Valerenic acid and extraction method thereof

Abstract

The invention provides valerenic acid and an extraction method thereof, and belongs to the technical field of biochemistry. According to the method, valerianoic acid is extracted from valerian, valerianoic acid powder is obtained through first reflux extraction, impurity adsorption by activated carbon, dissolution by hot water and second reflux extraction in sequence, and the content of valerianoic acid reaches 6%-9%. According to the method for extracting the valerenic acid, provided by the invention, a chromatographic refining step in a traditional method is abandoned, expensive extraction equipment is not adopted, and low-boiling-point volatile organic solvents (such as petroleum ether, ethyl acetate and the like) are not used, so that the extraction cost of the valerenic acid is reduced, and the yield of the valerenic acid is also improved.

Description

Technical Field

[0001] The invention relates to the technical field of biochemistry, and in particular to valeric acid and an extraction method thereof. Background Art

[0002] Valerian is a perennial herb with multiple medicinal and edible values. Its active ingredients mainly include monoterpenes, sesquiterpenes, cycloterpenes, alkaloids, flavonoids, lignans, etc., which have the following effects: (1) Antibacterial and anti-inflammatory, can inhibit a variety of bacteria and fungi, especially tuberculosis bacteria; (2) Enhance immunity and prevent the occurrence of autoimmune diseases such as eczema and asthma; (3) Prevent tumors; (4) Clear away heat and detoxify, suitable for patients with chronic diseases such as high fever, oral ulcers, etc.; (5) Diuretic and laxative, help promote urine excretion and relieve constipation; (6) Anti-inflammatory and antipruritic; (7) Tonify the spleen and digestion, can be used to treat indigestion, chronic enteritis, stomach pain, vomiting and other problems.

[0003] Valerenic acid is one of the characteristic components of valerian, which has a sedative and sleep-inducing effect. It can effectively induce the secretion of neuropeptide S, shorten the process of activating homologous receptors, and thus trigger intracellular Ca 2+ Mobilize, restore active sleep, reduce sleep latency, shorten sleep onset time, improve sleep depth, and wake up refreshed without hangover effect. In addition, valeric acid can enhance the response of γ-aminobutyric acid (GABA) receptors, change the transport and release of neurotransmitter GABA, inhibit sympathetic neurons, thereby eliminating depression and anxiety, and has sedative and anticonvulsant effects. It can be used to prepare safe, low-toxic, and effective sedative hypnotic and antianxiety drugs.

[0004] Currently, the extraction of valeric acid requires multiple reflux extractions and chromatography purifications, and the cost of chromatography purification is relatively high. Therefore, there is an urgent need for an extraction method that can reduce the extraction cost of valeric acid and increase the yield of valeric acid. Summary of the invention

[0005] The purpose of the present invention is to provide valerenic acid and an extraction method thereof, which abandons the chromatography purification step in the traditional method, reduces the extraction cost of valerenic acid, and improves the yield of valerenic acid.

[0006] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0007] The present invention provides a method for extracting valerene acid, comprising the following steps:

[0008] (1) First reflux extraction: After pretreatment, methanol solution is added to the broad-leaved valerian in a material-liquid mass ratio of 1:13-17, and reflux extraction is performed to obtain a valerian alcohol extract, which is cooled and filtered, and the filter residue is refluxed again for extraction, filtered, and the filtrates from the two extractions are combined;

[0009] (2) Activated carbon adsorbs impurities: Add activated carbon to the filtrate, stir, filter, concentrate and dry to obtain valerian extract;

[0010] (3) Dissolving in hot water: Add water to the valerian extract, heat and stir, filter, and discard the filtrate;

[0011] (4) Second reflux extraction: The filtered solid was added into anhydrous methanol for a second reflux extraction, cooled and filtered, concentrated and dried to obtain valeric acid.

[0012] Preferably, the step of pretreating the broadleaf valerian comprises: crushing the broadleaf valerian and passing it through a 20-mesh sieve to obtain valerian particles of which 80% to 100% pass through the 20-mesh sieve.

