CN106433988A - Extraction method of cinnamon spices - Google Patents
Extraction method of cinnamon spices Download PDFInfo
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- CN106433988A CN106433988A CN201610958879.XA CN201610958879A CN106433988A CN 106433988 A CN106433988 A CN 106433988A CN 201610958879 A CN201610958879 A CN 201610958879A CN 106433988 A CN106433988 A CN 106433988A
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- Prior art keywords
- cinnamon
- petroleum ether
- ether solution
- spices
- extracting
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Seasonings (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses an extraction method of cinnamon spices. The extraction method comprises the following steps: firstly drying and chopping cinnamon, distilling cinnamon oil with water vapor and meanwhile obtaining solid residues, wherein the cinnamon oil is used for making high-grade spices; adding solid residue raw materials into a petroleum ether solution with a volume percentage of 70-80 percent for soaking, and refluxing and extracting for three times by using a soxhlet reflux device, wherein the mass of the petroleum ether solution added for the first time is 8-10 times of that of the solid residue raw materials, and the mass of the petroleum ether solution added for the second time and the third time is 1-2 times of that of the solid residue raw materials; decompressing and concentrating an extracting solution to obtain an extract, dissolving the extract in ethanol, adding activated carbon to stir, putting at a normal temperature, filtering and recovering the ethanol to obtain the cinnamon spices. The spices can be used as high-grade cosmetics. The extraction method disclosed by the invention is simple in process, simple in production steps, low in production cost, free from environmental problems and suitable for large-scale production. Compared with those of a traditional method, the extraction rate can be improved by 20 percent, and the purity can be improved by 30 percent.
Description
Technical field
The present invention relates to chemical industry extractive technique field, specifically a kind of extracting method of cinnamon flavor.
Background technology
Cortex Cinnamomi,【Classification system】Cinnamomum cassia Presl,【Another name】Beautiful osmanthus, male osmanthus, cajaput, great Gui, peppery
Osmanthus, safety tree, cassia, are the dry bark of canella Cortex Cinnamomi.Bark fragrance, can make spice, taste with originate from Si Lilan
The Cortex cinnamomi japonici (Ramulus Cinnamomi) of card Cortex Cinnamomi is similar, but pepperyyer, delicious not as good as Cortex cinnamomi japonici (Ramulus Cinnamomi), and thick compared with Cortex cinnamomi japonici (Ramulus Cinnamomi).
Cortex Cinnamomi strips from stem and branch, shelves after being dried, crimps rolling.Some kinds are then scraping.Scrape taker thin and
For azarin brown, the bark do not scraped is thick and be Lycoperdon polymorphum Vitt.Cortex Cinnamomi powder light reddish brown color.In domestic Cortex Cinnamomi fragrance be slightly poorer than Vietnam and
Indonesia product person, three all has fragrance, and taste is sweet and peppery.Chinese cinnamon and male osmanthus(C. loureirii)Immature fruit
, in firmly and in the taupe cup-shaped calyx having wrinkle, generally long 11 is public for adhesion(0.4, including calyx tube);Top footpath about 6 is public
(0.25), connect calyx tube and take dry i.e. title Cortex Cinnamomi bud.There is the sweet pungent of fragrance like Cortex cinnamomi japonici (Ramulus Cinnamomi) and Cortex Cinnamomi, adjust for food
Taste.Cortex cinnamomi japonici (Ramulus Cinnamomi) 1.98%-2.06% containing volatile oil, its main component is cinnamic aldehyde(cinnamaldehyde), account for 52.92%-
61.20%, also acetic acid cassia bark ester(cinnamyl acetate), ethyl cinnamate(ethylcinnamate), benzyl benzoate
(benzyl benzoate), benzaldehyde(benzaldehyde), coumarin(coumarin), β-cadinene(β-
cadinene), Rhizoma Acori Graminei alkene(calamenene), beta-elemene(β-elemane), protocatechuic acid(protocatechuic
acid), trans isomer cinnamic acid(transcinnamic acid)Deng.
