CN113861262A - Tomatidine extraction and concentration process - Google Patents

Tomatidine extraction and concentration process Download PDF

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Publication number
CN113861262A
CN113861262A CN202111114578.6A CN202111114578A CN113861262A CN 113861262 A CN113861262 A CN 113861262A CN 202111114578 A CN202111114578 A CN 202111114578A CN 113861262 A CN113861262 A CN 113861262A
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China
Prior art keywords
tomatidine
solution
tomato
extraction
alkali
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CN202111114578.6A
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Chinese (zh)
Inventor
宋宏臣
仲晓晴
倪周娜
王建明
陈顺权
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Guangzhou Institute Of Advanced Technology
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Guangzhou Institute Of Advanced Technology
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Priority to CN202111114578.6A priority Critical patent/CN113861262A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J71/00Steroids in which the cyclopenta(a)hydrophenanthrene skeleton is condensed with a heterocyclic ring
    • C07J71/0005Oxygen-containing hetero ring

Abstract

The invention relates to the technical field of natural product separation, and particularly relates to a tomato alkali extraction and concentration process. The method comprises the following steps: step 1, crushing fresh tomato branches and leaves, adding an acid solution for leaching, and filtering to obtain a leaching solution; step 2, adding an alkali solution into the leaching solution, standing and filtering to obtain a precipitate which is a tomatidine crude product; step 3, re-dissolving the tomatidine crude product to obtain tomatidine feed liquid; step 4, separating and concentrating the tomatidine feed liquid by adopting a membrane filtration technology to obtain a tomatidine concentrated solution; and 5, evaporating the concentrated tomato alkali solution. The tomato alkali extraction and concentration process is combined with a membrane filtration and separation technology, a large amount of organic reagents are not needed for repeated extraction, so that the problems of difficulty in solvent treatment, strong toxicity, high pollution and the like do not exist, the tomato alkali extraction and concentration process has the technical advantages of convenience in operation, compact structure, low energy consumption, simple process and no secondary pollution, the extraction and concentration efficiency is greatly improved, and the tomato alkali extraction and concentration process is suitable for large-scale production.

