CN101818098A - Method for preparing cardamon oil resin through microwave assistance - Google Patents
Method for preparing cardamon oil resin through microwave assistance Download PDFInfo
- Publication number
- CN101818098A CN101818098A CN 201010157988 CN201010157988A CN101818098A CN 101818098 A CN101818098 A CN 101818098A CN 201010157988 CN201010157988 CN 201010157988 CN 201010157988 A CN201010157988 A CN 201010157988A CN 101818098 A CN101818098 A CN 101818098A
- Authority
- CN
- China
- Prior art keywords
- oil resin
- preparing
- temperature
- under
- microwave
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Fats And Perfumes (AREA)
- Seasonings (AREA)
- Edible Oils And Fats (AREA)
Abstract
The invention discloses a method for preparing cardamon oil resin through microwave assistance, which comprises the following steps of: (1) crushing: crushing dry fructus amomi into 30 to 60 meshes; (2) soaking: soaking the fructus amomi powder for 11 to 23 minutes by using 95 percent ethanol; (3) extracting: maintaining for 7 to 15 minutes under the conditions that the temperature is between 45 and 72 DEG C and the microwave power is between 100 and 300W; (4) separating: filtering by using a filter bag with 200 to 400 meshes to obtain filter liquor A; (5) repeatedly extracting: repeatedly extracting for 10 to 18 minutes by using the 95 percent ethanol; (6) repeatedly separating: filtering by using a filter bag with 200 to 400 meshes to obtain filter liquor B; (7) concentrating: merging the filter liquor A and B, and concentrating under the vacuum degree condition until the ethanol is evacuated; and (8) cooling: cooling the concentrated materials to room temperature to obtain the cardamon oil resin. The method for preparing the cardamon oil resin is economic and practical and has high efficiency; and the prepared cardamon oil resin is slurry, has pure fragrance and taste of the fructus amomi, can be applied to foods, health-care products, medicaments and daily supplies, and has wide application.
Description
Technical field
The present invention relates to a kind of method of from fructus amomi, extracting flavour substances.
Background technology
Fructus amomi (Amomum villosum Lour), the another name fructus amomi is the fruit that Zingiber beans bandit belongs to, and as one of " four Da Nan medicines ", has the function of promoting the circulation of qi, pain relieving, invigorating the spleen, dissipate-swelling, antiabortive preventing or arresting vomiting on traditional Chinese medicine; As the hot food raw material of perfume (or spice), it can be used as the seasonings spice, also can be used as protective foods.Fructus amomi contains nearly 60 kinds of detectable flavor compound, and wherein dl-Bornyl Acetate, (soil) camphor and borneol are main component, is R-cloves alkene secondly, flavor compound such as copaene.
The method of extracting at present the fructus amomi flavor compound has following three kinds: 1, steam distillation method: this method Yin Wendu is higher, the time is long and be difficult to obtain complete flavor compound; 2, supercritical extraction: this method equipment input and operation cost are higher, and it is relatively poor to extract the taste cost-effectiveness; 3, solvent thermal extraction process: this method is difficult to the flavor compound in the stripping fructus amomi when lower temperature, and comparatively high temps then makes lower boiling composition scatter and disappear.
Therefore,, study a kind of economical and practical fructus amomi local flavor extracting method, thereby prepare the Fructus Amomi oil resin, be very important from market demand and agricultural-food deep processing dual requirements.
Summary of the invention
The object of the present invention is to provide the flavor compound in a kind of microwave-assisted solvent method extraction fructus amomi and prepare the method for oleo-resinous, this method is economical and practical, yield is high.
