortcomings such as unstable product quality, difference of the present invention is to adopt supercritical carbon dioxide extraction and joins with the molecular distillation technique lotus root, ultrasonic extraction, the method for column chromatography again obtain respectively the method for essential oil, two kinds of compositions of ursolic acid.Prepared using degree of the present invention is high, and its meaning not only is to fully utilize local wild resource, develop new product, and to the reference frame that taken full advantage of similar sylvan life Resource Supply.
Summary of the invention:
Advantage of the present invention:
The present invention mainly adopts supercritical carbon dioxide extraction method, with molecular distillation lotus root connection, obtains the essential oil of purifying again; Extract slag and use again column chromatography purification with ultrasonic extraction, obtain high-purity ursolic acid.The present invention obtains essential oil and two kinds of products of ursolic acid simultaneously, and purity is high, and solvent-free chemistry is residual.
For achieving the above object, the technical solution used in the present invention is:
A kind of employing supercritical carbon dioxide extraction and with molecular distillation technique lotus root connection, ultrasonic extraction is the column chromatography again, obtains respectively the method for essential oil, two kinds of compositions of ursolic acid, its step is as follows:
(1) leaf of Ledum palustre L. var. dilatatum Wahl. is crushed to the 40-60 order, adopts supercritical carbon dioxide extraction, under certain temperature and pressure, with the CO of 1-2L/h 2Flow, extraction 4-6h reclaims CO 2, obtain the essential oil crude product;
(2) use wiped-film still, adopt two-stage to separate, with the certain pressure distillation, distillation temperature is 90-95 ℃ under input speed 1-1.5ml/min, 200-300r/min knifing rotating speed in the one-level distillation; With the certain pressure distillation, distillation temperature is 100-105 ℃ to secondary distillation, removes the essential oil peculiar smell, the essential oil of further purifying under input speed 1.2-2.0ml/min, 250-360r/min knifing rotating speed.Adopt GC-MS to analyze, the essential oil relative content is more than 75%;
(3) extract the ethanol that rear bits add certain volume concentration, ultrasonic extraction, ultrasonic frequency 50-70KHZ, solid-liquid ratio 1: 10-15, ultrasonic time 30-50min, thin-layer chromatography detect and analyze, and collect and obtain the ursolic acid extracting solution;
(4) Recycled ethanol, preliminary concentrated, get ursolic acid medicinal extract, be dissolved in butanols, upper 200-300 order silica gel column chromatography carries out purifying to extract;
(5) remove first the impurity such as remaining lipid with sherwood oil; Use again methanol-acetone with certain proportion as the elutriant wash-out, elutriant is with thin-layer chromatography tracking monitor (take 95% ursolic acid as reference substance contrast);
(6) it is concentrated to collect elutriant, and vacuum-drying obtains content and be the ursolic acid finished product more than 98%.
Embodiment:
Embodiment 1: a kind of employing supercritical carbon dioxide extraction and with molecular distillation technique lotus root connection, ultrasonic extraction is the column chromatography again, obtains respectively the method for essential oil, two kinds of compositions of ursolic acid, its step is as follows:
(1) the 1000g leaf of Ledum palustre L. var. dilatatum Wahl. is crushed to 40 orders, adopts supercritical carbon dioxide extraction, extracting pressure 10Mpa, and at 40 ℃, time 4h, CO 2Flow is 1L/h, reclaims CO 2, obtain the essential oil crude product;
(2) use wiped-film still, adopt two-stage to separate, one-level distillation pressure 3 handkerchiefs, in 1ml/min input speed, knifing rotating speed 200r/min distillation, distillation temperature is 90 ℃; Secondary distillation pressure 8 handkerchiefs, in 1.2ml/min input speed, knifing rotating speed 250r/min distillation, distillation temperature is 100 ℃, removes the essential oil peculiar smell, further purifies, and collects essential oil, adopts GC-MS to analyze, relative content is 75.3%;
(3) extract rear bits and add volume ratio 80% ethanol, ultrasonic extraction, ultrasonic frequency 50KHZ, solid-liquid ratio 1: 10, ultrasonic time 50min, thin-layer chromatography detect and analyze, and collect and obtain the ursolic acid extracting solution;
(4) Recycled ethanol, preliminary concentrated, get ursolic acid medicinal extract, be dissolved in butanols, upper 200-300 order silica gel column chromatography carries out purifying to extract;
(5) wash-out: remove first the impurity such as remaining lipid with sherwood oil; As the elutriant wash-out, elutriant was with thin-layer chromatography tracking monitor (contrast take 95% ursolic acid as reference substance) with methanol-acetone 10: 1;
(6) it is concentrated to collect elutriant, and vacuum-drying obtains content and be 98.2% ursolic acid finished product.
