阅读说明：本技术 提取茄尼醇的合溶剂及用该混合溶剂提取茄尼醇的方法 (Mixed solvent for extracting solanesol and method for extracting solanesol by using same ) 是由 刘京 刘家磊 何文清 韩小斌 刘明宏 彭玉龙 祝乾湘 芶剑渝 王小彦 黄纯杨 于 2020-07-02 设计创作，主要内容包括：本发明涉及一种使用有机溶剂提取茄尼醇的方法,茄尼醇属于弱极性物质,弱极性的提取溶剂比如正己烷对茄尼醇具有较好的溶解度,但是穿透力较弱。本发明使用一种混合溶剂提取茄尼醇,混合溶剂使用弱极性的正己烷和强极性的冰醋酸以体积比3∶1进行混合得到。具体步骤如下：(1)使用干燥箱烘干烟叶,测其含水量；(2)制作茄尼醇-正己烷冰醋酸溶液标准曲线；(3)使用去离子水加热浸提并过滤；(4)使用正己烷-冰醋酸混合溶剂进行浸提并改变提取条件优化提取工艺。最终得到优化后的提取工艺：提取温度为60℃、提取时间为6h、提取次数为2次、液固比为20mL/g。(The invention relates to a method for extracting solanesol by using an organic solvent, wherein the solanesol belongs to a low-polarity substance, and the low-polarity extraction solvent such as n-hexane has better solubility to the solanesol but weaker penetrating power. The invention uses a mixed solvent to extract solanesol, and the mixed solvent is obtained by mixing weak-polarity n-hexane and strong-polarity glacial acetic acid according to the volume ratio of 3: 1. The method comprises the following specific steps: (1) drying the tobacco leaves by using a drying oven, and measuring the water content of the tobacco leaves; (2) making a solanesol-n-hexane glacial acetic acid solution standard curve; (3) heating and leaching by using deionized water and filtering; (4) the extraction is carried out by using a mixed solvent of n-hexane and glacial acetic acid and changing the extraction conditions to optimize the extraction process. Finally, the optimized extraction process is obtained: the extraction temperature is 60 deg.C, the extraction time is 6h, the extraction times is 2 times, and the liquid-solid ratio is 20 mL/g.)

1. A mixed solvent for extracting solanesol is characterized in that: the solvent is prepared from weak-polarity n-hexane and strong-polarity glacial acetic acid in a volume ratio of 3: 1 are mixed to obtain the product.

2. A method for extracting solanesol by using an organic solvent is characterized by comprising the following steps:

(1) removing stems of waste and inferior tobacco leaves, and drying the waste and inferior tobacco leaves in a drying oven until the moisture content of the tobacco leaves is 5%;

(2) crushing the tobacco leaves with water removed, adding 1.5-2 parts of deionized water into 1 part of tobacco leaf powder according to the mass ratio, leaching the tobacco at 50 ℃ for 5 hours to reduce water-soluble impurities in the tobacco, and drying filter residues after filtering;

(3) putting the dried filter residue obtained in the step (2) into a container, adding a mixed solvent to extract the solanesol, wherein the mixed solvent comprises weak-polarity n-hexane and strong-polarity glacial acetic acid in a volume ratio of 3: 1, mixing to obtain the product; the extraction conditions comprise extraction temperature of 60 deg.C, extraction time of 6h, extraction frequency of 2 times, and liquid-solid ratio of 20 mL/g.

3. The method for extracting solanesol using organic solvent as claimed in claim 1, wherein: the water-soluble impurities in the tobacco are nicotine, inorganic salt and citric acid.

Technical Field

The invention relates to the field of tobacco, in particular to a mixed solvent for extracting solanesol and a method for extracting the solanesol by using the mixed solvent.

Background

There are many methods for extracting solanesol, such as ultrasonic-assisted extraction, microwave-assisted extraction, supercritical CO₂Extraction methods and organic solvent extraction. The ultrasonic wave auxiliary extraction is restricted by ultrasonic attenuation factors, and the equipment investment is large; the microwave-assisted extraction equipment is complex and high in price, and the solvent selection range is narrow; supercritical CO₂The extraction method also has the restriction of large equipment investment. Organic solvent extraction is still an important extraction method, but as the solanesol is a low-polarity substance, the low-polarity solvent should be selected for extracting the solanesol according to the similar compatibility principle. However, the weak polar solvent has low penetrating power, is difficult to penetrate tissues such as cell walls, cell membranes and the like, has slow extraction process, and the existing strong polar solvent methanol has good extraction effect on the solanesol, but has high toxicity and is not beneficial to environmental protection.

