CN1985977A - Zedoary oil leaching process from zedoary powder with petroleum ether - Google Patents
Zedoary oil leaching process from zedoary powder with petroleum ether Download PDFInfo
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- CN1985977A CN1985977A CN 200610110213 CN200610110213A CN1985977A CN 1985977 A CN1985977 A CN 1985977A CN 200610110213 CN200610110213 CN 200610110213 CN 200610110213 A CN200610110213 A CN 200610110213A CN 1985977 A CN1985977 A CN 1985977A
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- petroleum ether
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- powder
- rhizoma curcumae
- curcumae
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Abstract
The process of reflux extracting zedoary oil with petroleum ether form 20-325 mesh zedoary powder includes the following steps: setting 20-325 mesh zedoary powder obtained through low temperature crushing at 0 deg.c to -60 deg.c into reflux extractor and mixing with petroleum ether; water bath heating the reflux extractor to boil for determined time and suction filtering the extracted liquid with microporous filtering membrane for several times; merging the filtrate and decompression distilling to evaporate and recover petroleum ether; collecting volatile zedoary oil and volatilizing residual petroleum ether through natural ventilation. The process is simple, and has low operation temperature to avoid the change of heat sensitive matter and zedoary oil extracting rate as high as 3.24 %.
Description
Technical field
The present invention relates to a kind of from plant roots and stems the method for effective component extracting, be the method for from the Rhizoma Curcumae powder, extracting Oleum Curcumae concretely.
Background technology
Rhizoma Curcumae, the hot temperature of property, bitter in the mouth is returned the liver spleen channel.Have the circulation of qi promoting removing blood stasis, the removing food stagnancy pain-relieving functions cures mainly note of the ancient Chinese abdominal mass mass in the abdomen, blood stasis amenorrhea, food stagnation distending pain; Early cervical carcinoma.Consumption 6~9g all uses its dry rhizome.Rhizoma Curcumae has antineoplastic action, and the understanding that its main component that plays a role is relatively more consistent at present is the effective ingredient in the Oleum Curcumae.Document (chemical constitution study of Rhizoma Curcumae quintessence oil is produced in the Guizhou Province. GUIHAIA, 19 (1): make the light yellow quintessence oil that Rhizoma Curcumae is produced in the Guizhou Province with steam distillation 95~96), oil yield is 0.5%~0.8%, document (research of Rhizoma Curcumae volatile oil extraction and clathrate process. fine chemistry industry .2003,20 (3): 166~168) optimised process of extraction volatile oil is from the Rhizoma Curcumae powder: the Rhizoma Curcumae powder soaks 1h, add 8 times of decoctings and endure, carry oil time 8h, the yield of volatile oil is 2.38%.Document (warm Rhizoma Curcumae The Chemical Constituents [J]. CHINA JOURNAL OF CHINESE MATERIA MEDICA, 2000,25 (3): 163) with methanol extraction temperature Rhizoma Curcumae dry powder, pressure reducing and steaming methanol, the suitable quantity of water dilution, Petroleum ether extraction boils off solvent and promptly gets volatile oil, and oil yield is 3.12%.
Summary of the invention
Technical solution of the present invention is as follows:
Oleum Curcumae of the present invention extracts from the Rhizoma Curcumae powder with petroleum ether reflux, extract, technology, and extracting method may further comprise the steps:
(1) Rhizoma Curcumae is cleaned, dry, section, pulverize with pulverizer, set: pulverize temperature and be zero degree to-60 ℃, particle diameter was 20 order to 325 mesh sieves, the Rhizoma Curcumae powder, it is placed the reflux, extract, device, add the petroleum ether and the mixing of respective quality multiple;
(2) connect the reflux, extract, device, water-bath picks up counting when slowly being heated to boiling, and keeps little boiling to stop heating to the stipulated time, with microporous filter membrane (0.15 μ m) sucking filtration petroleum ether extract, extracts for several times merging filtrate with method;
(3) with merging filtrate reclaim under reduced pressure petroleum ether, after the solvent evaporated, volatile oil is taken out, and volatile oil appended on the wall is washed fully with an amount of petroleum ether, place clean container together, wave most petroleum ether in gravity-flow ventilation place, take by weighing volatile oil weight, record.
