阅读说明：本技术 一种柠檬苦素提取液的制备方法 (Preparation method of limonin extracting solution ) 是由 廖劲松 于 2020-12-02 设计创作，主要内容包括：本发明属于农产品深加工技术领域,具体涉及一种柠檬苦素提取液的制备方法。通过将柑橘类果皮,风干,洗涤、干燥,粉碎,过筛；粉体加入到甲醇与甲醚的混合溶液中在辅助超声的条件下进行提取,过滤,得到提取液。通过采用了甲醇与甲醚两种溶剂进行复配作为提取剂提取,两种之间具有优异的协同作用,进而提高了柠檬苦素的提取率,而且在超声辅助条件下,能够缩短提取时间,提高提取率。(The invention belongs to the technical field of deep processing of agricultural products, and particularly relates to a preparation method of a limonin extracting solution. Through drying orange peel in air, washing, drying, crushing and sieving; adding the powder into a mixed solution of methanol and dimethyl ether, extracting under the condition of auxiliary ultrasound, and filtering to obtain an extracting solution. By adopting two solvents of methanol and methyl ether to carry out compounding to be used as an extracting agent for extraction, the two solvents have excellent synergistic effect, so that the extraction rate of the limonin is improved, and the extraction time can be shortened and the extraction rate can be improved under the ultrasonic-assisted condition.)

1. A preparation method of limonin extracting solution is characterized by comprising the following steps: the preparation method comprises the following steps:

(1) air drying pericarp of citrus, washing, drying, pulverizing, and sieving;

(2) and (2) adding the powder obtained in the step (1) into a mixed solution of methanol and dimethyl ether, extracting under the condition of auxiliary ultrasound, and filtering to obtain an extracting solution.

2. The method for preparing limonin extracting solution according to claim 1, wherein the method comprises the following steps: in the step (1), the citrus peel is lemon peel.

3. The method for preparing limonin extracting solution according to claim 1, wherein the method comprises the following steps: in the step (1), the sieving is to sieve through 170-200 meshes.

4. The method for preparing limonin extracting solution according to claim 1, wherein the method comprises the following steps: in the step (1), the drying temperature is 100-120 ℃, and the drying time is 3-5 h.

5. The method for preparing limonin extracting solution according to claim 1, wherein the method comprises the following steps: in the step (2), the extraction temperature is 30-40 ℃, and the ultrasonic time is 30-60 min.

6. The method for preparing limonin extracting solution according to claim 1, wherein the method comprises the following steps: in the step (2), the filtration is to remove residues by adopting 200-mesh filter cloth.

7. The method for preparing limonin extracting solution according to claim 1, wherein the method comprises the following steps: in the step (2), the volume ratio of the methanol to the dimethyl ether is as follows: 3-5: 1.

8. The method for preparing limonin extracting solution according to claim 1, wherein the method comprises the following steps: in the step (2), the ratio of the mixed solution to the powder is 10-15 mL:1 g.

Technical Field

The invention belongs to the technical field of deep processing of agricultural products. More particularly, relates to a preparation method of a limonin extracting solution.

Background

Lemon belongs to evergreen arbor of Citrus of Rutaceae of Magnoliaceae, and is called Yimuguo or Yimuzi because of its extremely sour taste and preference for pregnant women with liver deficiency. Lemon contains abundant citric acid, so it is known as "citric acid warehouse". Limonin is a bitter substance of lemon which is widely researched in recent years, and belongs to an oxidative tetracyclic triterpenoid organic matter. Animal experiments prove that the compound has the functions of effectively reducing blood fat, promoting intestinal colony balance, improving neural excitability, preventing tumors, improving immunity and the like, and has extremely high enrichment and development values.

The limonin is extracted by organic solvent method, Soxhlet extraction method, reflux extraction method, supercritical extraction method and ultrasonic extraction method. LIU L optimizes the extraction process of limonin in fructus Aurantii Immaturus, and compares the extraction effects of chloroform, methanol, acetone, ethanol, diethyl ether, etc., to find that diethyl ether is the worst, and acetone and ethanol are the best. In the experiment, the lemon peel is pretreated by microwave, drying, crushing, sieving with a 18-mesh sieve and the like, and petroleum ether is used as a degreasing agent and acetone is used as an extracting agent, so that the extraction time is shortened and the extraction efficiency of limonoid is improved.

However, the problem of low extraction rate exists in the prior art of extracting functional limonin from pericarp residues. Therefore, a method for preparing a limonin extracting solution with high extraction rate is needed.

Disclosure of Invention

The invention aims to solve the technical problem of overcoming the defect and the defect of low extraction rate of the existing limonin and provides a preparation method of a limonin extracting solution.

The above purpose of the invention is realized by the following technical scheme:

a preparation method of limonin extracting solution comprises the following steps:

(1) air drying pericarp of citrus, washing, drying, pulverizing, and sieving;

(2) and (2) adding the powder obtained in the step (1) into a mixed solution of methanol and dimethyl ether, extracting under the condition of auxiliary ultrasound, and filtering to obtain an extracting solution.

Preferably, in step (1), the citrus peel is a lemon peel.

Preferably, in the step (1), the sieving is 170-200 mesh sieving.

Preferably, in the step (1), the drying temperature is 100-120 ℃, and the drying time is 3-5 hours;

preferably, in the step (2), the extraction temperature is 30-40 ℃, and the ultrasonic time is 30-60 min.

