CN109503329A - A kind of method of borneol camphor tree branches and leaves extraction purification - Google Patents

A kind of method of borneol camphor tree branches and leaves extraction purification Download PDF

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Publication number
CN109503329A
CN109503329A CN201811359112.0A CN201811359112A CN109503329A CN 109503329 A CN109503329 A CN 109503329A CN 201811359112 A CN201811359112 A CN 201811359112A CN 109503329 A CN109503329 A CN 109503329A
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China
Prior art keywords
camphor tree
borneol
extraction
tree branches
raw material
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Pending
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CN201811359112.0A
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Chinese (zh)
Inventor
汤佳炜
汤松法
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Huzhou Xiyuanlong Camphor Science And Technology Co Ltd
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Huzhou Xiyuanlong Camphor Science And Technology Co Ltd
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Priority to CN201811359112.0A priority Critical patent/CN109503329A/en
Publication of CN109503329A publication Critical patent/CN109503329A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/84Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2602/00Systems containing two condensed rings
    • C07C2602/36Systems containing two condensed rings the rings having more than two atoms in common
    • C07C2602/42Systems containing two condensed rings the rings having more than two atoms in common the bicyclo ring system containing seven carbon atoms

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

The invention discloses a kind of methods of borneol camphor tree branches and leaves extraction purification, including step S1: acquiring the sprig adhered in the old leaf and old leaf of camphor tree as raw material, pre-process to raw material;Step S2: pretreated raw material is added in extraction bucket, is extracted using high-temperature high-pressure overheat steam;Step S3: the natural borneol after the gasification being obtained by extraction is condensed using condenser, condensed natural borneol is purified using oil water separator;Step S4: the residue in step S2 extraction bucket is taken out, complex enzyme is added into residue, digests residue, obtains extracting solution;Step S5: extraction bucket is added in extracting solution, repeats step S2 ~ step S3.Method of the invention carries out secondary enzymolysis extraction process to the residue obtained after coarse extraction, the resin in borneol camphor tree branches and leaves is precipitated sufficiently, improve the recovery rate of natural borneol, raw material are saved, to reduce production cost on the basis of existing technology.