Case study on implementation 2: a kind of employing supercritical carbon dioxide extraction and with molecular distillation technique lotus root connection, ultrasonic extraction is the column chromatography again, obtains respectively the method for essential oil, two kinds of compositions of ursolic acid, its step is as follows:
(1) the 1000g leaf of Ledum palustre L. var. dilatatum Wahl. is crushed to 40 orders, adopts supercritical carbon dioxide extraction, at 45 ℃, and extracting pressure 12Mpa, time 5h, CO 2Flow is 1.5L/h, reclaims CO 2, obtain the essential oil crude product;
(2) use wiped-film still, adopt two-stage to separate, one-level distillation pressure 5 handkerchiefs, in 1.2ml/min input speed, knifing rotating speed 280r/min distillation, distillation temperature is 95 ℃; Secondary distillation pressure 9 handkerchiefs, in 1.5ml/min input speed, knifing rotating speed 300r/min distillation, distillation temperature is 105 ℃, removes the essential oil peculiar smell, further purifies, and collects essential oil, adopts GC-MS to analyze, relative content is 73.8%;
(3) extract rear bits and add volume ratio 90% ethanol, ultrasonic extraction, ultrasonic frequency 60KHZ, solid-liquid ratio 1: 12, ultrasonic time 40min, thin-layer chromatography detect and analyze, and collect and obtain the ursolic acid extracting solution;
(4) Recycled ethanol, preliminary concentrated, get ursolic acid medicinal extract, be dissolved in butanols, upper 200-300 order silica gel column chromatography carries out purifying to extract;
(5) wash-out: remove first the impurity such as remaining lipid with sherwood oil; Use methanol-acetone 9: 1 as the elutriant wash-out, elutriant is with thin-layer chromatography tracking monitor (contrast take 95% ursolic acid as reference substance) again;
(6) it is concentrated to collect elutriant, and vacuum-drying obtains content and be 98.73% ursolic acid finished product.
Case study on implementation 3: a kind of employing supercritical carbon dioxide extraction and with molecular distillation technique lotus root connection, ultrasonic extraction is the column chromatography again, obtains respectively the method for essential oil, two kinds of compositions of ursolic acid, its step is as follows:
(1) the 1000g leaf of Ledum palustre L. var. dilatatum Wahl. is crushed to 60 orders, adopts supercritical carbon dioxide extraction, at 45 ℃, and extracting pressure 15Mpa, time 6h, CO 2Flow is 2L/h, reclaims CO 2, obtain the essential oil crude product;
(2) use wiped-film still, adopt two-stage to separate, one-level distillation pressure 6 handkerchiefs, in 1.5ml/min input speed, knifing rotating speed 300r/min distillation, distillation temperature is 95 ℃; Secondary distillation pressure 10 handkerchiefs, in 2.0ml/min input speed, knifing rotating speed 360r/min distillation, distillation temperature is 100 ℃, removes the essential oil peculiar smell, further purifies, and collects essential oil, adopts GC-MS to analyze, relative content is 77.4%;
(3) extract rear bits and add volume ratio 95% ethanol, ultrasonic extraction, ultrasonic frequency 70KHZ, solid-liquid ratio 1: 15, ultrasonic time 30min, thin-layer chromatography detect and analyze, and collect and obtain the ursolic acid extracting solution;
(4) Recycled ethanol, preliminary concentrated, get ursolic acid medicinal extract, be dissolved in butanols, upper 200-300 order silica gel column chromatography carries out purifying to extract;
(5) wash-out: use first sherwood oil, remove the impurity such as remaining lipid; As the elutriant wash-out, elutriant was with thin-layer chromatography tracking monitor (contrast take 95% ursolic acid as reference substance) with methanol-acetone 8: 1;
(6) it is concentrated to collect elutriant, and vacuum-drying obtains content and be 98.5% ursolic acid finished product.