[0013] Preferably, the reflux extraction time is 3.5 to 5 hours, the extraction temperature is 60 to 65°C, and the cooling temperature is 38 to 45°C.

[0014] Preferably, the final concentration of the activated carbon is 5 to 10 g / L, and the stirring time is 2 to 3 h.

[0015] Preferably, after water is added to the valerian extract, the mass percentage of the valerian extract is 1.2-1.5%, the temperature of heating and stirring is 60-70° C., and the time is 2-3 hours.

[0016] Preferably, the mass percentage of the solid after adding anhydrous methanol is 4%-6%; the time of the second reflux extraction is 1-2h, and the extraction temperature is 60-65°C; the cooling temperature is 38-45°C.

[0017] The present invention also provides valerene acid prepared by the valerene acid extraction method.

[0018] The beneficial effects of the present invention compared with the prior art are:

[0019] (1) The method for extracting valerian acid from valerian of the present invention sequentially undergoes a first reflux extraction, activated carbon adsorption of impurities, hot water dissolution, and a second reflux extraction to obtain valerian acid powder, wherein the content of valerian acid reaches 6.0%-9.0%.

[0020] (2) The valerenic acid extraction method provided by the present invention abandons the chromatography purification step in the traditional method, does not use expensive extraction equipment, and does not use low-boiling point, easily volatile organic solvents (such as petroleum ether, ethyl acetate, etc.), thereby reducing the extraction cost of valerenic acid and improving the yield of valerenic acid. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0022] Figure 1 The figure is a flow chart of the extraction of valerene acid of the present invention. DETAILED DESCRIPTION

[0023] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as limiting the present invention, but should be understood as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0024] It should be understood that the terms described in the present invention are only for describing special embodiments and are not intended to limit the present invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper and lower limits of the scope is also specifically disclosed. Each smaller range between the intermediate value in any stated value or stated range and any other stated value or intermediate value in the described range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the scope.

[0025] Unless otherwise indicated, all technical and scientific terms used herein have the same meanings as those generally understood by those skilled in the art. Although the present invention describes only preferred methods and materials, any methods and materials similar or equivalent to those described herein may also be used in the implementation or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and / or materials associated with the documents. In the event of a conflict with any incorporated document, the content of this specification shall prevail.

[0026] It will be apparent to those skilled in the art that various modifications and variations may be made to the specific embodiments of the present invention description without departing from the scope or spirit of the present invention. Other embodiments derived from the present invention description will be apparent to those skilled in the art. The present invention description and examples are exemplary only.

[0027] The words “include,” “including,” “have,” “contain,” etc. used in this document are open-ended terms, meaning including but not limited to.

[0028] The present invention provides a method for extracting valeric acid, the process of which is as follows: Figure 1 As shown, the following steps are included:

[0029] (1) First reflux extraction: After pretreatment, methanol solution is added to the broad-leaved valerian in a material-liquid mass ratio of 1:13-17, and reflux extraction is performed to obtain a valerian alcohol extract, which is cooled and filtered, and the filter residue is refluxed again for extraction, filtered, and the filtrates from the two extractions are combined;

[0030] (2) Activated carbon adsorbs impurities: Add activated carbon to the filtrate, stir, filter, concentrate and dry to obtain valerian extract;

[0031] (3) Dissolving in hot water: Add water to the valerian extract, heat and stir, filter, and discard the filtrate;

[0032] (4) Second reflux extraction: The filtered solid was added into anhydrous methanol for a second reflux extraction, cooled and filtered, concentrated and dried to obtain valeric acid.

[0033] Preferably, the reflux extraction time is 3.5 to 5 hours, more preferably 4 hours; the extraction temperature is 60 to 65°C; the cooling temperature is 38 to 45°C, more preferably 40°C.

[0034] Preferably, the final concentration of the activated carbon is 5 to 10 g / L, more preferably 6.6 g / L; the stirring time is 2 to 3 h, more preferably 2 h.