Description

A kind of method of borneol camphor tree branches and leaves extraction purification
Technical field
The present invention relates to plant extraction process technical field more particularly to a kind of methods of borneol camphor tree branches and leaves extraction purification.
Background technique
The method that existing borneol camphor tree branches and leaves extract is to obtain day using the method for condensation after slightly being mentioned using high temperature and pressure Right borneol.Natural borneol is good assistant indispensable in many borneol products as rare Chinese medicine medicinal material and food additives Agent.The history that natural borneol is used as drug in China is more than 1500.Studies have shown that natural borneol is proven to have anti-inflammatory work With, anti thrombotic action and excellent antioxidation.It can be used as treating chronic bronchitis, pediatric burn, change in real life Purulent otitis media etc..It is rare as extracting borneol camphor tree used in natural borneol, cause the cost of raw material high, therefore, is extracting During natural borneol, need for the resin that can be precipitated in borneol camphor tree branches and leaves to be all precipitated as far as possible, to save cost. And in the prior art, after slightly being mentioned to borneol camphor tree branches and leaves, waste residue is directly abandoned, while resulting in waste of resources, is increased Production cost.
Summary of the invention
To solve extraction natural borneol technical problem at high cost, technology of the invention proposed in above-mentioned background technique Scheme is as follows:
The method of one of present invention borneol camphor tree branches and leaves extraction purification, comprising the following steps:
Step S1: the sprig adhered in the old leaf and old leaf of camphor tree is acquired as raw material, raw material is pre-processed;
Step S2: pretreated raw material obtained by step S1 is added in extraction bucket, is extracted using high-temperature high-pressure overheat steam;
Step S3: using condenser by after the gasification being obtained by extraction natural borneol condense, using oil water separator to condensation after Natural borneol purification;
Step S4: the residue in step S2 extraction bucket is taken out, complex enzyme is added into residue, digests residue, is mentioned Take liquid;
Step S5: extraction bucket is added in extracting solution, repeats step S2 ~ step S3.
In a preferred embodiment, the pretreatment in step S1 includes cleaning, drying, crushing.
In a preferred embodiment, the partial size of smashed raw material is 1.5mm ~ 2.5mm.
In a preferred embodiment, the temperature in step S2 in extraction bucket is, pressure be 1MPa ~ 4MPa。
In a preferred embodiment, the revolving speed of the oil water separator in step S3 is 4200 revs/min.
In a preferred embodiment, the purification time in step S3 is 5min ~ 10min.
In a preferred embodiment, the complex enzyme in step S4 is the papain of equal proportion mixing, fiber Plain enzyme extracts enzyme and pectase.
In a preferred embodiment, the time of enzymolysis processing is 3h ~ 4h, and the temperature of enzymatic hydrolysis is
The method of one of present invention borneol camphor tree branches and leaves extraction purification, compared with prior art, it has the advantage that:
The method of one of present invention borneol camphor tree branches and leaves extraction purification, on the basis of existing technology, to being obtained after coarse extraction Residue carry out secondary enzymolysis extraction process, the resin in borneol camphor tree branches and leaves is precipitated sufficiently, improves the extraction of natural borneol Rate saves raw material, to reduce production cost.Meanwhile the present invention utilizes 4200 revs/min of oil water separator to natural Borneol is purified, and the purity of natural borneol is made to be increased dramatically.
Specific embodiment
Technical solution of the present invention will be clearly and completely described below.Based on the embodiments of the present invention, ability Domain those of ordinary skill every other embodiment obtained without creative efforts, belongs to guarantor of the present invention The range of shield.
A kind of method of borneol camphor tree branches and leaves extraction purification of the invention, comprising the following steps:
Step S1: the sprig adhered in the old leaf and old leaf of camphor tree is acquired as raw material, raw material is pre-processed;Wherein pre- place Reason includes cleaning, dries and crush, and the partial size of smashed raw material is 1.5mm ~ 2.5mm;
Step S2: pretreated raw material obtained by step S1 is added in extraction bucket, is extracted using high-temperature high-pressure overheat steam, is extracted The temperature in bucket is taken to be, pressure is 1MPa ~ 4MPa;
Step S3: using condenser by after the gasification being obtained by extraction natural borneol condense, using oil water separator to condensation after Natural borneol purification;Wherein the revolving speed of oil water separator is 4200 revs/min, and the purification time is 5min ~ 10min;
Step S4: taking out the residue in step S2 extraction bucket, complex enzyme be added into residue, digests residue, enzymatic hydrolysis Time is 3h ~ 4h, and the temperature of enzymatic hydrolysis is, obtain extracting solution;Wherein complex enzyme is the Papain of equal proportion mixing Enzyme, extracts enzyme and pectase at cellulase.
Step S5: extraction bucket is added in extracting solution, repeats step S2 ~ step S3.
Illustrate the advantage of the extracting method in the present invention compared with the existing technology below in conjunction with embodiment.
Comparative example
The total 100kg of sprig adhered in the old leaf and old leaf of camphor tree is acquired, is cleaned, dried, crushed, smashed raw material Partial size is 2mm, and smashed raw material is added in extraction bucket, and the temperature extracted in bucket is, pressure 1MPa, condensation gasification Natural borneol afterwards purifies condensed natural borneol using oil water separator, and the revolving speed of oil water separator is 1200 revs/min Clock, purification time are 5min.The yield of natural borneol is 1.11%, purity 88%.
Embodiment 1
The total 100kg of sprig adhered in the old leaf and old leaf of camphor tree is acquired, is cleaned, dried, crushed, smashed raw material Partial size is 2mm, and smashed raw material is added in extraction bucket, and the temperature extracted in bucket is, pressure 1MPa, condensation gasification Natural borneol afterwards purifies condensed natural borneol using oil water separator, and the revolving speed of oil water separator is 4200 revs/min Clock, purification time are 5min.The residue in extraction bucket is then taken out, complex enzyme is added into residue, digests residue, enzyme The time of solution is 3h, and the temperature of enzymatic hydrolysis is, obtain extracting solution;Wherein complex enzyme is the papain of equal proportion mixing, fibre It ties up plain enzyme, extract enzyme and pectase.Extracting solution is added in extraction bucket and is extracted, the natural borneol after condensation gasification.It utilizes The yield of the resulting natural borneol of the above method is 1.98%, purity 95%.
Embodiment 2
The total 100kg of sprig adhered in the old leaf and old leaf of camphor tree is acquired, is cleaned, dried, crushed, smashed raw material Partial size is 1.5mm, and smashed raw material is added in extraction bucket, and the temperature extracted in bucket is, pressure 3MPa, condensing gas Natural borneol after change purifies condensed natural borneol using oil water separator, and the revolving speed of oil water separator is 4200 turns/ Minute, the purification time is 8min.The residue in extraction bucket is then taken out, complex enzyme is added into residue, digests residue, The time of enzymatic hydrolysis is 3.5h, and the temperature of enzymatic hydrolysis is, obtain extracting solution;Wherein complex enzyme is the Papain of equal proportion mixing Enzyme, extracts enzyme and pectase at cellulase.Extracting solution is added in extraction bucket and is extracted, the natural borneol after condensation gasification. Yield using the resulting natural borneol of the above method is 2.0%, purity 97%.
Embodiment 3
The total 100kg of sprig adhered in the old leaf and old leaf of camphor tree is acquired, is cleaned, dried, crushed, smashed raw material Partial size is 2.5mm, and smashed raw material is added in extraction bucket, and the temperature extracted in bucket is, pressure 4MPa, condensing gas Natural borneol after change purifies condensed natural borneol using oil water separator, and the revolving speed of oil water separator is 4200 turns/ Minute, the purification time is 10min.The residue in extraction bucket is then taken out, complex enzyme is added into residue, residue is made to carry out enzyme The time of solution, enzymatic hydrolysis is 4h, and the temperature of enzymatic hydrolysis is, obtain extracting solution;Wherein complex enzyme is the pawpaw egg of equal proportion mixing White enzyme, extracts enzyme and pectase at cellulase.Extracting solution is added in extraction bucket and is extracted, the natural ice after condensation gasification Piece.Yield using the resulting natural borneol of the above method is 2.2%, purity 98%.
From above-described embodiment, it can be concluded that, the natural borneol extracted using method of the invention is compared to traditional method for extracting Rate is higher, and the resin in borneol camphor tree branches and leaves can sufficiently be precipitated, to save raw material, reduces production cost.Meanwhile the present invention Natural borneol is purified using 4200 revs/min of oil water separator, the purity of natural borneol is made to be increased dramatically.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.

