阅读说明：本技术 一种烟碱纯化方法 (Nicotine purification method ) 是由 杨强 贺择 李江 林文 聂威 黄镕 刘齐洲 于 2020-06-30 设计创作，主要内容包括：本发明提出了一种烟碱纯化方法,包括：将待处理的烟碱投入到短程分子蒸馏器中,在温度为20-60℃,压力为10-20mbar条件下精馏,取重组分,将重组分再次投入到短程分子蒸馏器中,在温度为40-80℃,压力为0.01-1mbar条件下精馏,取轻组分,将轻组分溶解于流动相中,由进样阀进入已建立固定相-流动相动态平衡的高速逆流色谱仪中,利用紫外检测器图谱或高效液相色谱收集烟碱溶液,浓缩烟碱溶液既得到高纯度烟碱,本发明的烟碱纯化方法简单,且该纯化方法能够大幅度降低生产投入,提高烟碱的纯度和收率。(The invention provides a nicotine purification method, which comprises the following steps: putting nicotine to be treated into a short-range molecular distiller, rectifying under the conditions of temperature of 20-60 ℃ and pressure of 10-20mbar, taking heavy components, putting the heavy components into the short-range molecular distiller again, rectifying under the conditions of temperature of 40-80 ℃ and pressure of 0.01-1mbar, taking light components, dissolving the light components into a mobile phase, introducing the light components into a high-speed counter-current chromatograph with established stationary phase-mobile phase dynamic balance through a sample introduction valve, collecting nicotine solution by utilizing an ultraviolet detector spectrum or a high performance liquid chromatography, and concentrating the nicotine solution to obtain high-purity nicotine.)

1. A method of nicotine purification comprising the steps of:

step one, putting nicotine to be treated into a short-range molecular distiller, and rectifying at the temperature of 20-60 ℃ and under the pressure of 10-20mbar to obtain heavy components;

step two, putting the heavy component obtained in the step one into a short-distance molecular distiller again, rectifying the heavy component at the temperature of 40-80 ℃ and under the pressure of 0.01-1mbar, and taking a light component;

dissolving the light component obtained in the step two in a mobile phase, feeding the light component into a high-speed counter-current chromatograph with established stationary phase-mobile phase dynamic balance through a sample injection valve, and collecting nicotine solution by utilizing an ultraviolet detector spectrum or a high performance liquid chromatography;

and step four, concentrating the nicotine solution obtained in the step three to obtain high-purity nicotine.

2. The method of nicotine purification according to claim 1, wherein in step one, the temperature is 40-60 ℃ and the pressure is 10-15 mbar.

3. The nicotine purification process according to claim 1, wherein in step two, the temperature is 60-80 ℃ and the pressure is 0.01-0.05 mbar.

4. The nicotine purification method according to claim 1, wherein in step three, the method for establishing stationary phase-mobile phase dynamic equilibrium by high-speed countercurrent chromatography comprises:

step one, respectively preparing a stationary phase solvent system and a mobile phase solvent system;

filling the high-speed counter-current chromatograph with the stationary phase, setting the temperature of the constant-temperature circulator, adjusting the rotating speed of a host of the high-speed counter-current chromatograph, finally pumping the mobile phase, detecting by using an ultraviolet detector, and when the mobile phase flows out obviously, establishing the stationary phase-mobile phase dynamic balance by the high-speed counter-current chromatograph.

5. The method of purifying nicotine according to claim 4, wherein the fixed phase solvent system and the mobile phase solvent system are prepared by mixing petroleum ether, ethyl acetate, methanol and water, stirring them uniformly, standing and layering, and taking the upper layer as the fixed phase and the lower layer as the mobile phase.

6. The nicotine purification method of claim 5, wherein the petroleum ether: ethyl acetate: methanol: the volume ratio of water is (3-5): (3-5): (4-7): (3-6).

7. The nicotine purification method of claim 6, wherein the petroleum ether: ethyl acetate: methanol: the volume ratio of water is (3-4): (3-4): (5-6): (5-6).

8. The nicotine purification method according to claim 4, wherein in step two, the temperature of the constant temperature circulator is 20-30 ℃.

9. The nicotine purification method as claimed in claim 4, wherein in the second step, the rotation speed of the high-speed countercurrent chromatograph is 800-1200 r/min.

10. The nicotine purification method of claim 4, in which the mobile phase is pumped at a rate of 0.5 to 5 ml/min.

Technical Field

The invention relates to the technical field of purification of natural products, in particular to a nicotine purification method.