Extraction process with regard to Cortex Cinnamomi retrieves following patent:
1st, Chinese patent, application number:201110406279.X;Applicant:Guangxi Sheng Baotang pharmaceutcal corporation, Ltd;Address:Guangxi
Nanning City of Zhuang autonomous region high and new technology industrial development zone innovation West Road 13;Denomination of invention:A kind of method extracting Oleum Cinnamomi;Summary:This
Bright provide a kind of from Cortex Cinnamomi be dried branch and leaf extract Oleum Cinnamomi method.The method can shorten extraction time, improve oily
Rate, reducing energy consumption, reduces production cost simultaneously.This technique is:Make the leaching adjuvant of steam distillation of surfactant,
Accelerate water-wet cinnamon leaf surface using the moistening of surfactant, infiltration, solubilization, infiltrate through plant cell, plant
The quintessence oil of thing cell interior takes extracellular out of, obtains the exchange of system heat energy simultaneously, forms azeotropic with vapor, is together steamed
Go out, obtain Oleum Cinnamomi through condensation, cooling, centrifugation.This method is short because of distillation time, it is to avoid long-time heating and cause
The change of the thermal sensitivity chemical composition in quintessence oil, it also avoid making plant material coking because overheated and affects the fragrance of quintessence oil.
Products obtained therefrom paler colour, fragrance is purer, no the smell of burning.
2nd, Chinese patent, application number:201210518928.X;Applicant:Guangxi Jing Gui spice company limited;Address:Extensively
Western Zhuang autonomous region Wuzhou Teng County spark industrial park Xijing osmanthus spice company limited;Denomination of invention:Natural cinnamon oil extract work
Process;Summary:The invention discloses a kind of natural cinnamon oil process for extracting, it is related to forest chemical technical field, it is
Natural cinnamon oil is extracted with method according to the following steps using natural cinnamon oil extraction equipment:Cinnamon leaf is put into two distillations
In kettle, then water vapour is sprayed into the bottom of first distillating still, the mixed vapour of the generation top through first distillating still is defeated
Enter the bottom of second distillating still, the input multiple distillating still in top through second distillating still for the mixed vapour makees the heat of distillation distillate
Source, the condensed device condensation of multiple distillating still top mixed vapour out;Distillate enters oil water separator and carries out oil-water separation,
The distillate separated carries out multiple distillation by the multiple distillating still of pump input;Remaining waste in multiple distillating still is transported to first
Distillating still, upper once distillation is carried out when more multiple distillation once discharge afterwards.The present invention can solve distillation extracting natural Oleum Cinnamomi
When Oleum Cinnamomi output capacity low, the high problem of production cost.
3rd, Chinese patent, application number:87107543.1;Applicant:Guangzhou Inst of Chemistry, Chinese Academy of Sciences;Invention name
Claim:Straight run distillation cinnamon leaf extracts Oleum Cinnamomi;Summary:The invention belongs to vapor distillation extracts aromatic plant extract oil process.
Feature is to distill cinnamon leaf using boiler steam supply live (open) steam, and carries out mechanical activation comminution before it is distilled and use sodium-chloride water solution
Soak cinnamon leaf to accelerate the effusion of oil content, and the feature being not readily separated for cassia oil with water, there is provided a kind of shell and tube table
The big oil distribution device of area.The new technology that the present invention provides, improves 50-100%, cassia oil aldehyde contenting amount than existing technique oil yield
Bring up to 97% by 90%, can achieve industrialized production using boiler steam supply, fuel thermal efficiency improves 2 times.
At present the extracting method of cinnamon flavor have remaining solid slag after vapor distillation anise-oil all to abandon, have right
Cortex Cinnamomi carries out solvent extraction etc., and the extraction ratio of these methods is very low, causes the waste to Cortex Cinnamomi resource, has document report to be faced with super
Boundary CO2Fluid extraction Cortex Cinnamomi, the method extraction ratio is of a relatively high, but high cost, be not suitable for large-scale production.
Content of the invention
The invention provides a kind of extracting method of cinnamon flavor, with vapor distillation Cortex Cinnamomi anise-oil, obtain solid simultaneously
Slag, solid slag is extracted with Soxhlet circumfluence method, activated carbon decolorizing, finally gives anistree spice, the method process is simple, simplifies
Production stage, low production cost, no environmental problem, suitable large-scale production.