The method of a kind of preparing cardamon oil resin through microwave assistance provided by the invention may further comprise the steps:
(1) pulverizes: under 35～57 ℃ of temperature, dry sand benevolence is crushed to 30～60 orders;
(2) soak: amomum powder by weight: mix 95% ethanol=1: 3.2～5.5, soaked 11～23 minutes;
(3) extract: the mixture after will soaking is sent into extractor, is that 45～72 ℃, microwave power are to keep 7～15min under the condition of 100～300W in temperature;
(4) separate: mixture is sent into whizzer, under 800～1200 rev/mins, 35～65 ℃ of conditions of temperature, filter with 200～400 order filter bags, must filter residue and filtrate A;
(5) carry again: filter residue being added 3.5～6 times 95% ethanol by its weight, mix, is that 45～72 ℃, microwave power are to keep 10～18min under the condition of 100～300W in temperature;
(6) subdivision from: the mixture after will carrying is again sent into whizzer, filter under 800～1200 rev/mins, 35～65 ℃ of conditions of temperature with 200～400 order filter bags, liquor B;
(7) concentrate: merge A, B filtrate, under the condition of vacuum tightness 0.06～0.085MPa, 45～67 ℃ of Heating temperatures, 8～14 rev/mins of stirring velocitys, concentrate, exhausted until ethanol;
(8) cooling: will concentrate material and under the condition of 20～30 ℃ of temperature of cooling water, 8～14 rev/mins of stirring velocitys, be cooled to room temperature, and get the Fructus Amomi oil resin.
Among the above-mentioned preparation method, the used dry sand benevolence of step (1) is by nature or physical method exsiccant fructus amomi, its moisture mass percent≤7%; The used equipment of step (1) is the tooth-like pulverizer of band refrigerative; Step (3), the used equipment of step (5) are the microwave-assisted extractor of belt stirrer; Step (4), the used equipment of step (6) are the link-suspended basket centrifuge of adding a cover; The used equipment of step (7) is the vacuum concentrator of belt stirrer; The used equipment of step (8) is the cooling tank of belt stirrer.
Method of the present invention, as required its step (5), step (6) can repeat again for the third time or more times extraction with separate, also can not carry out this two step and only once extract and separate.
The inventive method is economical and practical, yield is high, and the Fructus Amomi oil resin that makes is the slurry shape, has pure fructus amomi fragrance and taste, can be used for food, healthcare products, medicine and cosmetics of everyday use, and is of many uses.
Embodiment
The present invention will be described below to enumerate specific embodiment.It is pointed out that embodiment only is used for that the invention will be further described, do not represent protection scope of the present invention, nonessential modification and adjustment that other people make according to the present invention still belong to protection scope of the present invention.In following examples, the used dry sand benevolence of step (1) is by nature or physical method exsiccant fructus amomi, its moisture mass percent≤7%; The used equipment of step (1) is the tooth-like pulverizer of band refrigerative; Step (3), the used equipment of step (5) are the microwave-assisted extractor of belt stirrer; Step (4), the used equipment of step (6) are the link-suspended basket centrifuge of adding a cover; The used equipment of step (7) is the vacuum concentrator of belt stirrer; The used equipment of step (8) is the cooling tank of belt stirrer.
Embodiment 1
The method of the preparing cardamon oil resin through microwave assistance that the embodiment of the invention 1 provides may further comprise the steps:
1, pulverizes
Under 45 ℃ of temperature, amomum powder is broken to 40 orders;
2, soak
Amomum powder by weight: 95% ethanol=mix at 1: 3.5, soaked 13 minutes;
3, extract
Mixture after soaking is sent into extractor, is that 52 ℃, microwave power are to keep 11min under the condition of 200W in temperature;
4, separate
Mixture is sent into whizzer, under 1200 rev/mins, 45 ℃ of conditions of temperature, filters with 400 order filter bags, filter residue and filtrate A;
5, carry again
Filter residue being added 4 times 95% ethanol by its weight, mix, is that 48 ℃, microwave power are to keep 15min under the condition of 100W in temperature;
6, subdivision from
Mixture after carrying is again sent into whizzer, under 1000 rev/mins, 40 ℃ of conditions of temperature, filters with 200 order filter bags, liquor B;
7, concentrate
Merge A, B filtrate, under the condition of vacuum tightness 0.075MPa, 57 ℃ of Heating temperatures, 12 rev/mins of stirring velocitys, concentrate, exhausted until ethanol;
8, cooling
Concentrated material is cooled to room temperature under the condition of 27 ℃ of temperature of cooling water, 8 rev/mins of stirring velocitys, gets the Fructus Amomi oil resin.
