CN112999252A - Industrial method for continuously extracting high-content marigold flavone - Google Patents

Industrial method for continuously extracting high-content marigold flavone Download PDF

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CN112999252A
CN112999252A CN202110232550.6A CN202110232550A CN112999252A CN 112999252 A CN112999252 A CN 112999252A CN 202110232550 A CN202110232550 A CN 202110232550A CN 112999252 A CN112999252 A CN 112999252A
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marigold
content
flavone
extraction
extracting high
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CN112999252B (en
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高兰兰
吴迪
崔平永
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Chenguang Biotech Group Co Ltd
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    • A61K36/185—Magnoliopsida (dicotyledons)
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    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH

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Abstract

The invention discloses an industrialized method for continuously extracting high-content marigold flavone, which comprises the following steps of 1) granulating marigold raw materials, wherein the compression ratio of a ring die of a granulator is 1 (1.2-2.2); 2) extracting the marigold flower particles by using 70-100% of acetone as an extracting agent, and filtering to obtain an extracting solution; 3) and adjusting the volume fraction of acetone to 0-30%, filtering to obtain a filter cake, and drying the filter cake to obtain the marigold flavone product. The method is simple, high in continuity and operability, high in productivity, low in energy consumption and suitable for industrial production.

Description

Industrial method for continuously extracting high-content marigold flavone
Technical Field
The invention belongs to the technical field of natural plant extraction, and particularly relates to an industrial method for continuously extracting high-content marigold flavone.
Background
Tagetes erecta (Tagetes erecta L) is an annual herb of the genus Tagetes of the family Compositae. Has the effects of clearing away heat and toxic materials, eliminating phlegm, and relieving cough; it has fragrance and can be used as aromatic; has been used as bacteriostatic, sedative and antispasmodic. Marigold flower mainly contains flavonoid, glycosides, amino acids, vitamins, pigment, etc. The marigold flavone is yellow green powder extracted from marigold flowers, the main component of the marigold flavone is quercitin, which accounts for about 80 percent of the marigold flavone, and the marigold flavone has important pharmacological actions of resisting inflammation, resisting allergy, reducing blood pressure, resisting arrhythmia, resisting platelet aggregation, resisting oxidation, resisting tumors and the like.
At present, the main method for extracting the pharmacological active ingredients in the marigold flower is a step-by-step extraction method, namely, firstly, the lutein is extracted by using hexane solvent, and then, the marigold flower residue is treated by using the solvent to obtain the marigold flavonoid product. In addition, the related patent applications adopt mixed solvents to extract the lutein and marigold flavone at one time, and then separation and purification are carried out, for example, in Chinese patent application 201410104645.X, propanol-potassium hydroxide aqueous phase solvent is adopted to extract marigold petal powder, so as to obtain lutein and flavone crude products. In the technical scheme, a light-shielding reaction is required, and phase separation is required after extraction. For another example, chinese patent application 201811188771.2 uses a mixed solvent of petroleum ether and acetone to extract lutein and marigold flavonoids from marigold particles. The method needs phase separation after extraction, and the separation mode adopted in the scheme is separation after water is added, so that the operation is complex, and high-purity marigold flavone is obtained without separation.
In the prior art, the preparation method of high-purity marigold flavone mainly utilizes chromatographic separation. For example, Chinese patent application CN201410708334.4 discloses that marigold flavone with high purity is obtained by one-dimensional liquid chromatography and two-dimensional liquid chromatography. However, the separation amount of preparative liquid chromatography is small, the equipment price is expensive, and the method is not suitable for industrial production. Chinese patent application 201610108596.6 describes the preparation of high content marigold flavone by repeated centrifugation, filtration, washing and other steps. However, this method involves many steps requiring repeated operations, and is cumbersome.
Therefore, in order to obtain high-content marigold flavone, the prior art generally needs more complicated purification steps to realize, the complicated processes have high cost and are not suitable for the requirements of industrial production, and the report of obtaining the marigold flavone product with the content of more than or equal to 98 percent by simple extraction, concentration, filtration and drying is not seen at present.
Disclosure of Invention
Aiming at overcoming the defects of complex extraction operation, low product purity and the like of the existing marigold flavone. The invention provides an industrial method capable of simply and efficiently extracting marigold flavone, and the content of marigold flavone extract obtained by the process can reach more than 98%.
The invention relates to an industrial method for continuously extracting high-content marigold flavone, which comprises the following steps:
1) granulating the marigold flower raw material by using a granulator, wherein the compression ratio of a ring mould of the granulator is 1 (1.2-2.2);
2) extracting the marigold flower particles by using 70-100% of acetone as an extracting agent, and filtering to obtain an extracting solution;
3) and (3) adjusting the volume fraction of acetone in the extracting solution to 0-30%, filtering to obtain a filter cake, and drying the filter cake to obtain the marigold flavone product.
In order to better explain the technical scheme, the following concepts are further clarified:
the marigold raw material in the step 1) is fresh or dried marigold, or various commercially available processed forms of marigold, such as flower pulp; the 70% -100% acetone in the step 2) refers to the volume fraction of acetone of 70% -100%.
The technical parameters in the technical scheme of the invention can be further selected as follows:
the hardness of the granulated particles in the step 1) is 3-8 kg/cm2；
The extraction temperature in the step 2) is 40-60 ℃; preferably 45 to 55 ℃; further preferably 50-55 ℃;
the mass/volume (g/mL) ratio of the marigold flower particles to the extraction solvent in the step 2) is not less than 1: 2; preferably 1: (2-6); further preferably 1: (3-5); still more preferably 1: 4;
the extraction mode in the step 2) is preferably countercurrent extraction;
the extraction times in the step 2) are not less than 4; preferably 4 to 7 times.
In the step 2), the extraction time is 0.5-2.5 hours, preferably 1-2 hours; further preferably 1.5 hours.
The volume fraction of acetone in the step 2) is preferably 70-75%; or 70-80%; or 70-85%, or 70-90%; or 70-95%; or 70 to 100 percent; or 75-80%; or 75-85%; or 75-90%; or 75-95%; or 75-100%; or 80-85%; or 80-90%; or 80-95%; or 80-100%; or 85% -90%; or 85% -95%; or 85 to 100 percent; or 90-100%; or 92-99%; or 70 to 99 percent; or 75 to 99 percent; or 80 to 99 percent; or 85 to 99 percent; or 90 to 99 percent.
The invention discloses an optimized industrial method for continuously extracting high-content marigold flavone, which comprises the following steps:
1) granulating the marigold flower raw material by using a granulator, wherein the compression ratio of a ring mould of the granulator is 1 (1.2-2.2), and the hardness of the granulated granules is 3-8 kg/cm;