Description

Tomatidine extraction and concentration process
Technical Field
The invention relates to the technical field of natural product separation, and particularly relates to a tomato alkali extraction and concentration process.
Background
The molecular formula of the tomatidine is C27H45NO2Is easily soluble in ethanol, methanol, ethyl acetate and propylene glycol, is hardly soluble in water, diethyl ether and petroleum ether, is stable in alkaline environment, is used inIs easy to hydrolyze in acid environment. The tomatidine has high content in tomato plants, is a secondary metabolite in the growth process of tomatoes, can inhibit the growth of fungi and bacteria, and can resist virus and insect invasion.
At present, a large amount of waste tomato branches and leaves are produced after the tomatoes are harvested, the treatment mode mainly comprises landfill and composting, time and labor are consumed, and the resource utilization rate is low. The tomatidine has good biological activity and can be applied to the technical fields of medicine, agricultural pest control and the like, so that the tomatidine extraction method has great market demand and wide development prospect by recycling waste tomato branches and leaves. In the prior art, the modes of resource utilization of the tomato leaves and extraction of effective ingredients of the tomato leaves are few, and the process of extracting and concentrating the tomato alkali is few and few.
Chinese patent publication No. CN102558283A discloses a method for extracting tomatidine from tomato branches and leaves, which mainly adopts solvents such as methanol, chloroform, etc. to extract and concentrate, and adds diatomite and activated carbon into the extract, and adopts a resin separation column to enrich and separate tomatidine. However, organic reagents such as chloroform and the like used in the method have high toxicity and strong pollution, and the method has long process route, long time consumption and large cost investment. The Chinese patent with publication number CN110326630A discloses a method for preparing biological pesticide by using tomato stems and leaves, which uses a fermentation extraction mode to replace reagent extraction. However, the method has long fermentation time and low extraction rate, and the extracted tomatidine is only suitable for biological pesticides in quality and is difficult to apply to high-end fields such as medicines.
Disclosure of Invention
In view of the above, there is a need to provide a process for extracting and concentrating tomatidine, which avoids using a large amount of toxic organic reagents for multiple extractions, and adopts a membrane filtration separation technique, thereby simplifying the operation, reducing the cost, and improving the extraction purity, content and purification efficiency of tomatidine.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a tomatidine extraction and concentration process, which comprises the following steps:
step 1, crushing fresh tomato branches and leaves, adding an acid solution for leaching, and filtering to obtain a leaching solution;
step 2, adding an alkali solution into the leaching solution, standing and filtering to obtain a precipitate which is a tomatidine crude product;
step 3, re-dissolving the tomatidine crude product to obtain tomatidine feed liquid;
step 4, separating and concentrating the tomatidine feed liquid by adopting a membrane filtration technology to obtain a tomatidine concentrated solution;
and 5, evaporating the concentrated tomato alkali solution.
Furthermore, in the above process, the fresh tomato branches and leaves are distilled with pure water before being crushed, and the volatile components of the tomato branches and leaves are distilled.
Further, in the tomato alkali extraction and concentration process, the acid solution is an acetic acid water solution with the mass fraction of 5-10%; the ratio of the volume (mL) of the acetic acid aqueous solution to the mass (g) of the tomato branches and leaves is (3-6): 1.
further, in the tomato alkali extraction and concentration process, the acid solution is extracted twice, the extraction time is 2-4 hours, and the extract is the mixture of the two extractions.
Further, in the above-mentioned alkali extraction and concentration process for tomato, the alkali solution is a sodium hydroxide solution, and the pH of the leaching solution is adjusted to 11 by the alkali solution.
Further, in the tomato alkali extraction and concentration process, the solvent used for re-dissolving in the step 3 is an ethanol water solution with the mass fraction of 70-90%.
Further, in the above-mentioned tomatidine extraction and concentration process, before separation and concentration by membrane separation technology, tomatidine feed liquid is roughly filtered by filter paper or nylon filter cloth.
Further, in the process for extracting and concentrating the tomatidine, the step 4 specifically comprises the steps of firstly carrying out ultrafiltration on the tomatidine feed liquid and then carrying out nanofiltration.
Further, in the tomato alkali extraction and concentration process, the evaporation in the step 5 is rotary evaporator evaporation, the rotary evaporation temperature is 40-50 ℃, and the rotating speed is 30-50 r/min.
Further, in the process for extracting and concentrating the tomatidine, a drying step is also included after evaporation, and the drying step is drying for more than 24 hours at the temperature of 60-80 ℃ until the water in the tomatidine concentrated solution is completely removed.
In a second aspect, the invention provides tomatidine, which is prepared by adopting the tomatidine extraction and concentration process.
The invention has the beneficial effects that:
the tomato alkali extraction and concentration process is combined with a membrane filtration and separation technology, a large amount of organic reagents are not needed for repeated extraction, so that the problems of difficulty in solvent treatment, strong toxicity, high pollution and the like do not exist, the tomato alkali extraction and concentration process has the technical advantages of convenience in operation, compact structure, low energy consumption, simple process and no secondary pollution, the extraction and concentration efficiency is greatly improved, and the tomato alkali extraction and concentration process is suitable for large-scale production.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be further clearly and completely described below with reference to the embodiments of the present invention. It should be noted 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