The yield of the Fructus Amomi oil resin of above method preparation is 8.2%, resulting Fructus Amomi oil resin adopts gas chromatography-mass spectrography analysis flavor compound wherein, preceding four compounds that content is the highest are followed successively by: retention time reaches 48.12% at 15.70 compound (±) camphor relative content, retention time is 36.12% at 23.85 compound dl-Bornyl Acetate relative content, retention time is 5.37% at compound R-cloves alkene relative content of 31.26, and retention time is 1.84% at 16.95 compound borneol relative content.
Embodiment 2
The method of the preparing cardamon oil resin through microwave assistance that the embodiment of the invention 2 provides may further comprise the steps:
1, pulverizes
Under 54 ℃ of temperature, amomum powder is broken to 60 orders;
2, soak
Amomum powder by weight: 95% ethanol=mix at 1: 5.0, soaked 20 minutes;
3, extract
Mixture after soaking is sent into extractor, is that 55 ℃, microwave power are to keep 15min under the condition of 300W in temperature;
4, separate
Mixture is sent into whizzer, under 1200 rev/mins, 45 ℃ of conditions of temperature, filters with 400 order filter bags, filter residue and filtrate A;
5, concentrate
Filtrate A is concentrated under the condition of vacuum tightness 0.08MPa, 55 ℃ of Heating temperatures, 12 rev/mins of stirring velocitys, exhausted until ethanol;
6, cooling
Concentrated material is cooled to room temperature under the condition of 20 ℃ of temperature of cooling water, 10 rev/mins of stirring velocitys, gets the Fructus Amomi oil resin.
The yield that above method is extracted the Fructus Amomi oil resin is 8.7%, resulting Fructus Amomi oil resin adopts gas chromatography-mass spectrometry analysis flavor compound wherein, preceding four compounds that content is the highest are followed successively by: retention time reaches 50.22% at 15.70 compound (±) camphor relative content, retention time is 34.35% at 23.85 compound dl-Bornyl Acetate relative content, retention time is 3.45% at compound R-cloves alkene relative content of 31.26, and retention time is 1.11% at 16.95 compound borneol relative content.
Embodiment 3
The method of the preparing cardamon oil resin through microwave assistance that the embodiment of the invention 3 provides may further comprise the steps:
1, pulverizes
Under 40 ℃ of temperature, amomum powder is broken to 40 orders;
2, soak
Amomum powder by weight: 95% ethanol=mix at 1: 4.5, soaked 12 minutes;
3, extract
Mixture after soaking is sent into extractor, is that 50 ℃, microwave power are to keep 12min under the condition of 150W in temperature;
4, separate
Mixture is sent into whizzer, under 1000 rev/mins, 45 ℃ of conditions of temperature, filters with 300 order filter bags, filter residue and filtrate A;
5, carry again for the first time
Filter residue being added 3.6 times 95% ethanol by its weight, mix, is that 52 ℃, microwave power are to keep 10min under the condition of 200W in temperature;
6, first subdivision from
Mixture after carrying is again for the first time sent into whizzer, under 1200 rev/mins, 55 ℃ of conditions of temperature, filters with 400 order filter bags, filter residue and liquor B;
7, carry again once more
Multiple isolating filter residue for the first time being added 4 times 95% ethanol by its weight, mix, is that 50 ℃, microwave power are to keep 15min under the condition of 200W in temperature;
8, once more subdivision from
Mixture after carrying is again once more sent into whizzer, under 1200 rev/mins, 50 ℃ of conditions of temperature, filters with 300 order filter bags, liquor C;
9, concentrate
Merge A, B, C filtrate, under the condition of vacuum tightness 0.085MPa, 60 ℃ of Heating temperatures, 12 rev/mins of stirring velocitys, concentrate, exhausted until ethanol;
10, cooling
Concentrated material is cooled to room temperature under the condition of 25 ℃ of temperature of cooling water, 10 rev/mins of stirring velocitys, gets the Fructus Amomi oil resin.
The yield that above method is extracted the Fructus Amomi oil resin is 6%, resulting Fructus Amomi oil resin adopts gas chromatography-mass spectrometry analysis flavor compound wherein, preceding four compounds that content is the highest are followed successively by: retention time reaches 45.66% at 15.70 compound (±) camphor relative content, retention time is 33.21% at 23.85 compound dl-Bornyl Acetate relative content, retention time is 7.21% at compound R-cloves alkene relative content of 31.26, and retention time is 3.11% at 16.95 compound borneol relative content.