A kind of extracting method of cinnamon flavor, comprises the following steps:
(1), the Cortex Cinnamomi gathering dried or dries, chopping, cross 30-60 mesh sieve, extract Oleum Cinnamomi with vapor distillation, simultaneously
Obtain solid slag, Oleum Cinnamomi is used for manufacturing high-grade spice;
(2), by solid slag raw material add volume fraction be 70-80% petroleum ether solution soak, use cable type extractor according reflux, extract,
Three times, temperature is 60-85 DEG C, and the quality adding for the first time petroleum ether solution is 8-10 times of solid slag raw material, and extraction time is
60-90min, after add the quality of petroleum ether solution to be 2-4 times of solid slag raw material twice, extraction time is 20-30min,
Filter and merge, obtain extracting solution and phase analysis, extracting solution concentrating under reduced pressure obtains the paste that water content is 5%;
(3), by step(2)Middle gained water content is 5% paste volume fraction is that the ethanol solution of 80-90% soaks again
Bubble, and add activated carbon to stir, room temperature filters after placing 24h, obtains light spice, reclaims ethanol, obtains cinnamon flavor.
Above step(1)Described in dry method can be dried with firewood or Linesless charcoal.
Above step(2)Described in phase analysis break into powder after, can be used as the perfume additive in medicated cigarette.
Above step(3)Described in cinnamon flavor can serve as superior cosmetics or medical material.
Advantage of the invention is that:
(1)Cortex Cinnamomi first distills Oleum Cinnamomi, obtains fine perfumery raw material, and remaining solid slag makes full use of, and all of spice is become
Divide and all reclaim.
(2)Solid slag raw material is added the petroleum ether solution that volume fraction is 70-80% to soak, using apparatus,Soxhlet'ses
Complete this law operation, compensate in conventional backflow extraction method that solvent-oil ratio is big, the deficiency of troublesome poeration.Extraction time is short, steady
Qualitative high, extraction efficiency height, saving solvent.
(3)The inventive method compares supercritical CO2Fluid extraction is more economical, simple to operate easily controllable, with biography
System method is compared, and extraction ratio can improve 20%, and purity can improve 30%.
Specific embodiment
Embodiment 1
The Cortex Cinnamomi gathering 500g is dried or dries, chopping, cross 30-60 mesh sieve, extract Oleum Cinnamomi with vapor distillation, simultaneously
Obtain solid slag, Oleum Cinnamomi is used for manufacturing high-grade spice;The petroleum ether solution that solid slag addition volume fraction is 70% is soaked,
With cable type extractor according reflux, extract, three times, first time reflux temperature is 60 DEG C, and the quality adding petroleum ether solution is 4000g, carries
Take the time to be 60min, the twice reflux temperature be 70 DEG C, add quality 1000g of petroleum ether solution, extraction time is 20min,
Third time reflux temperature is 80 DEG C, adds quality 2000g of petroleum ether solution, and extraction time is 30min, filters and merges, must carry
Take liquid and phase analysis, extracting solution concentrating under reduced pressure obtains the paste that water content is 5%;The paste volume that above-mentioned water content is 5%
Fraction is that 85% ethanol solution soaks again, and adds activated carbon to stir, and room temperature filters after placing 24h, obtains light spice,
Reclaim ethanol, obtain cinnamon flavor.
Embodiment 2
The Cortex Cinnamomi gathering 500g is dried or dries, chopping, cross 30-60 mesh sieve, extract Oleum Cinnamomi with vapor distillation, simultaneously
Obtain solid slag, Oleum Cinnamomi is used for manufacturing high-grade spice;The petroleum ether solution that solid slag addition volume fraction is 80% is soaked,
With cable type extractor according reflux, extract, three times, first time reflux temperature is 60 DEG C, and the quality adding petroleum ether solution is 5000g, carries
Take the time to be 90min, the twice reflux temperature be 70 DEG C, add quality 1500g of petroleum ether solution, extraction time is 20min,
Third time reflux temperature is 85 DEG C, adds quality 2000g of petroleum ether solution, and extraction time is 20min, filters and merges, must carry
Take liquid and phase analysis, extracting solution concentrating under reduced pressure obtains the paste of water content 5%;The paste volume integral that above-mentioned water content is 5%
The ethanol solution for 80% for the number soaks again, and adds activated carbon to stir, and room temperature filters after placing 24h, obtains light spice, returns
Receive ethanol, obtain cinnamon flavor.