Claims (5)

  1. One kind adopt supercritical carbon dioxide extraction and with molecular distillation technique lotus root connection, ultrasonic extraction is the column chromatography again, obtains respectively the method for essential oil, two kinds of compositions of ursolic acid, its step is as follows:
    (1) leaf of Ledum palustre L. var. dilatatum Wahl. is crushed to the 40-60 order, adopts supercritical carbon dioxide extraction, under certain temperature and pressure, with the CO of 1-2L/h 2Flow, extraction 4-6h reclaims CO 2, obtain the essential oil crude product;
    (2) use wiped-film still, adopt two-stage to separate, the one-level distillation is distilled under input speed 1-1.5ml/min, 200-300r/min knifing rotating speed, and distillation temperature is 90-95 ℃; Secondary distillation distills under input speed 1.2-2.0ml/min, 250-360r/min knifing rotating speed, and distillation temperature is 100-105 ℃, removes the essential oil peculiar smell, and the essential oil of further purifying adopts GC-MS to analyze, and the essential oil relative content is more than 65%;
    (3) extract rear bits and add the certain volume concentration ethanol, ultrasonic extraction, ultrasonic frequency 50-70KHZ, solid-liquid ratio 1: 10-15, ultrasonic time 30-50min, thin-layer chromatography detect and analyze, and collect and obtain the ursolic acid extracting solution;
    (4) Recycled ethanol, preliminary concentrated, get ursolic acid medicinal extract, be dissolved in butanols, upper 200-300 order silica gel column chromatography carries out purifying to extract,
    (5) remove first the impurity such as remaining lipid with sherwood oil; Use again methanol-acetone with certain proportion as the elutriant wash-out, elutriant is with thin-layer chromatography tracking monitor (take 95% ursolic acid as reference substance contrast);
    (6) it is concentrated to collect elutriant, and vacuum-drying obtains content and be the ursolic acid finished product more than 98%.
  2. 2. employing supercritical carbon dioxide extraction according to claim 1 and join with the molecular distillation technique lotus root, ultrasonic extraction is the column chromatography again, obtain respectively the method for essential oil, two kinds of compositions of ursolic acid, it is characterized in that: in the described step (1), the supercritical carbon dioxide extraction temperature is 40-45 ℃, extracting pressure 10-15Mpa.
  3. 3. employing supercritical carbon dioxide extraction according to claim 2 and join with the molecular distillation technique lotus root, ultrasonic extraction is the column chromatography again, obtain respectively the method for essential oil, two kinds of compositions of ursolic acid, it is characterized in that: in the described step (2), one-level distillation pressure is the 3-5 handkerchief, secondary distillation pressure 8-10 handkerchief.
  4. 4. employing supercritical carbon dioxide extraction according to claim 3 and join with the molecular distillation technique lotus root, ultrasonic extraction is the column chromatography again, obtain respectively the method for essential oil, two kinds of compositions of ursolic acid, it is characterized in that: in the described step (3), organic solvent ethanol volumetric concentration is 80-95%.
  5. 5. employing supercritical carbon dioxide extraction according to claim 4 and join with the molecular distillation technique lotus root, ultrasonic extraction is the column chromatography again, obtain respectively the method for essential oil, two kinds of compositions of ursolic acid, it is characterized in that: in the described step (5), eluting solvent methanol-acetone ratio is 8-10: 1.