Claims (8)
1. the method for a preparing cardamon oil resin through microwave assistance is characterized in that may further comprise the steps:
(1) pulverizes: under 35～57 ℃ of temperature, dry sand benevolence is crushed to 30～60 orders;
(2) soak: amomum powder by weight: mix 95% ethanol=1: 3.2～5.5, soaked 11～23 minutes;
(3) extract: the mixture after will soaking is sent into extractor, is that 45～72 ℃, microwave power are to keep 7～15min under the condition of 100～300W in temperature;
(4) separate: mixture is sent into whizzer, under 800～1200 rev/mins, 35～65 ℃ of conditions of temperature, filter with 200～400 order filter bags, must filter residue and filtrate A;
(5) carry again: filter residue being added 3.5～6 times 95% ethanol by its weight, mix, is that 45～72 ℃, microwave power are to keep 10～18min under the condition of 100～300W in temperature;
(6) subdivision from: the mixture after will carrying is again sent into whizzer, filter under 800～1200 rev/mins, 35～65 ℃ of conditions of temperature with 200～400 order filter bags, liquor B;
(7) concentrate: merge A, B filtrate, under the condition of vacuum tightness 0.06～0.085MPa, 45～67 ℃ of Heating temperatures, 8～14 rev/mins of stirring velocitys, concentrate, exhausted until ethanol;
(8) cooling: will concentrate material and under the condition of 20～30 ℃ of temperature of cooling water, 8～14 rev/mins of stirring velocitys, be cooled to room temperature, and get the Fructus Amomi oil resin.
2. the method for preparing cardamon oil resin through microwave assistance according to claim 1 is characterized in that used dry sand benevolence is for passing through nature or physical method exsiccant fructus amomi, its moisture mass percent≤7%.
3. the method for preparing cardamon oil resin through microwave assistance according to claim 1 is characterized in that the used equipment of step (1) is the tooth-like pulverizer of band refrigerative.
4. the method for preparing cardamon oil resin through microwave assistance according to claim 1 is characterized in that step (3), the used equipment of step (5) are the microwave-assisted extractor of belt stirrer.
5. the method for preparing cardamon oil resin through microwave assistance according to claim 1 is characterized in that step (4), the used equipment of step (6) are the link-suspended basket centrifuge of adding a cover.
6. the method for preparing cardamon oil resin through microwave assistance according to claim 1 is characterized in that the used equipment of step (7) is the vacuum concentrator of belt stirrer.
7. the method for preparing cardamon oil resin through microwave assistance according to claim 1 is characterized in that the used equipment of step (8) is the cooling tank of belt stirrer.
8. the method for preparing cardamon oil resin through microwave assistance according to claim 1, it is characterized in that as required that step (5), step (6) repeat for the third time again or more times extraction with separate, or do not carry out this two step and only once extract and separate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010157988 CN101818098A (en) | 2010-04-21 | 2010-04-21 | Method for preparing cardamon oil resin through microwave assistance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010157988 CN101818098A (en) | 2010-04-21 | 2010-04-21 | Method for preparing cardamon oil resin through microwave assistance |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101818098A true CN101818098A (en) | 2010-09-01 |
Family
ID=42653377
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010157988 Pending CN101818098A (en) | 2010-04-21 | 2010-04-21 | Method for preparing cardamon oil resin through microwave assistance |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101818098A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311870A (en) * | 2011-08-30 | 2012-01-11 | 南昌大学 | Method for extracting tea oil, |
| CN102669679A (en) * | 2012-05-11 | 2012-09-19 | 广东汇香源生物科技股份有限公司 | Method for preparing chrysanthemum morifolium ramat extract in microwave-assisted way |
| CN112023442A (en) * | 2020-10-23 | 2020-12-04 | 湖北中烟工业有限责任公司 | Preparation method and application of allspice extract |