The above-described method of using petroleum ether reflux, extract, technology to extract Oleum Curcumae from the Rhizoma Curcumae powder, the boiling range of used petroleum ether is 30 ℃~60 ℃.
The above-described method of using petroleum ether reflux, extract, technology to extract Oleum Curcumae from the Rhizoma Curcumae powder, when adding the petroleum ether of respective quality multiple, its quality multiple is 10 times~20 times.
Above-describedly extracts the method for Oleum Curcumae with petroleum ether reflux, extract, technology from the Rhizoma Curcumae powder, slowly be heated to when seething with excitement in water-bath and pick up counting, and keep little and boil to the stipulated time, its stipulated time is 1 hour~3 hours.
The above-described method of using petroleum ether reflux, extract, technology to extract Oleum Curcumae from the Rhizoma Curcumae powder, when extracting for several times with method, its extraction time is 1~3 time.
Above-described Rhizoma Curcumae powder, be to pulverize with pulverizer, setup parameter is respectively during pulverizing: 0 ℃ of temperature crosses that 20 mesh sieves ,-30 ℃ of temperature are crossed 50 mesh sieves ,-60 ℃ of temperature are crossed 80 mesh sieves and 325 mesh sieves, and the detected value of pulverizing the back powder body is followed successively by: surface area/volume is 0.1732m
2/ cm
3, 0.1648m
2/ cm
3, 0.15896m
2/ cm
3, 0.6282m
2/ cm
3, volume average particle size is D[4:3] 107.462, D[4:3] 84.984, D[4:3] 71.893, D[4:3] 34.938, the area mean diameter is D[3:2] 43.266, D
50=83.261 μ m, D[3:2] 34.138, D
50=78.539 μ m, D[3:2] 31.824, D
50=72.137 μ m, D[3:2] 8.954, D
50=31.905 μ m, calculating mean diameter according to concrete grain diameter value is R
1=126.13 μ m, R
1=90.65 μ m, R
1=81.92 μ m, R
1=37.27 μ m know with the biology microscope sem observation: cross 20 orders, 50 orders, all acellular breaking cellular wall of 80 mesh sieve powder body; Cross all cell wall breaking of 325 order powder body.
Oleum Curcumae purposes of the present invention is: Oleum Curcumae is used for antitumor, antiviral, perhaps as the application of Chinese medicine preparation raw material.
Extract the method for Oleum Curcumae compares with steam distillation, substantive distinguishing features of the present invention and obvious improvement are: easy and simple to handle, oil extracting rate is higher than steam distillation, and this law operative temperature is low, can avoid the variation of heat-sensitive materials, thereby has preserved the natural quality of Oleum Curcumae better.Oil extracting rate can reach more than 3.24%.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
The specific embodiment
Embodiment 1: get an amount of Rhizoma Curcumae, clean, 50 ℃ of oven dry descended 20 mesh sieves to pulverize with HFM-6 micronizing vibromill in 0 ℃ of low temperature, obtained the Rhizoma Curcumae powder.With its cell wall breaking situation of biology microscope sem observation.Detect its particle diameter with JL-1178 dry method laser particle analyzer.It is an amount of that precision takes by weighing the Rhizoma Curcumae powder, places the reflux, extract, device, and adding quality multiple is 10 times petroleum ether (30 ℃~60 ℃) and a mixing; Connect the reflux, extract, device, water-bath picks up counting when slowly being heated to boiling, and keeps stopping heating behind little 1h of boiling, and with microporous filter membrane (0.15 μ m) sucking filtration petroleum ether extract, extracts 3 times merging filtrate with method; With merging filtrate reclaim under reduced pressure petroleum ether, after the solvent evaporated, volatile oil is taken out, and with an amount of petroleum ether volatile oil appended on the wall is washed fully, place clean container together, wave most petroleum ether in gravity-flow ventilation place, take by weighing volatile oil weight, and the calculating oil extracting rate is 3.235%.