Claims (8)

1. a kind of method of borneol camphor tree branches and leaves extraction purification, which comprises the following steps:
Step S1: the sprig adhered in the old leaf and old leaf of camphor tree is acquired as raw material, raw material is pre-processed;
Step S2: pretreated raw material obtained by step S1 is added in extraction bucket, is extracted using high-temperature high-pressure overheat steam;
Step S3: using condenser by after the gasification being obtained by extraction natural borneol condense, using oil water separator to condensation after Natural borneol purification;
Step S4: the residue in step S2 extraction bucket is taken out, complex enzyme is added into residue, digests residue, is mentioned Take liquid;
Step S5: extraction bucket is added in extracting solution, repeats step S2 ~ step S3.
2. a kind of method of borneol camphor tree branches and leaves extraction purification according to claim 1, which is characterized in that pre- in step S1 Processing includes cleaning, drying, crushing.
3. a kind of method of borneol camphor tree branches and leaves extraction purification according to claim 2, which is characterized in that smashed raw material Partial size be 1.5mm ~ 2.5mm.
4. a kind of method of borneol camphor tree branches and leaves extraction purification according to claim 1, which is characterized in that extracted in step S2 Bucket in temperature be, pressure is 1MPa ~ 4MPa.
5. a kind of method of borneol camphor tree branches and leaves extraction purification according to claim 1, which is characterized in that the oil in step S3 The revolving speed of separator is 4200 revs/min.
6. a kind of method of borneol camphor tree branches and leaves extraction purification according to claim 5, which is characterized in that mentioning in step S3 The pure time is 5min ~ 10min.
7. a kind of method of borneol camphor tree branches and leaves extraction purification according to claim 1, which is characterized in that answering in step S4 Synthase is the papain of equal proportion mixing, cellulase, extracts enzyme and pectase.
8. a kind of method of borneol camphor tree branches and leaves extraction purification according to claim 7, which is characterized in that enzymolysis processing when Between be 3h ~ 4h, the temperature of enzymatic hydrolysis is
CN201811359112.0A 2018-11-15 2018-11-15 A kind of method of borneol camphor tree branches and leaves extraction purification Pending CN109503329A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104693008A (en) * 2015-03-16 2015-06-10 江苏金叶子生物科技有限公司 Method for coarsely extracting natural borneol from cinnamomum camphora
CN105837405A (en) * 2016-04-20 2016-08-10 江西林科龙脑科技有限公司 Method for preparing natural borneol
CN107473942A (en) * 2017-09-19 2017-12-15 北京国康本草物种生物科学技术研究院有限公司 The extracting method of natural borneol
CN108484362A (en) * 2018-05-16 2018-09-04 江南大学 A method of improving natural borneol recovery rate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104693008A (en) * 2015-03-16 2015-06-10 江苏金叶子生物科技有限公司 Method for coarsely extracting natural borneol from cinnamomum camphora
CN105837405A (en) * 2016-04-20 2016-08-10 江西林科龙脑科技有限公司 Method for preparing natural borneol
CN107473942A (en) * 2017-09-19 2017-12-15 北京国康本草物种生物科学技术研究院有限公司 The extracting method of natural borneol
CN108484362A (en) * 2018-05-16 2018-09-04 江南大学 A method of improving natural borneol recovery rate

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