A tomatidine extraction and concentration process comprises the following steps:
(1) crushing fresh tomato branches and leaves, adding 6% by mass of acetic acid aqueous solution, leaching twice for 3 hours each time, and combining leaching liquor obtained by leaching twice; wherein the volume (mL) of the acetic acid aqueous solution is 5 times of the mass (g) of the tomato branches and leaves;
(2) adding sodium hydroxide solution to the combined leaching liquor, and adjusting the pH of the leaching liquor to 11; standing for layering, and filtering with rapid filter paper to obtain precipitate as tomatidine crude product;
(3) re-dissolving the tomatidine crude product by using 80% ethanol water solution by mass fraction, and fully stirring to obtain tomatidine feed liquid;
(4) coarsely filtering the tomatidine solution with a 1300-mesh nylon filter screen, and then sequentially performing ultrafiltration and nanofiltration to separate and concentrate the tomatidine solution to obtain a tomatidine concentrated solution;
(5) rotary evaporating the concentrated tomato alkali solution at 50 deg.C at rotation speed of 30 rpm to remove ethanol water solution.
Example 2
A tomatidine extraction and concentration process comprises the following steps:
(1) crushing fresh tomato branches and leaves, adding an acetic acid aqueous solution with the mass fraction of 8%, leaching twice, leaching for 2 hours each time, and combining leaching liquor obtained by leaching twice; wherein the volume (mL) of the acetic acid aqueous solution is 4 times of the mass (g) of the tomato branches and leaves;
(2) adding sodium hydroxide solution to the combined leaching liquor, and adjusting the pH of the leaching liquor to 11; standing for layering, and filtering with rapid filter paper to obtain precipitate as tomatidine crude product;
(3) re-dissolving the tomatidine crude product by using 75% of ethanol water solution by mass fraction, and fully stirring to obtain tomatidine feed liquid;
(4) coarsely filtering the tomatidine solution with a 1300-mesh nylon filter screen, and then sequentially performing ultrafiltration and nanofiltration to separate and concentrate the tomatidine solution to obtain a tomatidine concentrated solution;
(5) rotary evaporating the concentrated tomato alkali solution at 40 deg.C at rotation speed of 50 rpm to remove ethanol water solution.
Example 3
A tomatidine extraction and concentration process comprises the following steps:
(1) crushing fresh tomato branches and leaves, adding 9% acetic acid aqueous solution by mass, leaching twice for 2 hours each time, and combining leaching liquor obtained by leaching twice; wherein the volume (mL) of the acetic acid aqueous solution is 3 times of the mass (g) of the tomato branches and leaves;
(2) adding sodium hydroxide solution to the combined leaching liquor, and adjusting the pH of the leaching liquor to 11; standing for layering, and filtering with rapid filter paper to obtain precipitate as tomatidine crude product;
(3) re-dissolving the tomatidine crude product by using an ethanol water solution with the mass fraction of 85%, and fully stirring to obtain tomatidine feed liquid;
(4) coarsely filtering the tomatidine solution with a 1300-mesh nylon filter screen, and then sequentially performing ultrafiltration and nanofiltration to separate and concentrate the tomatidine solution to obtain a tomatidine concentrated solution;
(5) rotary evaporating the concentrated tomato alkali solution at 45 deg.C at rotation speed of 30 rpm to remove ethanol water solution.
Example 4
A tomatidine extraction and concentration process comprises the following steps:
(1) removing big branches of fresh tomato branches and leaves, distilling the fresh tomato branches and leaves by pure water to distill out volatile components of the tomato branches and leaves; then crushing the distilled tomato branches and leaves, adding an acetic acid aqueous solution with the mass fraction of 8% after crushing, leaching twice, leaching for 2 hours each time, and combining leaching liquor obtained by leaching twice; wherein the volume (mL) of the acetic acid aqueous solution is 4 times of the mass (g) of the tomato branches and leaves;
(2) adding sodium hydroxide solution to the combined leaching liquor, and adjusting the pH of the leaching liquor to 11; standing for layering, and filtering with rapid filter paper to obtain precipitate as tomatidine crude product;
(3) re-dissolving the tomatidine crude product by using 75% of ethanol water solution by mass fraction, and fully stirring to obtain tomatidine feed liquid;
(4) coarsely filtering the tomatidine solution with a 1300-mesh nylon filter screen, and then sequentially performing ultrafiltration and nanofiltration to separate and concentrate the tomatidine solution to obtain a tomatidine concentrated solution;
(5) rotary evaporating the concentrated tomato alkali solution at 40 deg.C at rotation speed of 50 rpm to remove ethanol water solution.
Example 5
A tomatidine extraction and concentration process comprises the following steps:
(1) crushing 500g of fresh tomato branches and leaves, adding 6% by mass of acetic acid aqueous solution, leaching twice for 3 hours each time, and combining leaching solutions obtained by leaching twice; wherein the volume (mL) of the acetic acid aqueous solution is 5 times of the mass (g) of the tomato branches and leaves;
(2) adding sodium hydroxide solution to the combined leaching liquor, and adjusting the pH of the leaching liquor to 11; standing for layering, and filtering with rapid filter paper to obtain precipitate as tomatidine crude product;
(3) re-dissolving the tomatidine crude product by using 80% ethanol water solution by mass fraction, and fully stirring to obtain tomatidine feed liquid;
(4) coarsely filtering the tomatidine solution with 1300-mesh nylon filter cloth, and then sequentially performing ultrafiltration and nanofiltration to separate and concentrate the tomatidine solution to obtain tomatidine concentrated solution;
(5) rotary evaporating the concentrated tomato alkali solution at 50 deg.C at rotation speed of 30 rpm to remove ethanol water solution.
