CN111205169B - Refining process of natural borneol - Google Patents
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- CN111205169B CN111205169B CN201911023354.7A CN201911023354A CN111205169B CN 111205169 B CN111205169 B CN 111205169B CN 201911023354 A CN201911023354 A CN 201911023354A CN 111205169 B CN111205169 B CN 111205169B
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- C07—ORGANIC CHEMISTRY
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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Abstract
The invention relates to the technical field of biochemical engineering, and discloses a refining process of natural borneol aiming at the problems of high water content and low purity of the natural borneol, which comprises the following steps: (1) Collecting branches and leaves of the borneol camphora, cleaning, drying, crushing and sieving to obtain borneol camphora branch and leaf powder; (2) Soaking in water, distilling with water, and condensing and crystallizing the fraction to obtain crude extract of natural borneol; (3) Adding methyl tert-butyl ether, stirring and dissolving to obtain a mixed solution A; (4) distilling to obtain anhydrous natural borneol; (5) Adding petroleum ether, and performing ultrasonic dissolution to obtain a mixed solution B; (6) Sealing, refrigerating, recrystallizing, filtering, and vacuum drying to obtain pure natural Borneolum. The refining process of the invention obviously reduces the loss of natural borneol in the dehydration process, the water content of the refined product is as low as 0.02%, the content of d-borneol is more than 98.46%, the recovery rate of methyl tert-butyl ether is more than 86.7%, and the refined product has stable quality and simple process.
Description
Technical Field
The invention relates to the technical field of biochemical engineering, in particular to a natural borneol extraction technology, and in particular relates to a natural borneol refining process.
Background
The natural borneol is a precious medicinal material and high-grade spice, is also called natural d-borneol and plum slice, has fragrant smell, bitter taste and pungent and cool property, and has the medicinal effects of dredging orifices, relieving swelling and pain, clearing heat and detoxicating, reducing phlegm and improving eyesight, refreshing mind, resisting cancer, treating fever and coma and the like. At present, borneol is widely applied clinically, generally used as a compatible preparation, has the functions of resisting thrombus, bacteria and inflammation, resisting pregnancy and virus and relieving pain, and can bidirectionally regulate the excitability of the central nerve of a human body. In addition, borneol is also used for beauty treatment, and many skin care products and daily cosmetics also contain borneol.
At present, natural borneol produced in China is mainly extracted from branches and leaves of Cinnamomum camphora (L.) Presl which is a lauraceae plant, and is refined, and the medicinal effect of the natural borneol is far better than that of synthetic borneol and natural levo-borneol (borneol). However, the production scale of the domestic natural borneol is small, the equipment is backward, most of the natural borneol is crude products, the production status of the natural borneol can not meet the market demand, the backward production process can not adapt to the modern industrial production, the process of entering the international market of the traditional Chinese medicine formula and the preparation is hindered by the synthesis of the borneol, especially the improvement of the living standard of people and the enhancement of the environmental awareness in recent years, and the demand of some international and domestic high-grade cosmetics, medicines, foods, essences and spices on the natural borneol is increased day by day, so that the industrial production of the natural borneol is very urgent.
The patent number CN201510113454.4, the patent name of "a method for crude extraction of natural borneol from cinnamomum camphora", comprises the following steps: 1) Pulverizing branches and leaves of Cinnamomum camphora, the length of the pulverized particles is no more than 10cm; 2) Adding the crushed branches and leaves of the borneol camphora into an extraction tank, directly acting high-pressure superheated steam on the branches and leaves, controlling the temperature to ensure that natural borneol in the borneol camphora is vaporized and sublimated, and extracting for 35-40 minutes; 3) Condensing the gasified natural borneol by a condenser and collecting.
The existing extraction method of borneol camphor is mainly a steam distillation method, but the crude extract of borneol obtained by the steam distillation method contains higher water content (the water content is about 8%), and the purity of d-borneol is low (the content is generally about 80%), while the content of d-borneol in natural borneol is required to reach more than 96% according to the pharmacopoeia. The refining process generally adopts the traditional sublimation method, but can not remove water, and meanwhile, the molecular weights of the borneol and the camphor are close, the sublimation temperature difference is not large, the refining effect is not ideal, and the industrial development of the natural borneol is seriously influenced. Therefore, how to prepare natural borneol with low water content, high purity and stable quality is a problem to be solved urgently by the technical personnel in the field.