2) carrying out countercurrent extraction on the marigold flower particles by taking 70-100% of acetone as an extracting agent, wherein the mass/volume (g/mL) ratio of the marigold flower particles to an extracting solvent is not less than 1: 2; the extraction temperature is 40-60 ℃, and the extraction times are not less than 4; the extraction time is 0.5-2.5 hours each time; filtering to obtain extractive solution;
3) and (3) adjusting the volume fraction of acetone in the extracting solution to 0-30%, filtering to obtain a filter cake, and drying the filter cake to obtain the marigold flavone product.
According to the industrial method for continuously extracting the high-content marigold flavone, the mode of reducing the volume fraction of the organic solvent in the extracting solution in the step 3) can be concentration or adding a strong polar solvent.
The invention also provides a marigold flavone product prepared by the preparation process. The flavone content in the product is not less than 98%.
The invention has the beneficial effects that:
1. the method optimizes the pretreatment stage of marigold flower raw materials, granulates the raw materials, optimizes the ring die compression ratio of the granulator, creates precondition for large-scale extraction of high-content marigold flavone, and simultaneously finds that the control of the ring die compression ratio of the granulator has good effect on the specific extraction of marigold flavone;
2. the method realizes the full extraction of the flavone in the chrysanthemum by controlling the volume fractions of the extraction solvent and the organic solvent in the extracting solution; the marigold flavone can be well separated from impurities;
3. the content of the flavone in the marigold flavone product obtained by the method is more than or equal to 98 percent, the production is continuous, the yield is high, the operation is simple, the requirement of industrial mass production is met, the industrialization of the high-content marigold flavone product is realized, and the industrial benefit is improved.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The specifications of raw materials and reagents of products used in the embodiments are the same, and a granulator, extraction equipment, filtering equipment and the like used in the embodiments are the same.
Example 1
1) Granulating the marigold flower meal by using a granulator, adjusting the compression ratio of a ring mould of the granulator to 1:1.8, and introducing steam for granulation;
2) adding 0.4m flos Tagetis Erectae granule 100kg3Extracting 98% acetone for 4 times, each time for 1 hr, and keeping the temperature of the extractive solution at about 52 deg.C;
3) concentrating the extracting solution until the volume fraction of acetone is about 10%;
4) filtering to obtain filtrate and filter cake;
5) the filter cake was transported to a dryer for drying to obtain the product of example 1.
Example 2
Compared with the example 1, the difference is that the step 1) ring die compression ratio is 1:1.2, and other operations are the same as the example 1, so that the product of the example 2 is obtained.
Example 3
Compared with the example 1, the difference is that the step 1) ring die compression ratio is 1:2.2, and other operations are the same as the example 1, so that the product of the example 3 is obtained.
Example 4
Compared with the example 1, the difference is that the marigold particles are extracted by 92% acetone in the step 2), and other operations are the same as the example 1, so that the product of the example 4 is obtained.
Example 5
Compared with the example 1, the difference is that the marigold particles are extracted by 70% acetone in the step 2), and other operations are the same as the example 1, so that the product of the example 5 is obtained.
Example 6
Compared with the example 1, the difference is that the marigold particles are extracted by 100% acetone in the step 2), and the other operations are the same as the example 1, so as to obtain the product of the example 6.
Example 7
The difference compared with example 1 is that step 3) is concentrated to 30% acetone volume fraction, and the other operations are the same as example 1, thus obtaining the product of example 7.
Example 8
Compared with the example 1, the difference is that the step 3) is concentrated to 0% of acetone volume fraction (namely concentrated to the solution without acetone), and the other operations are the same as the example 1, so as to obtain the product of the example 8.
Example 9
The difference from example 1 is that the step 3) adds an aqueous solution to adjust the volume fraction of acetone to 10%, and the other operations are the same as example 1 to obtain the product of example 9.
Comparative example 1
Compared with the example 1, the difference is that the step 1) ring die compression ratio is 1:3.0, and other operations are the same as the example 1, so that the product of the comparative example 1 is obtained.
Comparative example 2
Compared with the example 1, the difference is that the marigold particles are extracted by acetone with the concentration of 65% in the step 2), and other operations are the same as the example 1, so that the product of the comparative example 2 is obtained.
Comparative example 3
Compared with the example 1, the difference is that the step 3) is concentrated to the acetone volume fraction of 40%, and other operations are the same as the example 1, so that the product of the comparative example 3 is obtained.
Comparative example 4
Compared with the example 1, the difference is that the comparative example 4 is obtained by directly concentrating and drying without adjusting the solvent after the extraction in the step 3).
The contents and yields of the products obtained in the above examples and comparative examples are shown in the following table:
TABLE 1 Tagetes erecta content and yield table
Product(s) Content of longevity flavone Yield of
Example 1 99.67％ 98.45％
Example 2 98.54％ 97.37％
Example 3 98.13％ 96.12％
Example 4 99.17％ 96.53％
Example 5 92.34％ 96.32％
Example 6 99.70％ 95.42％
Example 7 98.90％ 95.60％
Example 8 95.34％ 98.10％
Example 9 99.30％ 98.20％
Comparative example 1 81.12％ 85.10％
Comparative example 2 78.92％ 81.30％
Comparative example 3 89.51％ 97.70％
Comparative example 4 60.54％ 98.30％
The method for measuring the content of the marigold flavone comprises the following steps:
dissolving marigold flavone samples obtained in the examples and the comparative examples by using ethanol to a constant volume, adding 1ml of 5% sodium nitrite solution, shaking up, standing for 6min, adding 1ml of 10% aluminum nitrate solution, shaking up, standing for 6min, adding 10ml of sodium hydroxide test solution, adding water to the scales, shaking up, standing for 15min, and measuring the absorbance at the wavelength of 500nm by using a corresponding reagent as a blank according to an ultraviolet-visible spectrophotometry. And (3) taking the quercetagetin as a standard reference substance, and performing content calculation.
The technical method for the yield comprises the following steps:
marigold flavone yield (%) - (total weight of product × content of product detected) × 100%/(total weight of raw material × content of raw material detected)
The content and yield results show that: the granulation parameters and the acetone content in the solvent before and after extraction have obvious influence on the extraction effect of marigold flavone products. According to the method, the optimal extraction product is obtained through the specifically selected granulation parameters and the content of acetone in the solvent before and after extraction, and an unexpected technical effect is achieved.
The foregoing is a further description of the invention with reference to preferred embodiments, and the examples described are some, but not all, examples of the invention. It will be apparent to those skilled in the art that various modifications, additions, substitutions, and other embodiments can be made without departing from the spirit and scope of the invention.