Embodiment 2: get an amount of Rhizoma Curcumae, clean, 50 ℃ of oven dry descended 50 mesh sieves to pulverize with HFM-6 micronizing vibromill in-30 ℃ of low temperature, obtained the Rhizoma Curcumae powder.With its cell wall breaking situation of biology microscope sem observation.Detect its particle diameter with JL-1178 dry method laser particle analyzer.It is an amount of that precision takes by weighing the Rhizoma Curcumae powder, places the reflux, extract, device, and adding quality multiple is 20 times petroleum ether (30 ℃~60 ℃) and a mixing; Connect the reflux, extract, device, water-bath picks up counting when slowly being heated to boiling, and keeps stopping heating behind little 2h of boiling, and with microporous filter membrane (0.15 μ m) sucking filtration petroleum ether extract, extracts 3 times merging filtrate with method; With merging filtrate reclaim under reduced pressure petroleum ether, after the solvent evaporated, volatile oil is taken out, and with an amount of petroleum ether volatile oil appended on the wall is washed fully, place clean container together, wave most petroleum ether in gravity-flow ventilation place, take by weighing volatile oil weight, and the calculating oil extracting rate is 3.2614%.
Embodiment 3: get an amount of Rhizoma Curcumae, clean, 50 ℃ of oven dry descended 80 mesh sieves to pulverize with HFM-6 micronizing vibromill in-60 ℃ of low temperature, obtained the Rhizoma Curcumae powder.With its cell wall breaking situation of biology microscope sem observation.Detect its particle diameter with JL-1178 dry method laser particle analyzer.It is an amount of that precision takes by weighing the Rhizoma Curcumae powder, places the reflux, extract, device, and adding quality multiple is 20 times petroleum ether (30 ℃~60 ℃) and a mixing; Connect the reflux, extract, device, water-bath picks up counting when slowly being heated to boiling, and keeps stopping heating behind little 3h of boiling, and with microporous filter membrane (0.15 μ m) sucking filtration petroleum ether extract, extracts 2 times merging filtrate with method; With merging filtrate reclaim under reduced pressure petroleum ether, after the solvent evaporated, volatile oil is taken out, and with an amount of petroleum ether volatile oil appended on the wall is washed fully, place clean container together, wave most petroleum ether in gravity-flow ventilation place, take by weighing volatile oil weight, and the calculating oil extracting rate is 3.2818%.
Embodiment 4: get an amount of Rhizoma Curcumae, clean, 50 ℃ of oven dry descended 325 mesh sieves to pulverize with HFM-6 micronizing vibromill in-60 ℃ of low temperature, obtained the Rhizoma Curcumae powder.With its cell wall breaking situation of biology microscope sem observation.Detect its particle diameter with JL-1178 dry method laser particle analyzer.It is an amount of that precision takes by weighing the Rhizoma Curcumae powder, places the reflux, extract, device, and adding quality multiple is 20 times petroleum ether (30 ℃~60 ℃) and a mixing; Connect the reflux, extract, device, water-bath picks up counting when slowly being heated to boiling, and keeps stopping heating behind little 3h of boiling, and with microporous filter membrane (0.15 μ m) sucking filtration petroleum ether extract, extracts 1 time with method; Filtrate decompression is reclaimed petroleum ether, after the solvent evaporated, volatile oil is taken out, and with an amount of petroleum ether volatile oil appended on the wall is washed fully, place clean container together, wave most petroleum ether in gravity-flow ventilation place, take by weighing volatile oil weight, and the calculating oil extracting rate is 3.2935%.
Claims (3)
1, a kind of method with Oleum Curcumae in the Petroleum ether extraction Rhizoma Curcumae powder, it is characterized in that: described Oleum Curcumae extracts and extracts from the Rhizoma Curcumae powder with the petroleum ether reflux extraction, and extracting method may further comprise the steps:
(1) Rhizoma Curcumae is cleaned, dry, section, pulverize with pulverizer, set: pulverizing temperature is 0 ℃ to-60 ℃, and particle diameter was 20 order to 325 mesh sieves, the Rhizoma Curcumae powder, it is placed the reflux, extract, device, the petroleum ether and the mixing of adding respective quality multiple;
(2) connect the reflux, extract, device, water-bath picks up counting when slowly being heated to boiling, and keeps little boiling to stop heating to the stipulated time, with microporous filter membrane (0.15 μ m) sucking filtration petroleum ether extract, extracts for several times merging filtrate with method;
(3) with merging filtrate reclaim under reduced pressure petroleum ether, after the solvent evaporated, volatile oil is taken out, and volatile oil appended on the wall is washed fully with an amount of petroleum ether, place clean container together, wave most petroleum ether in gravity-flow ventilation place, take by weighing volatile oil weight, record.