Embodiment 3
The Cortex Cinnamomi gathering 500g is dried or dries, chopping, cross 30-60 mesh sieve, extract Oleum Cinnamomi with vapor distillation, simultaneously
Obtain solid slag, Oleum Cinnamomi is used for manufacturing high-grade spice;The petroleum ether solution that solid slag addition volume fraction is 70% is soaked,
With cable type extractor according reflux, extract, three times, first time reflux temperature is 70 DEG C, and the quality adding petroleum ether solution is 4500g, carries
Take the time to be 70min, the twice reflux temperature be 70 DEG C, add quality 1000g of petroleum ether solution, extraction time is 25min,
Third time reflux temperature is 85 DEG C, adds quality 1500g of petroleum ether solution, and extraction time is 30min, filters and merges, must carry
Take liquid and phase analysis, extracting solution concentrating under reduced pressure obtains the paste of water content 5%;The paste volume integral that above-mentioned water content is 5%
The ethanol solution for 90% for the number soaks again, and adds activated carbon to stir, and room temperature filters after placing 24h, obtains light spice, returns
Receive ethanol, obtain cinnamon flavor.
Claims (4)
1. a kind of extracting method of cinnamon flavor it is characterised in that:Comprise the following steps:
(1)The Cortex Cinnamomi gathering is dried or dries, chopping, cross 30-60 mesh sieve, extract Oleum Cinnamomi with vapor distillation, simultaneously
Obtain solid slag, Oleum Cinnamomi is used for manufacturing high-grade spice;
(2)Solid slag raw material is added the petroleum ether solution that volume fraction is 70-80% to soak, uses cable type extractor according reflux, extract,
Three times, temperature is 60-85 DEG C, and the quality adding for the first time petroleum ether solution is 8-10 times of solid slag raw material, and extraction time is
60-90min, after add the quality of petroleum ether solution to be 2-4 times of solid slag raw material twice, extraction time is 20-30min,
Filter and merge, obtain extracting solution and phase analysis, extracting solution concentrating under reduced pressure obtains the paste that water content is 5%;
(3)By step(2)Middle gained water content is 5% paste volume fraction is that the ethanol solution of 80-90% soaks again,
And adding activated carbon to stir, room temperature filters after placing 24h, obtains light spice, reclaims ethanol, obtains cinnamon flavor.
2. cinnamon flavor according to claim 1 extracting method it is characterised in that:Step(1)Described in dry side
Method is dried with firewood or Linesless charcoal.
3. cinnamon flavor according to claim 1 extracting method it is characterised in that:Step(2)Described in phase analysis beat
Cheng Fenhou, as the perfume additive in medicated cigarette.
4. cinnamon flavor according to claim 1 extracting method it is characterised in that:Step(3)Described in Cortex Cinnamomi fragrant
Material is used as superior cosmetics or medical material.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107308400A (en) * | 2017-07-05 | 2017-11-03 | 张军 | Application of the fat oil in treatment baby diarrhea navel paster is prepared in antidiarrheal prescription |
CN113403135A (en) * | 2021-06-03 | 2021-09-17 | 贵州新农汇生态农业发展有限公司 | Comprehensive processing method of dried ginger slices and ginger oil |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107308400A (en) * | 2017-07-05 | 2017-11-03 | 张军 | Application of the fat oil in treatment baby diarrhea navel paster is prepared in antidiarrheal prescription |
CN113403135A (en) * | 2021-06-03 | 2021-09-17 | 贵州新农汇生态农业发展有限公司 | Comprehensive processing method of dried ginger slices and ginger oil |
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