CN106397166A - Method for extracting cinnamaldehyde from cinnamomum cassia presl - Google Patents
Method for extracting cinnamaldehyde from cinnamomum cassia presl Download PDFInfo
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- CN106397166A CN106397166A CN201610797116.1A CN201610797116A CN106397166A CN 106397166 A CN106397166 A CN 106397166A CN 201610797116 A CN201610797116 A CN 201610797116A CN 106397166 A CN106397166 A CN 106397166A
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- Prior art keywords
- cortex cinnamomi
- extracting
- ramulus cinnamomi
- ethanol
- cinnamic aldehyde
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/79—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Seasonings (AREA)
Abstract
The invention relates to the field of extraction and preparation of spices, in particular to a method for extracting cinnamaldehyde from cinnamomum cassia presl. The method comprises the following steps: crushing cinnamomum cassia presl, extracting with ethanol, enzymolysis and inactivation, flocculent-precipitating, chromatographic refining, crystallizing and recrystallizing, and vacuum-drying a crystal to obtain a finished product and cinnamaldehyde in the finished product. According to the method for extracting cinnamaldehyde from cinnamomum cassia presl provided by the invention, the physicochemical property characteristics of cinnamaldehyde and coexisting impurities are fully combined, a route of flocculation and alumina chromatography firstly and then crystallization and recrystallization is adopted, the working procedure of secondary decoloring through active carbon adopted by a conventional method is eliminated; the production operation is saved, for example, the links of heat preservation and microporous membrane filtration are eliminated; the color of the finished product is also improved; high-quality cinnamaldehyde is produced.
Description
Technical field
The present invention relates to spice extract preparation field and in particular to a kind of from Cortex cinnamomi japonici (Ramulus Cinnamomi) extract cinnamic aldehyde method.
Background technology
Cortex cinnamomi japonici (Ramulus Cinnamomi) is one of the most frequently used natural flavouring, and Cortex cinnamomi japonici (Ramulus Cinnamomi) contains ethereal oil 1%～2%, is yellow or yellowish-brown
Supernatant liquid, has the special fragrance of Cortex Cinnamomi, and taste is sweet, pungent, and dew is put in the air or deposited with the passing of time, and color gradual change is deep, and matter is gradually thick.Cortex cinnamomi japonici (Ramulus Cinnamomi)
Oil has sterilization, antioxidation.The food synthetic perfume allowing to use that cinnamic aldehyde specifies for GB2076-2011, can be used for
Prepare meat, flavoring agent, oral care implement, chewing gum, confection essence.The method that tradition extracts cinnamic aldehyde, extraction ratio is low.
Content of the invention
The present invention provides a kind of extraction ratio high cinnamic aldehyde extracting method.
The technical solution adopted in the present invention is：
A kind of method extracting cinnamic aldehyde from Cortex cinnamomi japonici (Ramulus Cinnamomi), comprises the following steps：
(1) Cortex cinnamomi japonici (Ramulus Cinnamomi) is crushed to by No. 1 sieve >=70%；
(2) ethanol extraction；Add 60% ethanol of 5～6 times of Cortex cinnamomi japonici (Ramulus Cinnamomi) weight；Extract three times, each 1-2 hour；
(3) concentrate and reclaim ethanol；3 Cortex cinnamomi japonici (Ramulus Cinnamomi) extracting solution are pressed prior art and reclaims ethanol to no alcohol taste, be concentrated into phase
To density 1.15 about.
(4) enzymolysis and inactivation：Cortex cinnamomi japonici (Ramulus Cinnamomi) extraction concentrated solution is cooled to 45 DEG C～50 DEG C, within 45 DEG C～50 DEG C；Add
The pH value that citric acid adjusts concentrated solution is 4.5～5.0, adds Cortex cinnamomi japonici (Ramulus Cinnamomi) weight 0.2%～0.5% cellulase 45 DEG C～50
DEG C constant temperature digests 4～5 days；It is warming up to 85-100 DEG C, maintain 2 minutes, by enzyme-deactivating；Filter, filtering residue is thick through conversion
Product cinnamic aldehyde；
(5) flocculation sediment：Crude product cinnamic aldehyde is dissolved with 65%～85% ethanol, filters；Add crude product cinnamic aldehyde weight in wet base
0.8～1.0 times of flocculant, is sufficiently stirred for 10min, then stands 2h, so that precipitation is fully precipitated, and supernatant layering is good；Cross
Filter, obtains filtrate；
(6) chromatograph and refine：Filtrate is entered alumina chromatographic column, own liquid starts when flowing out to collect；Liquid is carried out point
Section, from flow out red to during black liquor change alumina column；After whole filtrates have entered alumina column, then with 65%～
85% ethanol elution, is eluted to effluent always and adds 2 times of water and do not produce muddiness and stop；
(7) crystallization and recrystallization：Effluent on alumina column is added water and is crystallized and recrystallization, adjust concentration of alcohol
For 10%～20%, standing 1h, then filter, recrystallization, till crystallization color is pure white；
(8) crystallization is vacuum dried to obtain finished product, cinnamic aldehyde in finished product.