Background

Nicotine, also called nicotine, is an important pharmaceutical and chemical raw material, which is mainly extracted from tobacco leaves or tobacco stems, wherein in the current industrial production, alkali liquor is adopted to extract free nicotine from tobacco raw materials, and then the free nicotine is extracted by an organic solvent, and then the free nicotine is extracted by an acid liquor and an organic solvent to obtain nicotine with relatively high purity, because the boiling point difference of the nicotine and the conventional organic solvent is large, partial impurities with high boiling points, such as dehydroneonicotine, meslamine, cotinine, L (-) -octagon and the like, can exist in the nicotine obtained by rectification and extraction of the organic solvent, wherein the partial impurities, such as mestamine and cotinine, are quite close to the boiling point of the nicotine, the impurities are difficult to separate by the way of separation of the boiling point difference, although different products can be effectively separated by the way of adsorption separation of resin, a large amount of solvent and time can still be consumed for cleaning and reducing the resin after separation, thereby reducing the efficiency of the purification of the whole nicotine and easily generating a waste solvent.

Therefore, how to provide a nicotine purification method which has an industrial application prospect, can effectively purify nicotine and is not easy to generate three wastes is called a technical problem which needs to be solved urgently in the field.

Disclosure of Invention

In view of the above, the present invention provides a purification method of nicotine, which can effectively separate nicotine with similar boiling points and less waste solvent.

The technical scheme of the invention is realized as follows: the invention provides a nicotine purification method, which comprises the following steps:

step one, putting nicotine to be treated into a short-range molecular distiller, and rectifying at the temperature of 20-60 ℃ and under the pressure of 10-20mbar to obtain heavy components;

step two, putting the heavy component obtained in the step one into a short-distance molecular distiller again, rectifying the heavy component at the temperature of 40-80 ℃ and under the pressure of 0.01-1mbar, and taking a light component;

dissolving the light component obtained in the step two in a mobile phase, feeding the light component into a high-speed counter-current chromatograph with established stationary phase-mobile phase dynamic balance through a sample injection valve, and collecting nicotine solution by utilizing an ultraviolet detector spectrum or a high performance liquid chromatography;

and step four, concentrating the nicotine solution obtained in the step three to obtain high-purity nicotine.

On the basis of the technical scheme, preferably, in the step one, the temperature is 40-60 ℃, and the pressure is 10-15 mbar.

On the basis of the technical scheme, preferably, in the second step, the temperature is 60-80 ℃, and the pressure is 0.01-0.05 mbar.

On the basis of the above technical solution, preferably, in step three, the method for establishing the stationary phase-mobile phase dynamic equilibrium by the high-speed countercurrent chromatograph includes:

step one, respectively preparing a stationary phase solvent system and a mobile phase solvent system;

filling the high-speed counter-current chromatograph with the stationary phase, setting the temperature of the constant-temperature circulator, adjusting the rotating speed of a host of the high-speed counter-current chromatograph, finally pumping the mobile phase, detecting by using an ultraviolet detector, and when the mobile phase flows out obviously, establishing the stationary phase-mobile phase dynamic balance by the high-speed counter-current chromatograph.

More preferably, the preparation method of the stationary phase solvent system and the mobile phase solvent system comprises the steps of mixing and stirring petroleum ether, ethyl acetate, methanol and water uniformly, standing for layering, taking the upper layer as the stationary phase, and taking the lower layer as the mobile phase.

On the basis of the above technical solution, preferably, the petroleum ether: ethyl acetate: methanol: the volume ratio of water is (3-5): (3-5): (4-7): (3-6).

On the basis of the above technical solution, preferably, the petroleum ether: ethyl acetate: methanol: the volume ratio of water is (3-4): (3-4): (5-6): (5-6).

On the basis of the above technical solution, preferably, in the second step, the temperature of the constant temperature circulator is 20 to 30 ℃.

On the basis of the above technical solution, preferably, in the step two, the rotation speed of the host of the high-speed countercurrent chromatograph is 800-.

On the basis of the technical scheme, the pumping speed of the mobile phase is preferably 0.5-5 ml/min.

Compared with the prior art, the nicotine purification method has the following beneficial effects:

(1) the method utilizes the short-path molecular distiller to carry out rectification twice on the nicotine crude product, respectively removes low-boiling impurities and high-boiling impurities, reduces the types of the impurities in the nicotine crude product, and then utilizes the high-speed counter-current chromatograph to carry out impurity separation, does not need the high-temperature process of conventional rectification, does not need a large amount of cost brought by adsorption of a resin tower and the cleaning treatment flow of the resin tower, has high production efficiency, can produce more pure nicotine as far as possible, and has good application prospect;

(2) the whole purification method has simple steps, the distillation efficiency of the short-range molecular distiller is high, nicotine can be prevented from being at a higher temperature, more impurities are avoided, and after primary impurity separation, the nicotine is purified by using a more accurate high-speed counter-current chromatograph, so that the investment of raw materials can be reduced, the yield is improved, and meanwhile, the operation method is simple and has a good application prospect.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a gas chromatography-mass spectrum of a nicotine solution of the heavy component obtained in example 1;

FIG. 2 is a gas chromatography-mass spectrum of a nicotine solution of the light fraction obtained in example 1;

FIG. 3 is a gas chromatography-mass spectrum of the high purity nicotine solution obtained in example 1.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.