(6) And (3) placing the rotary evaporated tomatidine concentrated solution in a forced air drying oven, drying for 24h at 70 ℃ until the moisture is completely removed, and obtaining 1.48g of solid product.
Comparative example 1
A tomatidine extraction and concentration process comprises the following steps:
(1) crushing fresh tomato branches and leaves, adding an acetic acid aqueous solution with the mass fraction of 8%, leaching twice, leaching for 2 hours each time, and combining leaching liquor obtained by leaching twice; wherein the volume of the acetic acid water solution is 4 times of the mass of the tomato branches and leaves;
(2) adding sodium hydroxide solution to the combined leaching liquor, and adjusting the pH of the leaching liquor to 11; after standing and layering, filtering by using quick filter paper.
Comparative example 2
A tomatidine extraction and concentration process comprises the following steps:
(1) crushing fresh tomato branches and leaves, adding an acetic acid aqueous solution with the mass fraction of 8%, leaching twice, leaching for 2 hours each time, and combining leaching liquor obtained by leaching twice; wherein the volume of the acetic acid water solution is 4 times of the mass of the tomato branches and leaves;
(2) adding sodium hydroxide solution to the combined leaching liquor, and adjusting the pH of the leaching liquor to 11; standing for layering, and filtering with rapid filter paper to obtain precipitate as tomatidine crude product;
(3) re-dissolving the tomatidine crude product by using 75% of ethanol water solution by mass fraction, and fully stirring to obtain tomatidine feed liquid;
(4) coarsely filtering the tomatidine solution with 1300 mesh nylon filter cloth, and separating and concentrating the tomatidine solution by ultrafiltration.
Comparative example 3
A tomatidine extraction and concentration process comprises the following steps:
(1) crushing fresh tomato branches and leaves, adding an acetic acid aqueous solution with the mass fraction of 8%, leaching twice, leaching for 2 hours each time, and combining leaching liquor obtained by leaching twice; wherein the volume of the acetic acid water solution is 4 times of the mass of the tomato branches and leaves;
(2) adding sodium hydroxide solution to the combined leaching liquor, and adjusting the pH of the leaching liquor to 11; standing for layering, and filtering with rapid filter paper to obtain precipitate as tomatidine crude product;
(3) re-dissolving the tomatidine crude product by using 75% of ethanol water solution by mass fraction, and fully stirring to obtain tomatidine feed liquid;
(4) coarsely filtering the tomatidine solution with 1300 mesh nylon filter cloth, and sequentially separating and concentrating the tomatidine solution by ultrafiltration and nanofiltration.
Data comparison
The concentration of the tomato alkali solution obtained in example 2 and comparative examples 1 to 3 was measured, and the results are shown in table 1.
TABLE 1
Group of Concentration (mg/L)
Example 2 9300
Comparative example 1 110
Comparative example 2 600
Comparative example 3 850
As can be seen from table 1, the tomatidine extraction and concentration process provided in embodiment 2 of the present invention adopts a membrane filtration and separation technique to perform filtration and concentration, which can avoid the use of toxic organic solvents and greatly reduce the amount of ethanol, thereby reducing the volume of the material liquid treated by the rotary evaporation process and significantly improving the tomatidine extraction efficiency.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A tomatidine extraction and concentration process is characterized by comprising the following steps:
step 1, crushing fresh tomato branches and leaves, adding an acid solution for leaching, and filtering to obtain a leaching solution;
step 2, adding an alkali solution into the leaching solution, standing and filtering to obtain a precipitate which is a tomatidine crude product;
step 3, re-dissolving the tomatidine crude product to obtain tomatidine feed liquid;
step 4, separating and concentrating the tomatidine feed liquid by adopting a membrane filtration technology to obtain a tomatidine concentrated solution;
and 5, evaporating the concentrated tomato alkali solution.
2. The process for extracting and concentrating tomato alkali as claimed in claim 1, wherein the fresh tomato branches and leaves are distilled with pure water before being crushed, and volatile components of the tomato branches and leaves are distilled.
3. The tomato alkali extraction and concentration process as claimed in claim 1, wherein the acid solution is an acetic acid aqueous solution with a mass fraction of 5-10%; the volume of the acetic acid water solution and the mass ratio of the tomato branches and leaves are (3-6): 1.
4. the tomato alkali extraction and concentration process as claimed in claim 1, wherein the acid solution leaching is performed twice, and the leaching time is 2-4 h.
5. The process of claim 1, wherein the alkali solution is sodium hydroxide solution, and the alkali solution adjusts the pH of the leaching solution to 11.
6. The tomato alkali extraction and concentration process as claimed in claim 1, wherein the solvent used for re-dissolution in step 3 is 70-90% by weight of ethanol aqueous solution.
7. The process of claim 1, wherein the tomatidine solution is coarsely filtered through filter paper or nylon filter cloth before being separated and concentrated by membrane filtration.
8. The tomatidine extraction and concentration process as claimed in claim 1, wherein the step 4 comprises ultrafiltration of tomatidine solution, followed by nanofiltration.
9. The tomato alkali extraction and concentration process as claimed in claim 1, further comprising a drying step after evaporation, wherein the drying step is drying at 60-80 ℃ for more than 24h, until water in the tomato alkali concentrate is completely removed.
10. A tomatidine is prepared by the above tomatidine extraction and concentration process.
CN202111114578.6A 2021-09-23 2021-09-23 Tomatidine extraction and concentration process Pending CN113861262A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115413682A (en) * 2022-08-29 2022-12-02 京博农化科技有限公司 Application and composition of tomato stem and leaf extract for preventing and treating thrips