Disclosure of Invention
The invention aims to solve the problems of high water content and low purity of natural borneol obtained by a steam distillation method in the extraction method of borneol camphor and provides a refining process of natural borneol.
In order to achieve the purpose, the invention adopts the following technical scheme:
a refining process of natural borneol comprises the following steps:
(1) Collecting and drying fresh branches and leaves of borneol camphora, and then crushing and sieving to obtain borneol camphora branch and leaf powder;
(2) Adding water into the borneol camphor branch and leaf powder obtained in the step (1) for soaking, then carrying out co-water distillation, and condensing and crystallizing fractions to obtain a natural borneol crude extract;
(3) Adding methyl tert-butyl ether into the crude extract of the natural borneol obtained in the step (2), and stirring and dissolving to obtain a mixed solution A;
(4) Distilling the mixed solution A obtained in the step (3) to obtain anhydrous natural borneol;
(5) Adding petroleum ether into the anhydrous natural borneol obtained in the step (4), and performing ultrasonic dissolution to obtain a mixed solution B;
(6) And (5) sealing the mixed solution B obtained in the step (5), refrigerating, recrystallizing, filtering, and drying in vacuum to obtain the pure natural borneol.
The preparation method has the advantages that because the proper water separating agent is stable, does not react with water and other materials, is insoluble with water, can be azeotroped with water, has low toxicity, is safe and easy to recycle, the preparation method is researched by long-term tortuosity, and finally adopts methyl tert-butyl ether as the water separating agent, is colorless transparent liquid which is insoluble in water and can be dissolved in ethanol, diethyl ether, benzene, petroleum ether and the like, has the specific gravity of 0.74 (20 ℃), the boiling point of 55.2 ℃, and the acute toxicity: LD50 3030mg (oral mouse); the water separating agent has stable property, is not easy to generate oxidation reaction of other ethers to generate peroxide, is hardly dissolved in water, has large specific gravity and water difference, has good layering property with water, can be azeotroped with water, is easy to take away water from a system, and is removed and separated by layering.
Preferably, in the step (1), the mesh number of the screen is 10 to 40 mesh.
Adopt above-mentioned further beneficial effect to lie in, smash to sieve and can reduce the particle size of borneol camphor branch and leaf powder, increase the area of contact with water to be favorable to soaking and the going on of distillation reaction.
Preferably, in the step (2), the feed-liquid ratio of the borneol camphor branch and leaf powder to the water is 1:6-10; the soaking time is 0.5 to 1 hour; the distillation temperature is 90-100 ℃ and the distillation time is 1.5-2.5 h.
The method has the further beneficial effects that the natural borneol in the borneol camphor branches and leaves is extracted by adopting a steam distillation method, so that the extraction efficiency is obviously improved, and the extraction time is shortened.
Preferably, in the step (3), the feed-liquid ratio (mass to volume ratio) of the natural ice flake crude extract to the methyl tert-butyl ether is 1:3.
the methyl tert-butyl ether is used as a water removal agent, has good water absorption performance and low boiling point, can be azeotroped with water, is immiscible with water after distillation and is layered, and thus, is easy to recover.
Preferably, in the step (4), the distillation temperature is 55-65 ℃ and the distillation time is 1-2 h.
The further advantage of using the above is that the methyl tert-butyl ether is distilled off while removing the water from the crude natural borneol extract.
Preferably, in the step (5), the ratio (mass to volume) of the anhydrous natural borneol to the petroleum ether is 1:1 to 1.5, preferably 1:1.
The further beneficial effect of adopting the above is that petroleum ether is used as solvent, can efficiently dissolve crude extract of natural borneol and is easy to separate.
Preferably, in the step (5), the power of ultrasonic dissolution is 200 to 400W, and the time is 5 to 10min.
The further advantage of using the above is that the natural ice flakes crude extract can be dissolved in petroleum ether more rapidly and dispersed therein uniformly by the aid of ultrasound.
Preferably, in the step (6), the refrigerating temperature is-4 to 0 ℃, preferably-4 ℃; the refrigerating time is 15-24 h, preferably 20h.
The adoption of the further beneficial effects is that the refrigeration can reduce impurities such as mother liquor and the like included in the natural borneol crystal, and can ensure that the crystal form is better and the yield is also increased.
Preferably, in the step (6), the degree of vacuum for vacuum drying is 93.3 to 98.6KPa; the drying temperature is 55-75 ℃ and the drying time is 4-6 h.