CN201210595537.8A 2012-12-13 2012-12-13 A kind of preparation method of purify from the wild Du Xiang in Daxing'an Mountainrange essential oil and ursolic acid Active CN103045371B (en)

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Cited By (13)

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CN103263072A (en) * 2013-05-23 2013-08-28 红云红河烟草(集团)有限责任公司 Preparation method of medium-temperature tobacco material for non-combustion cigarette
CN103263078A (en) * 2013-05-23 2013-08-28 红云红河烟草(集团)有限责任公司 Preparation method of low-temperature tobacco material for non-combustion cigarette
CN103558324A (en) * 2013-10-25 2014-02-05 齐齐哈尔大学 Method for extracting and identifying aesculin, fraxin, fraxetin and resveratrol from ledum palustre l.var.angustum e.busch
CN104450190A (en) * 2014-12-03 2015-03-25 湖北中烟工业有限责任公司 Method for preparing chamomile extract for tobaccos
CN105001991A (en) * 2015-06-15 2015-10-28 中国林业科学研究院林产化学工业研究所 Ledum palustre extractive with sterilization function and preparing method and application thereof
CN105273833A (en) * 2015-11-30 2016-01-27 中华全国供销合作总社南京野生植物综合利用研究所 Method for carrying out supercritical CO2 extraction on kosteletzkya virginica L. flower essential oil
CN105273846A (en) * 2015-11-30 2016-01-27 中华全国供销合作总社南京野生植物综合利用研究所 Method for carrying out supercritical CO2 extraction on kosteletzkya virginica L. leaf essential oil
CN106318641A (en) * 2016-09-30 2017-01-11 湖北中烟工业有限责任公司 Method for refining lemongrass essential oil
CN106433983A (en) * 2016-09-30 2017-02-22 湖北中烟工业有限责任公司 Refining method of thyme essential oil
CN108102788A (en) * 2018-01-22 2018-06-01 重庆汇达柠檬科技集团有限公司 The extracting method of essential oil in a kind of lemonlike citrus leaf
CN109897730A (en) * 2019-03-18 2019-06-18 黑龙江中医药大学 A kind of Du Xiang refined volatile oil refinement method
CN110237017A (en) * 2019-07-24 2019-09-17 黑龙江省科学院高技术研究院 A kind of toner and preparation method thereof containing Ledum palustreL .subsp .decumdens essential oil
CN115322837A (en) * 2022-08-17 2022-11-11 东北林业大学 Refined ledum essential oil refining process and antibacterial application thereof

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103263078A (en) * 2013-05-23 2013-08-28 红云红河烟草(集团)有限责任公司 Preparation method of low-temperature tobacco material for non-combustion cigarette
CN103263072B (en) * 2013-05-23 2015-05-27 红云红河烟草(集团)有限责任公司 Preparation method of medium-temperature tobacco material for non-combustion cigarette
CN103263072A (en) * 2013-05-23 2013-08-28 红云红河烟草(集团)有限责任公司 Preparation method of medium-temperature tobacco material for non-combustion cigarette
CN103558324A (en) * 2013-10-25 2014-02-05 齐齐哈尔大学 Method for extracting and identifying aesculin, fraxin, fraxetin and resveratrol from ledum palustre l.var.angustum e.busch
CN104450190B (en) * 2014-12-03 2017-02-01 湖北中烟工业有限责任公司 Method for preparing chamomile extract for tobaccos
CN104450190A (en) * 2014-12-03 2015-03-25 湖北中烟工业有限责任公司 Method for preparing chamomile extract for tobaccos
CN105001991A (en) * 2015-06-15 2015-10-28 中国林业科学研究院林产化学工业研究所 Ledum palustre extractive with sterilization function and preparing method and application thereof
CN105273833A (en) * 2015-11-30 2016-01-27 中华全国供销合作总社南京野生植物综合利用研究所 Method for carrying out supercritical CO2 extraction on kosteletzkya virginica L. flower essential oil
CN105273846A (en) * 2015-11-30 2016-01-27 中华全国供销合作总社南京野生植物综合利用研究所 Method for carrying out supercritical CO2 extraction on kosteletzkya virginica L. leaf essential oil
CN106318641A (en) * 2016-09-30 2017-01-11 湖北中烟工业有限责任公司 Method for refining lemongrass essential oil
CN106433983A (en) * 2016-09-30 2017-02-22 湖北中烟工业有限责任公司 Refining method of thyme essential oil
CN108102788A (en) * 2018-01-22 2018-06-01 重庆汇达柠檬科技集团有限公司 The extracting method of essential oil in a kind of lemonlike citrus leaf
CN109897730A (en) * 2019-03-18 2019-06-18 黑龙江中医药大学 A kind of Du Xiang refined volatile oil refinement method
CN110237017A (en) * 2019-07-24 2019-09-17 黑龙江省科学院高技术研究院 A kind of toner and preparation method thereof containing Ledum palustreL .subsp .decumdens essential oil
CN110237017B (en) * 2019-07-24 2022-02-15 黑龙江省科学院高技术研究院 Toning lotion containing ledum tenuifolia essential oil and preparation method thereof
CN115322837A (en) * 2022-08-17 2022-11-11 东北林业大学 Refined ledum essential oil refining process and antibacterial application thereof

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