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102558283A (en) * 2010-12-24 2012-07-11 苏州宝泽堂医药科技有限公司 Method for extracting tomatidine from tomato branches and leaves
CN104561220A (en) * 2014-12-30 2015-04-29 成都普思生物科技有限公司 Method for preparing tomatidine through cellulose hydrolysis of tomato branches and leaves
CN109212054A (en) * 2018-07-24 2019-01-15 山东农业大学 A kind of method of HPLC MS measurement tomatidine and tomato saponin(e
CN110305144A (en) * 2019-06-12 2019-10-08 苏州岚云医药科技有限公司 A kind of technique using membrane technology separating natural anticancer drug

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102558283A (en) * 2010-12-24 2012-07-11 苏州宝泽堂医药科技有限公司 Method for extracting tomatidine from tomato branches and leaves
CN104561220A (en) * 2014-12-30 2015-04-29 成都普思生物科技有限公司 Method for preparing tomatidine through cellulose hydrolysis of tomato branches and leaves
CN109212054A (en) * 2018-07-24 2019-01-15 山东农业大学 A kind of method of HPLC MS measurement tomatidine and tomato saponin(e
CN110305144A (en) * 2019-06-12 2019-10-08 苏州岚云医药科技有限公司 A kind of technique using membrane technology separating natural anticancer drug

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115413682A (en) * 2022-08-29 2022-12-02 京博农化科技有限公司 Application and composition of tomato stem and leaf extract for preventing and treating thrips
CN115413682B (en) * 2022-08-29 2024-04-05 山东京博农化科技股份有限公司 Application of tomato stem and leaf extract in preventing and treating thrips and composition

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Application publication date: 20211231