Claims (9)

1. An industrial method for continuously extracting high-content marigold flavone is characterized by comprising the following steps:
1) granulating the marigold flower raw material by using a granulator, wherein the compression ratio of a ring mould of the granulator is 1 (1.2-2.2);
2) extracting the marigold flower particles by using 70-100% of acetone as an extracting agent, and filtering to obtain an extracting solution;
3) and (3) adjusting the volume fraction of acetone in the extracting solution to 0-30%, filtering to obtain a filter cake, and drying the filter cake to obtain the marigold flavone product.
2. The industrial method for continuously extracting high-content marigold flavone as claimed in claim 1, wherein the marigold raw material in 1) is fresh or dried marigold flower, or various commercially available processed forms of marigold flower; flower meal is preferred.
3. The industrial method for continuously extracting high-content marigold flavone according to claim 1 or 2, wherein the hardness of the granulated particles in the step 1) is 3-8 kg/cm2。
4. The industrial method for continuously extracting high-content marigold flavone according to any one of claims 1 to 3, wherein the extraction temperature in the step 2) is 40-60 ℃.
5. The industrial method for continuously extracting high-content marigold flavone as claimed in any one of claims 1 to 4, wherein the ratio of the extraction particles to the extraction solvent in the step 2) is not more than 1:2 (g/mL).
6. The industrial method for continuously extracting high-content marigold flavone according to any one of claims 1 to 5, wherein the extraction in the step 2) is countercurrent extraction.
7. The industrial method for continuously extracting high-content marigold flavone according to any one of claims 1 to 6, wherein the extraction times in the step 2) are not less than 4; the extraction time is 0.5-2.5 hr.
8. The industrial process for continuously extracting high content of marigold flavonoids according to any one of claims 1 to 7, wherein the volume fraction of the solvent is reduced in step 2) by concentrating or adding a strongly polar solvent.
9. A marigold flavone product prepared according to the method of any one of claims 1 to 8.
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