The further beneficial effect of adopting the above is that the vacuum drying can remove the water, and simultaneously reduce the loss and oxidation of the natural borneol.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1) The refining process of the natural borneol is provided, and the loss of the natural borneol in the dehydration process is obviously reduced;
(2) The water content of the refined product is as low as 0.02%, the content of the D-borneol is more than 98.46%, and all indexes are higher than the standard of natural borneol in pharmacopeia 2015 edition;
(3) The recovery rate of the methyl tert-butyl ether is above 86.7 percent, the production cost is low, the process is simple, and the economic benefit is good.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The refining process of the natural borneol specifically comprises the following steps:
(1) Collecting fresh branches and leaves of the cinnamomum camphora, drying, crushing, and sieving with a 20-mesh sieve to obtain powder of the branches and leaves of the cinnamomum camphora;
(2) Taking 100g of borneol camphor branch and leaf powder obtained in the step (1), adding 800mL of water to soak for 0.8h, then putting the powder into a distillation flask, carrying out co-water distillation at 95 ℃ for 2h, and condensing and crystallizing fractions to obtain a natural borneol crude extract (repeating for multiple times, and collecting 10g of the natural borneol crude extract);
(3) Taking 10g of the crude natural borneol extract obtained in the step (2) to a conical flask, adding 30mL of methyl tert-butyl ether, and stirring for dissolving to obtain a mixed solution A;
(4) Putting the mixed solution A obtained in the step (3) into a distillation flask, distilling for 1.5h under the water bath heating condition of 60 ℃, and recovering methyl tert-butyl ether to obtain anhydrous natural borneol;
(5) Taking 5g of the anhydrous natural borneol obtained in the step (4), adding 5mL of petroleum ether, and performing ultrasonic treatment at 300W for 8min to assist dissolution to obtain a mixed solution B;
(6) And (3) sealing the mixed solution B obtained in the step (5), putting the sealed mixed solution B into a refrigerator, refrigerating the mixed solution B for 20 hours at the temperature of minus 4 ℃, recrystallizing the obtained product, performing suction filtration, putting the obtained crystallized product into a vacuum drying oven, adjusting the vacuum degree to 95KPa, and drying the crystallized product for 5 hours at the temperature of 60 ℃ to obtain the pure natural borneol product.
Example 2
The refining process of the natural borneol specifically comprises the following steps:
(1) Collecting fresh branches and leaves of the cinnamomum camphora, drying, crushing and sieving by a sieve with 10 meshes to obtain powder of the branches and leaves of the cinnamomum camphora;
(2) Taking 100g of borneol camphor branch and leaf powder obtained in the step (1), adding 600mL of water to soak for 0.5h, then putting the powder into a distillation flask, carrying out co-water distillation at 90 ℃ for 1.5h, and condensing and crystallizing fractions to obtain a natural borneol crude extract (repeating for multiple times, collecting 10g of the natural borneol crude extract);
(3) Taking 10g of the crude extract of the natural borneol obtained in the step (2) to be put in a conical flask, adding 25mL of methyl tert-butyl ether, and stirring for dissolving to obtain a mixed solution A;
(4) Putting the mixed solution A obtained in the step (3) into a distillation flask, distilling for 1h under the water bath heating condition of 55 ℃, and recovering methyl tert-butyl ether to obtain anhydrous natural borneol;
(5) Taking 5g of the anhydrous natural borneol obtained in the step (4), adding 5mL of petroleum ether, and performing ultrasonic treatment at 200W for 5min to assist dissolution to obtain a mixed solution B;
(6) And (3) sealing the mixed solution B obtained in the step (5), placing the mixed solution in a refrigerator, refrigerating for 15h at 0 ℃, recrystallizing, performing suction filtration, placing the obtained crystallized product in a vacuum drying oven, adjusting the vacuum degree to 93.3KPa, and drying for 4h at 55 ℃ to obtain the pure natural borneol product.