[0035] Preferably, after adding water to the valerian extract, the mass percentage of the valerian extract is 1.2-1.5%, more preferably 1.2%; the temperature of heating and stirring is 60-70°C, more preferably 70; and the time is 2-3h, more preferably 2h.

[0036] Preferably, the mass percentage of the solid after adding anhydrous methanol is 4%-6%, more preferably 4%; the time for the second reflux extraction is 1 to 2 hours, more preferably 1 hour; the extraction temperature is 60 to 65°C, more preferably 65°C; the cooling temperature is 38 to 45°C, more preferably 40°C.

[0037] Example 1

[0038] Embodiment 1 of the present invention provides a method for extracting valerene acid, and the specific steps are as follows:

[0039] (1) Select broadleaf valerian, grind it, and pass it through a 20-mesh sieve to obtain valerian granules of which at least 80% pass through the 20-mesh sieve; take 200 grams of valerian granules, add 15 times the weight of methanol solution to the valerian granules, and reflux extract for 4 hours at an extraction temperature of 65° C. to obtain valerian alcohol extract, cool the 65° C. solution to 40° C., and filter it by suction. Repeat the extraction of the residue according to the first extraction step.

[0040] (2) Combine the filtrates, add 20 g of activated carbon to the filtrates, stir at room temperature for 2 hours, filter, and vacuum concentrate to dryness at 60°C to obtain valerian extract.

[0041] (3) 4 L of water was added to the valerian extract, heated to 70° C. and stirred for 2 hours, cooled to room temperature, filtered and dried as much as possible to obtain 18.20 g of a solid sample with a valerene acid content of 7.507%.

[0042] (4) Secondary reflux: add the filtered solid into 1 L of anhydrous methanol and reflux for 1 hour at an extraction temperature of 65°C, cool to 40°C, filter, and concentrate the filtrate to dryness under vacuum at 60°C to obtain 4.17 g of product with a valeric acid content of 8.713%.

[0043] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for extracting valerene acid, characterized in that: The steps include: (1) First reflux extraction: After pretreatment, methanol solution is added to the broad-leaved valerian in a material-liquid mass ratio of 1:13-17, and reflux extraction is performed to obtain a valerian alcohol extract, which is cooled and filtered, and the filter residue is refluxed again for extraction, filtered, and the filtrates from the two extractions are combined; (2) Activated carbon adsorbs impurities: Add activated carbon to the filtrate, stir, filter, concentrate and dry to obtain valerian extract; (3) Dissolving in hot water: Add water to the valerian extract, heat and stir, filter, and discard the filtrate; (4) Second reflux extraction: The filtered solid was added into anhydrous methanol for a second reflux extraction, cooled and filtered, concentrated and dried to obtain valeric acid.

2. The method for extracting valerene acid according to claim 1, characterized in that: In step (1), the step of pre-treating the broad-leaved valerian includes: crushing the broad-leaved valerian and passing it through a 20-mesh sieve to obtain valerian particles of which 80% to 100% pass through the 20-mesh sieve.

3. The method for extracting valerene acid according to claim 1, characterized in that: In step (1), the reflux extraction time is 3.5 to 5 hours, the extraction temperature is 60 to 65°C; the cooling temperature is 38 to 45°C.

4. The method for extracting valerene acid according to claim 1, characterized in that: In step (2), the final concentration of the activated carbon is 5 to 10 g / L, and the stirring time is 2 to 3 h.

5. The method for extracting valerene acid according to claim 1, characterized in that: In step (3), after water is added to the valerian extract, the mass percentage of the valerian extract is 1.2-1.5%, the temperature of heating and stirring is 60-70° C., and the time is 2-3 hours.

6. The method for extracting valerene acid according to claim 1, characterized in that: In step (4), the mass percentage of the solid after adding anhydrous methanol is 4%-6%; the time of the second reflux extraction is 1-2h, and the extraction temperature is 60-65°C; the cooling temperature is 38-45°C.

7. Valerenic acid prepared by the method for extracting valerenic acid according to any one of claims 1 to 6.

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