The above-described method of using petroleum ether reflux, extract, technology to extract Oleum Curcumae from the Rhizoma Curcumae powder, the boiling range of used petroleum ether is 30 ℃~60 ℃.
The above-described method of using petroleum ether reflux, extract, technology to extract Oleum Curcumae from the Rhizoma Curcumae powder, when adding the petroleum ether of respective quality multiple, its quality multiple is 10 times~20 times.
Above-describedly extracts the method for Oleum Curcumae with petroleum ether reflux, extract, technology from the Rhizoma Curcumae powder, slowly be heated to when seething with excitement in water-bath and pick up counting, and keep little and boil to the stipulated time, its stipulated time is 1 hour~3 hours.
The above-described method of using petroleum ether reflux, extract, technology to extract Oleum Curcumae from the Rhizoma Curcumae powder, when extracting for several times with method, its extraction time is 1~3 time.
2, the method for from the Rhizoma Curcumae powder, extracting Oleum Curcumae according to claim 1, it is characterized in that: pulverize Rhizoma Curcumae with pulverizer, setup parameter is respectively: 0 ℃ of temperature crosses that 20 mesh sieves ,-30 ℃ of temperature are crossed 50 mesh sieves ,-60 ℃ of temperature are crossed 80 mesh sieves and 325 mesh sieves, and the detected value of pulverizing the back powder body is followed successively by: surface area/volume is 0.1732m
2/ cm
3, 0.1648m
2/ cm
3, 0.15896m
2/ cm
3, 0.6282m
2/ cm
3, volume average particle size is D[4:3] 107.462, D[4:3] 84.984, D[4:3] 71.893, D[4:3] 34.938, the area mean diameter is D[3:2] 43.266, D
50=83.261 μ m, D[3:2] 34.138, D
50=78.539 μ m, D[3:2] 31.824, D
50=72.137 μ m, D[3:2] 8.954, D
50=31.905 μ m, calculating mean diameter according to concrete grain diameter value is R
1=126.13 μ m, R
1=90.65 μ m, R
1=81.92 μ m, R
1=37.27 μ m know with the biology microscope sem observation: cross 20 orders, 50 orders, all acellular breaking cellular wall of 80 mesh sieve powder body; Cross all cell wall breaking of 325 mesh sieve powder body.
3, the purposes of Oleum Curcumae as claimed in claim 1 is characterized in that: Oleum Curcumae is at antitumor, antiviral, perhaps as the application of Chinese medicine preparation raw material.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106387475A (en) * | 2016-09-30 | 2017-02-15 | 安徽华澳生物技术有限公司 | Feed additive for prolonging egg production period of laying chickens and application thereof |
CN108896688A (en) * | 2018-05-04 | 2018-11-27 | 贵州景诚制药有限公司 | A kind of oil of zedoary turmeric extracting method and the oil of zedoary turmeric obtained by this method and its application |
-
2006
- 2006-12-12 CN CN 200610110213 patent/CN1985977A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106387475A (en) * | 2016-09-30 | 2017-02-15 | 安徽华澳生物技术有限公司 | Feed additive for prolonging egg production period of laying chickens and application thereof |
CN108896688A (en) * | 2018-05-04 | 2018-11-27 | 贵州景诚制药有限公司 | A kind of oil of zedoary turmeric extracting method and the oil of zedoary turmeric obtained by this method and its application |
CN108896688B (en) * | 2018-05-04 | 2021-05-04 | 贵州景诚制药有限公司 | Zedoary turmeric oil extraction method, zedoary turmeric oil obtained by the method and application thereof |
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