| CN112608795A (en) * | 2020-11-26 | 2021-04-06 | 福建中特药业有限公司 | Fructus amomi leaf oil and water extraction-low-temperature pressure-swing extraction process method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1420121A (en) * | 2002-05-31 | 2003-05-28 | 云南中科生物产业有限公司 | Mtehod for microwave extracting nimbin from nim kernel |
| CN101067104A (en) * | 2007-06-06 | 2007-11-07 | 广州大学 | Process of extracting amomum oil resin from spring amomum fruit |
-
2010
- 2010-04-21 CN CN 201010157988 patent/CN101818098A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1420121A (en) * | 2002-05-31 | 2003-05-28 | 云南中科生物产业有限公司 | Mtehod for microwave extracting nimbin from nim kernel |
| CN101067104A (en) * | 2007-06-06 | 2007-11-07 | 广州大学 | Process of extracting amomum oil resin from spring amomum fruit |
Non-Patent Citations (3)
| Title |
|---|
| 《中国中药杂志》 20040229 张英等 中草药和天然植物有效成分提取新技术--微波协助萃取》 104-108 第29卷, 第2期 2 * |
| 《食品工业科技》 20081231 魏荣华等 微波提取条件与春砂仁挥发成分的机构分布关系的研究 90-93 , 第2期 2 * |
| 《食品科学》 20051231 樊亚鸣等 微波法萃取春砂仁中低级性油树脂的研究 177-180 第26卷, 第8期 2 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311870A (en) * | 2011-08-30 | 2012-01-11 | 南昌大学 | Method for extracting tea oil, |
| CN102311870B (en) * | 2011-08-30 | 2013-03-13 | 南昌大学 | Method for extracting tea oil, |
| CN102669679A (en) * | 2012-05-11 | 2012-09-19 | 广东汇香源生物科技股份有限公司 | Method for preparing chrysanthemum morifolium ramat extract in microwave-assisted way |
| CN112023442A (en) * | 2020-10-23 | 2020-12-04 | 湖北中烟工业有限责任公司 | Preparation method and application of allspice extract |
| CN112608795A (en) * | 2020-11-26 | 2021-04-06 | 福建中特药业有限公司 | Fructus amomi leaf oil and water extraction-low-temperature pressure-swing extraction process method thereof |
| CN112608795B (en) * | 2020-11-26 | 2023-11-07 | 福建中特药业有限公司 | Fructus amomi leaf oil and water extraction-low-temperature pressure transformation extraction process method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103283865B (en) | Preparation method of healthcare red oil and healthcare red oil prepared by same | |
| CN103251025A (en) | Spice seasoning and preparation method thereof | |
| CN106107268B (en) | Fruit juice antipyretic beverage and its preparation process | |
| CN104095093A (en) | Honeysuckle health-care tea and preparation method thereof | |
| CN101818098A (en) | Method for preparing cardamon oil resin through microwave assistance | |
| CN102964866A (en) | Method for extracting perilla color from perilla leaves | |
| CN106176878A (en) | The extracting method of Radix Codonopsis extract | |
| CN105725143A (en) | Royal jelly lozenge | |
| CN101982191A (en) | Method for extracting fat-reducing compound functional materials from lotus leaves | |
| CN104621659A (en) | Preparation method of rose ultrafine powder | |
| CN101628857B (en) | Production technique for extracting resveratrol from giant knotweed | |
| CN104161987A (en) | Traditional Chinese medicinal composition for lipid and sugar reduction, and its application | |
| CN103409278A (en) | Preparation method of nutritional rice wine | |
| CN105613829A (en) | Instant health tea and preparation method thereof | |
| CN104997099A (en) | Heat clearing and dampness reducing health-care beverage and preparation method thereof | |
| CN102061219A (en) | Method for extracting tea seed oil | |
| CN103695179A (en) | Production process method of cinnamon volatile oil | |
| CN103146474A (en) | Method for preparing anise resin and seasoning oil thereof | |
| KR20060093145A (en) | Extraction method of grape seed oil by supercritical fluid extraction | |
| CN103283848A (en) | Milk tablet containing sweet potato extract and preparation method thereof | |
| CN103525539B (en) | Method for preparing chili seed oil with stable spicy fragrance | |
| CN106720637A (en) | One kind is relieved inflammation or internal heat nti-freckle tealeaves and its preparation technology | |
| CN102669679B (en) | Method for preparing chrysanthemum morifolium ramat extract in microwave-assisted way | |
| CN105969632A (en) | Processing method of vitex negundo leaf composite tea vinegar | |
| CN106333023A (en) | Ganoderma-linearstripe rabdosia teabag and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100901 |