Meanwhile, the existing method for extracting solanesol has lower extraction rate and larger waste, for example, the patent name is a method for extracting solanesol from waste tobacco leaves, application number 201610316518, the invention patent discloses a method for extracting solanesol from waste tobacco leaves, the concentration of the solanesol is completed by utilizing the solubility difference of the solanesol in different organic solvents according to the solvent distribution proportion, and the characteristics of dissolution of pure solanesol in the solvent when being heated and crystallization when being frozen are utilized to achieve the purification, and the method comprises the following process steps: extracting → saponifying → extracting → dewaxing → degreasing → purifying to obtain the final product of solanesol; the method for extracting the solanesol from the waste tobacco leaves has the advantages of simple process, low cost, short realization time, high efficiency, low energy consumption and easy realization of industrialization and scale production. However, in the examples, it can be seen that 200 kg of jin tobacco leaves can obtain 1.92 kg of solanesol, and the extraction rate is 0.96%. The patent name is a method for extracting high-purity solanesol from tobacco leaves, and the application number is 201610075560; in the examples, the amount of solanesol obtained from 50g of tobacco leaves was 0.32g, and the extraction rate was 0.64%. Therefore, the extraction rate of the solanesol extracted by the prior art is low.

Disclosure of Invention

The technical problem to be solved by the invention is to provide a synthetic solvent for extracting solanesol and a method for extracting solanesol by using the same, which can improve the polarity of a solvent system, accelerate the extraction process and have less influence on the environment by the solvent system, and can overcome the defects of the prior art.

The technical scheme of the invention is as follows: a mixed solvent for extracting solanesol is prepared by mixing weak polar n-hexane and strong polar glacial acetic acid in a volume ratio of 3: 1 are mixed to obtain the product.

The method for extracting solanesol by using organic solvent includes the following steps

(1) Removing stems of waste and inferior tobacco leaves, and drying the waste and inferior tobacco leaves in a drying oven until the moisture content of the tobacco leaves is 5%;

(2) crushing the tobacco leaves with water removed, adding 1.5-2 parts of deionized water into 1 part of tobacco leaf powder according to the mass ratio, leaching the tobacco at 50 ℃ for 5 hours to reduce water-soluble impurities in the tobacco, and drying filter residues after filtering;

(3) putting the dried filter residue obtained in the step (2) into a container, adding a mixed solvent to extract the solanesol, wherein the mixed solvent comprises weak-polarity n-hexane and strong-polarity glacial acetic acid in a volume ratio of 3: 1, mixing to obtain the product; the extraction conditions comprise extraction temperature of 60 deg.C, extraction time of 6h, extraction frequency of 2 times, and liquid-solid ratio of 20 mL/g.

The water-soluble impurities in the tobacco are nicotine, inorganic salt and citric acid.

Compared with the prior art, the invention aims at the problems of the existing solanesol extraction by adopting an organic solvent, prepares the mixed solvent for extracting the solanesol with the effect far exceeding the existing extraction rate, and adopts weak-polarity normal hexane and strong-polarity glacial acetic acid in a volume ratio of 3: 1, the glacial acetic acid has higher polarity, compared with a single n-hexane extraction solvent, the added glacial acetic acid can improve the polarity of an extracting solution, is favorable for penetrating cell membranes and other structures to accelerate the extraction mass transfer process, has lower toxicity and less environmental pollution compared with a methanol extraction solvent, and can ensure that the boiling point of an extraction solvent system is increased and the solvent is not easy to volatilize in the extraction process. Therefore, under the solvent system, only two times of extraction are needed to be carried out on the tobacco, so that the extraction times are reduced, and the consumption of the extraction time is reduced. The solvent system has the advantages of low cost, little environmental pollution and high extraction speed.

Meanwhile, the invention optimizes the use process of the mixed solvent for extracting the solanesol to obtain the optimal use process of the mixed solvent for extracting the solanesol, wherein the extraction temperature is 60 ℃, the extraction time is 6h, the extraction times are 2 times, and the liquid-solid ratio is 20mL/g, so that the extraction process of the solanesol can be increased to 2.85 percent, and the two patents which are far beyond the background technology break through the barriers of the prior art.

Drawings

FIG. 1 is a standard graph of a solanesol solution;

FIG. 2 is a graph showing the effect of liquid-solid ratio on extraction yield;

FIG. 3 is a graph of the effect of extraction time on extraction yield;

FIG. 4 is a graph of the effect of extraction times on extraction yield;

fig. 5 is a graph of the effect of extraction temperature on extraction yield.

Detailed Description