Described flocculant, following components is constituted according to weight portion：Silica gel 30-45, aluminium oxide 25-40, activated carbon 15-
30.
Compared with the prior art, beneficial effects of the present invention are as follows：
A kind of method extracting cinnamic aldehyde from Cortex cinnamomi japonici (Ramulus Cinnamomi) that the present invention provides, fully combines cinnamic aldehyde and coexistent impurity
Physicochemical property feature, using first flocculation, alumina column chromatography, then recrystallization and the route of recrystallization, eliminate conventional method institute
Using activated carbon carry out the operation of secondary decolourization, not only save production operation, such as save insulation and micro-pore-film filtration link,
Also so that finished color is improved, produce the cinnamic aldehyde of high-quality.
Specific embodiment
The present invention is further illustrated with reference to embodiments, but the present invention is not limited only to these embodiments, not
On the premise of departing from present inventive concept, any improvement made is within the scope of the present invention.
A kind of method extracting cinnamic aldehyde from Cortex cinnamomi japonici (Ramulus Cinnamomi), comprises the following steps：
(1) Cortex cinnamomi japonici (Ramulus Cinnamomi) is crushed to by No. 1 sieve >=70%；
(2) ethanol extraction；Add 60% ethanol of 5～6 times of Cortex cinnamomi japonici (Ramulus Cinnamomi) weight；Extract three times, each 1-2 hour；
(3) concentrate and reclaim ethanol；3 Cortex cinnamomi japonici (Ramulus Cinnamomi) extracting solution are pressed prior art and reclaims ethanol to no alcohol taste, be concentrated into phase
To density 1.15 about.
(4) enzymolysis and inactivation：Cortex cinnamomi japonici (Ramulus Cinnamomi) extraction concentrated solution is cooled to 45 DEG C～50 DEG C, within 45 DEG C～50 DEG C；Add
The pH value that citric acid adjusts concentrated solution is 4.5～5.0, adds Cortex cinnamomi japonici (Ramulus Cinnamomi) weight 0.2%～0.5% cellulase 45 DEG C～50
DEG C constant temperature digests 4～5 days；It is warming up to 85-100 DEG C, maintain 2 minutes, by enzyme-deactivating；Filter, filtering residue is thick through conversion
Product cinnamic aldehyde；
(5) flocculation sediment：Crude product cinnamic aldehyde is dissolved with 65%～85% ethanol, filters；Add crude product cinnamic aldehyde weight in wet base
0.8～1.0 times of flocculant, is sufficiently stirred for 10min, then stands 2h, so that precipitation is fully precipitated, and supernatant layering is good；Cross
Filter, obtains filtrate；
(6) chromatograph and refine：Filtrate is entered alumina chromatographic column, own liquid starts when flowing out to collect；Liquid is carried out point
Section, from flow out red to during black liquor change alumina column；After whole filtrates have entered alumina column, then with 65%～
85% ethanol elution, is eluted to effluent always and adds 2 times of water and do not produce muddiness and stop；
(7) crystallization and recrystallization：Effluent on alumina column is added water and is crystallized and recrystallization, adjust concentration of alcohol
For 10%～20%, standing 1h, then filter, recrystallization, till crystallization color is pure white；
(8) crystallization is vacuum dried to obtain finished product, cinnamic aldehyde in finished product.
Described flocculant, following components is constituted according to weight portion：Silica gel 30-45, aluminium oxide 25-40, activated carbon 15-
30.