Preferably, in the step (2), the filtration is performed by filtering with a 200-mesh filter cloth to remove residues.

Preferably, in the step (2), the volume ratio of methanol to dimethyl ether is: 3-5: 1.

Preferably, in the step (2), the ratio of the mixed solution to the powder is 10-15 mL:1 g.

The invention has the following beneficial effects:

according to the preparation method of the limonin extracting solution, two solvents of methanol and methyl ether are compounded to be used as an extracting agent for extraction, the two solvents have an excellent synergistic effect, so that the extraction rate of the limonin is improved, and the extraction time can be shortened and the extraction rate can be improved under the ultrasonic auxiliary condition.

Detailed Description

The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.

Unless otherwise indicated, reagents and materials used in the following examples are commercially available.

Example 1

A preparation method of limonin extracting solution comprises the following steps:

(1) drying orange peel in air, washing, drying, pulverizing, and sieving with 200 mesh sieve; the drying temperature is 110 ℃, the drying time is 4h,

(2) adding the powder obtained in the step (1) into a mixed solution of methanol and dimethyl ether, extracting under the condition of auxiliary ultrasound, wherein the extraction temperature is 35 ℃, the ultrasound time is 40min, and filtering by using a 200-mesh filter cloth to remove residues to obtain an extracting solution; the volume ratio of the methanol to the dimethyl ether is as follows: 4: 1; the ratio of the mixed solution to the powder is 12mL:1 g.

Example 2

A preparation method of limonin extracting solution comprises the following steps:

(1) drying orange peel in air, washing, drying, pulverizing, and sieving with 200 mesh sieve; the drying temperature is 120 ℃, the drying time is 3 hours,

(2) adding the powder obtained in the step (1) into a mixed solution of methanol and dimethyl ether, extracting under the condition of auxiliary ultrasound, wherein the extraction temperature is 30 ℃, the ultrasound time is 60min, and filtering by using a 200-mesh filter cloth to remove residues to obtain an extracting solution; the volume ratio of the methanol to the dimethyl ether is as follows: 5: 1; the ratio of the mixed solution to the powder is 15mL:1 g.

Example 3

A preparation method of limonin extracting solution comprises the following steps:

(1) drying citrus peel in the air, washing, drying, crushing and sieving with a 170-mesh sieve; the drying temperature is 100 ℃, the drying time is 5h,

(2) adding the powder obtained in the step (1) into a mixed solution of methanol and methyl ether, extracting under the condition of auxiliary ultrasound, wherein the extraction temperature is 40 ℃, the ultrasound time is 30min, and filtering with a 200-mesh filter cloth to remove residues to obtain an extracting solution; the volume ratio of the methanol to the dimethyl ether is as follows: 3: 1; the ratio of the mixed solution to the powder is 10mL to 1 g.

Comparative example 1

A preparation method of limonin extracting solution comprises the following steps:

(1) drying orange peel in air, washing, drying, pulverizing, and sieving with 200 mesh sieve; the drying temperature is 110 ℃, the drying time is 4h,

(2) adding the powder obtained in the step (1) into methanol, extracting under the condition of auxiliary ultrasound, wherein the extraction temperature is 35 ℃, the ultrasound time is 40min, and filtering by adopting a filter cloth of 200 meshes to remove residues to obtain an extracting solution; the ratio of the mixed solution to the powder is 12mL:1 g.

Comparative example 2

A preparation method of limonin extracting solution comprises the following steps:

(1) drying orange peel in air, washing, drying, pulverizing, and sieving with 200 mesh sieve; the drying temperature is 110 ℃, the drying time is 4h,

(2) adding the powder obtained in the step (1) into methyl ether, extracting under the condition of auxiliary ultrasound, wherein the extraction temperature is 35 ℃, the ultrasound time is 40min, and filtering by adopting a filter cloth of 200 meshes to remove residues to obtain an extracting solution; (ii) a The ratio of the mixed solution to the powder is 12mL:1 g.

Comparative example 3

A preparation method of limonin extracting solution comprises the following steps:

(1) drying orange peel in air, washing, drying, pulverizing, and sieving with 200 mesh sieve; the drying temperature is 110 ℃, the drying time is 4h,

(2) adding the powder obtained in the step (1) into a mixed solution of methanol and methyl ether for extraction at 35 ℃ for 40min, and filtering with a 200-mesh filter cloth to remove residues to obtain an extracting solution; the volume ratio of the methanol to the dimethyl ether is as follows: 4: 1; the ratio of the mixed solution to the powder is 12mL:1 g.

The total yield of the limonoid components of examples 1-3 and comparative examples 1-3 was determined by a liquid chromatography method. Specific chromatographic conditions were as follows:

a chromatographic column: UItimate AQ-C18(2.1 mm. times.100 mm); mobile phase: acetonitrile-water (45: 55, volume ratio); column temperature: 30 ℃; flow rate: 0.21 mL/min; detection wavelength: 210 nm; sample introduction amount: 0.8. mu.L.

Through the comparison examples of examples 1-3 and comparison examples 1-3, the preparation method provided by the invention is adopted, two solvents of methanol and methyl ether are used as extracting agents for extraction, and the two solvents have excellent synergistic effect, so that the extraction rate of limonin is improved, and the extraction time can be shortened and the extraction rate can be improved under the ultrasonic-assisted condition.

The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.