Example 3
The refining process of the natural borneol specifically comprises the following steps:
(1) Collecting fresh branches and leaves of a cinnamomum camphora tree, drying, crushing, and sieving by a 40-mesh sieve to obtain cinnamomum camphora branch and leaf powder;
(2) Taking 100g of the borneol camphor branch and leaf powder obtained in the step (1), adding 1000mL of water to soak for 1h, then putting the powder into a distillation flask, carrying out co-water distillation at 100 ℃ for 2.5h, and condensing and crystallizing fractions to obtain a natural borneol crude extract (repeating for multiple times, and collecting 10g of the natural borneol crude extract);
(3) Putting 10g of the crude extract of the natural borneol obtained in the step (2) into a conical flask, adding 35mL of methyl tert-butyl ether, and stirring for dissolving to obtain a mixed solution A;
(4) Putting the mixed solution A obtained in the step (3) into a distillation flask, distilling for 2 hours under the water bath heating condition of 65 ℃, and recovering methyl tert-butyl ether to obtain anhydrous natural borneol;
(5) Taking 5g of the anhydrous natural borneol obtained in the step (4), adding 7.5mL of petroleum ether, and carrying out 400W ultrasonic treatment for 10min to assist dissolution to obtain a mixed solution B;
(6) And (3) sealing the mixed solution B obtained in the step (5), putting the mixed solution in a refrigerator for refrigerating for 24h at the temperature of minus 4 ℃, recrystallizing, performing suction filtration, putting the obtained crystallized product in a vacuum drying box, adjusting the vacuum degree to 98.6KPa, and drying for 6h at the temperature of 75 ℃ to obtain the pure natural borneol.
Comparative example 1
The difference from the example 1 is that the anhydrous sodium sulfate is used for removing water in the step (3), and the rest steps are the same as the example 1.
Comparative example 2
The difference from the example 1 is that the absolute ethyl alcohol is adopted to remove water in the step (3), and the rest steps are the same as the example 1.
Comparative example 3
The difference from example 1 is that 20mL of methyl t-butyl ether was added to 10g of crude natural ice flakes in step (3) and dissolved by stirring, and the procedure was the same as in example 1.
Comparative example 4
The difference from example 1 is that 40mL of methyl t-butyl ether was added to 10g of crude natural ice flakes in step (3) and dissolved with stirring, and the procedure was the same as in example 1.
Comparative example 5
The difference from example 1 is that 50mL of methyl t-butyl ether was added to 10g of crude natural ice flakes in step (3) and dissolved with stirring, and the procedure was the same as in example 1.
Performance testing
1. Selection of water removal agent
The water content of each of the purified natural borneol prepared in example 1 and comparative examples 1 to 2 was measured by a Karl Fischer moisture meter, and the results are shown in Table 1.
TABLE 1 Water content of the purified natural borneol prepared in example 1 and comparative examples 1-2
| Item | Water removing agent | Water content (%) |
| Example 1 | Methyl tert-butyl ether | 0.02 |
| Comparative example 1 | Anhydrous sodium sulfate | 2.04 |
| Comparative example 2 | Anhydrous ethanol | 3.00 |
As can be seen from Table 1, the methyl tert-butyl ether selected in the present invention is the most effective in removing water as compared with anhydrous sodium sulfate and anhydrous ethanol.
2. Selection of dosage of water removing agent
The water content of each of the purified natural borneol prepared in example 1 and comparative examples 3 to 5 was measured by a Karl Fischer moisture meter, and the results are shown in Table 2.
Table 2 water content of the purified natural borneol prepared in example 1 and comparative examples 3 to 5
| Item | Feed-liquid ratio of natural borneol crude extract to methyl tert-butyl ether | Water content (%) |
| Example 1 | 1:3 | 0.02 |
| Comparative example 3 | 1:2 | 0.12 |
| Comparative example 4 | 1:4 | 0.05 |
| Comparative example 5 | 1:5 | 0.04 |
As can be seen from Table 2, the water removal effect is best when the feed-liquid ratio of the natural borneol crude extract to the methyl tert-butyl ether is 1:3, the water content is as low as 0.02%, and basically no residual water exists.
3. Determination of various indexes
The pure natural borneol prepared in each of examples 1 to 3 was taken, and the properties, the identification results, the camphor content (not more than 3.0%) and the d-borneol content (not less than 96.0%) of the three products were respectively detected according to the properties, the identification methods, the inspection methods and the content measurement methods in the "chinese pharmacopoeia" of the 2015 edition-quality standard for natural borneol (d-borneol).
The measurement results are shown in Table 3.