Claims (2)
1. a kind of method of cinnamic aldehyde of extracting from Cortex cinnamomi japonici (Ramulus Cinnamomi) is it is characterised in that comprise the following steps：
(1) Cortex cinnamomi japonici (Ramulus Cinnamomi) is crushed to by No. 1 sieve >=70%；
(2) ethanol extraction；Add 60% ethanol of 5～6 times of Cortex cinnamomi japonici (Ramulus Cinnamomi) weight；Extract three times, each 1-2 hour；
(3) concentrate and reclaim ethanol；3 Cortex cinnamomi japonici (Ramulus Cinnamomi) extracting solution are pressed prior art and reclaims ethanol to no alcohol taste, be concentrated into relatively close
Degree 1.15 about.
(4) enzymolysis and inactivation：Cortex cinnamomi japonici (Ramulus Cinnamomi) extraction concentrated solution is cooled to 45 DEG C～50 DEG C, within 45 DEG C～50 DEG C；Add Fructus Citri Limoniae
The pH value that acid adjusts concentrated solution is 4.5～5.0, adds Cortex cinnamomi japonici (Ramulus Cinnamomi) weight 0.2%～0.5% cellulase in 45 DEG C～50 DEG C perseverances
Temperature enzymolysis 4～5 days；It is warming up to 85-100 DEG C, maintain 2 minutes, by enzyme-deactivating；Filter, filtering residue is the crude product osmanthus through conversion
Skin aldehyde；
(5) flocculation sediment：Crude product cinnamic aldehyde is dissolved with 65%～85% ethanol, filters；Add crude product cinnamic aldehyde weight in wet base 0.8～
1.0 times of flocculant, is sufficiently stirred for 10min, then stands 2h, so that precipitation is fully precipitated, and supernatant layering is good；Filter, obtain
Filtrate；
(6) chromatograph and refine：Filtrate is entered alumina chromatographic column, own liquid starts when flowing out to collect；Liquid is carried out segmentation, from
Flow out red to during black liquor change alumina column；After whole filtrates have entered alumina column, then with 65%～85% second
Alcohol eluting, is eluted to effluent always and adds 2 times of water and do not produce muddiness and stop；
(7) crystallization and recrystallization：Effluent on alumina column is added water and is crystallized and recrystallization, adjusting concentration of alcohol is
10%～20%, stand 1h, then filter, recrystallization, till crystallization color is pure white；
(8) crystallization is vacuum dried to obtain finished product, cinnamic aldehyde in finished product.
2. according to claim 1. a kind of method extracting cinnamic aldehyde from Cortex cinnamomi japonici (Ramulus Cinnamomi) is it is characterised in that described flocculation
Agent, following components is constituted according to weight portion：Silica gel 30-45, aluminium oxide 25-40, activated carbon 15-30.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610797116.1A CN106397166A (en) | 2016-08-31 | 2016-08-31 | Method for extracting cinnamaldehyde from cinnamomum cassia presl |
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| CN201610797116.1A CN106397166A (en) | 2016-08-31 | 2016-08-31 | Method for extracting cinnamaldehyde from cinnamomum cassia presl |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI691355B (en) * | 2019-08-02 | 2020-04-21 | 臺灣三益創價生技有限公司 | Method for extracting cinnamaldehyde-rich composition from cinnamon |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101338327A (en) * | 2008-08-13 | 2009-01-07 | 长沙华诚生物科技有限公司 | Process for extracting resveratrol with purity higher than 98 0.000000rom giant knotweed |
| CN104073360A (en) * | 2014-06-16 | 2014-10-01 | 南京泽朗医药科技有限公司 | Extraction method of cinnamon volatile oil |
-
2016
- 2016-08-31 CN CN201610797116.1A patent/CN106397166A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101338327A (en) * | 2008-08-13 | 2009-01-07 | 长沙华诚生物科技有限公司 | Process for extracting resveratrol with purity higher than 98 0.000000rom giant knotweed |
| CN104073360A (en) * | 2014-06-16 | 2014-10-01 | 南京泽朗医药科技有限公司 | Extraction method of cinnamon volatile oil |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI691355B (en) * | 2019-08-02 | 2020-04-21 | 臺灣三益創價生技有限公司 | Method for extracting cinnamaldehyde-rich composition from cinnamon |
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