Table 3 measurement results of each index of the purified natural borneol prepared in examples 1 to 3
| Item | Example 1 | Example 2 | Example 3 |
| Traits | White crystalline powder | White crystalline powder | White crystalline powder |
| Identification result | Compliance with regulations | Compliance with regulations | Compliance with regulations |
| Camphor content (%) | 0.32 | 1.11 | 0.63 |
| D-borneol content (%) | 99.63 | 98.46 | 99.00 |
As can be seen from table 3, the pure natural borneol prepared in examples 1 to 3 of the present invention is white crystalline powder, and the identification results are in accordance with the specification, the camphor content is up to 1.11% (standard is not more than 3.0%), the d-borneol content is as low as 99.00% (standard is not less than 96.0%), and particularly, when the material-to-liquid ratio of the crude natural borneol extract to the methyl tert-butyl ether is 1:3, the prepared pure natural borneol has the highest purity and the lowest impurity content.
The tests show that all indexes of the pure natural borneol prepared by the refining process are higher than those of the natural borneol standard in pharmacopoeia 2015 edition.
4. Methyl tert-butyl ether recovery determination
The amount of methyl t-butyl ether used and the amount of methyl t-butyl ether recovered in examples 1 to 3 were weighed and the recovery rates thereof were calculated, respectively. The measurement results are shown in Table 4.
TABLE 4 results of measurement of recovery of methyl t-butyl ether in examples 1 to 3
| Item | Amount used (mL) | Recovery mass (mL) | Recovery (%) |
| Example 1 | 30.0 | 27.0 | 93.3 |
| Example 2 | 25.0 | 22.5 | 90.0 |
| Example 3 | 35.0 | 30.3 | 86.7 |
As can be seen from Table 4, the recovery rate of methyl tert-butyl ether in the invention is more than 85%, and particularly, when the feed-to-liquid ratio of the natural borneol crude extract to the methyl tert-butyl ether is 1:3, the recovery rate of the methyl tert-butyl ether is the highest, and the production cost is low.
From the data of examples 1 to 3 and comparative examples 1 to 5, it is clear that only the embodiments within the scope of the claims of the present invention can satisfy the above requirements in all aspects, and an optimized embodiment can be obtained, and natural borneol with optimal performance can be obtained. The change of the mixture ratio, the replacement/addition/subtraction of raw materials or the change of the feeding sequence can bring corresponding negative effects.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. The refining process of the natural borneol is characterized by comprising the following steps:
(1) Collecting fresh branches and leaves of the cinnamomum camphora, cleaning, drying, crushing and sieving to obtain powder of the branches and leaves of the cinnamomum camphora;
(2) Adding water into the borneol camphor branch and leaf powder obtained in the step (1) for soaking, then carrying out co-water distillation, and condensing and crystallizing fractions to obtain a crude extract of natural borneol;
(3) Adding methyl tert-butyl ether into the crude extract of the natural borneol obtained in the step (2), and stirring and dissolving to obtain a mixed solution A; the mass and volume ratio of the natural ice flake crude product to the methyl tert-butyl ether is 1:3;
(4) Distilling the mixed solution A obtained in the step (3) to obtain anhydrous natural borneol; the distillation temperature is 55-65 ℃, and the distillation time is 1-2 h;
(5) Adding petroleum ether into the anhydrous natural borneol obtained in the step (4), and performing ultrasonic dissolution to obtain a mixed solution B;
(6) And (5) sealing the mixed solution B obtained in the step (5), refrigerating, recrystallizing, filtering, and drying in vacuum to obtain the pure natural borneol.
2. The refining process of natural borneol according to claim 1, wherein in step (1), the mesh number of the sieved mesh is 10-40 meshes.
3. The refining process of natural borneol according to claim 1, wherein in the step (2), the mass and volume ratio of the borneol camphor branch and leaf powder to water is 1:6-10.
4. The refining process of natural borneol according to claim 1, wherein in the step (2), the soaking time is 0.5-1 h; the distillation temperature is 90-100 ℃, and the distillation time is 1.5-2.5 h.
5. The refining process of natural borneol according to claim 1, wherein in step (5), the mass and volume ratio of the anhydrous natural borneol to the petroleum ether is 1:1-1.5.
6. The refining process of natural borneol according to claim 1, wherein in the step (5), the power of the ultrasonic wave is 200-400W.
7. The refining process of natural borneol according to claim 1, wherein in the step (6), the refrigeration temperature is-4 to 0 ℃ and the time is 15 to 24 hours.
8. The refining process of natural borneol according to claim 1, wherein in step (6), the vacuum degree of vacuum drying is 93.3-98.6 KPa, the temperature is 55-75 ℃, and the time is 4-6 h.
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