阅读说明：本技术 一种提取叶黄素和槲皮万寿菊素的工业化方法 (Industrial method for extracting lutein and quercetagetin ) 是由 高伟 吴迪 王欢欢 连运河 张玉芬 于 2019-10-22 设计创作，主要内容包括：本发明涉及一种提取叶黄素和槲皮万寿菊素的工业化方法,包括如下步骤：用体积分数为90～99％的丙酮溶液对万寿菊花颗粒进行提取,得提取液；将所述提取液浓缩至固形物含量为60～95％,用体积分数为70～100％的低级醇溶液对浓缩物进行萃取,得槲皮万寿菊素产品和叶黄素产品。采用丙酮溶液对万寿菊花进行提取,可对叶黄素和槲皮万寿菊素进行充分地提取,并通过低级醇溶液萃取进行分离,得到两种产品,整个过程中严格控制丙酮浓度和浓缩程度,可对叶黄素和槲皮万寿菊素进行充分的提取以及较好的精制,所得提取物有较好的生物功效。(The invention relates to an industrialized method for extracting lutein and quercetagetin, which comprises the following steps: extracting marigold flower particles by using an acetone solution with the volume fraction of 90-99% to obtain an extracting solution; concentrating the extracting solution until the solid content is 60-95%, and extracting the concentrate by using a low alcohol solution with the volume fraction of 70-100% to obtain a quercetagetin product and a lutein product. The method adopts acetone solution to extract marigold flowers, can fully extract lutein and quercetagetin, and separate the lutein and the quercetagetin through low-grade alcohol solution extraction to obtain two products, the acetone concentration and the concentration degree are strictly controlled in the whole process, the lutein and the quercetagetin can be fully extracted and well refined, and the obtained extract has good biological efficacy.)

1. An industrial method for extracting lutein and quercetagetin is characterized by comprising the following steps:

1) extracting marigold flower particles by using an acetone solution with the volume fraction of 90-99% to obtain an extracting solution;

2) concentrating the extracting solution until the solid content is 60-95%, and extracting the concentrate by using a solution of lower alcohol with the volume fraction of 70-100% to obtain a quercetagetin product and a lutein product.

2. The industrial method according to claim 1, wherein the lower alcohol is one or more of alcohols having 1 to 4 carbon atoms.

3. The industrial process according to claim 2, wherein the lower alcohol is one or more of methanol, ethanol or propanol.

4. The industrial method according to any one of claims 1 to 3, wherein the mass-to-volume ratio of the marigold flower particles to the acetone solution is 1: 4-20, preferably 1: 5 to 10.

5. The industrial process according to any one of claims 1 to 4, wherein the extraction is carried out at a temperature of 30 to 60 ℃ and/or for a time of 2 to 6 hours.

6. The industrial process according to any one of claims 1 to 5, wherein the concentration temperature is 50 to 90 ℃.

7. The industrial process according to any one of claims 1 to 6, wherein the concentration is carried out until the solid content is 80 to 90%.

8. The industrial process according to any one of claims 1 to 7, wherein the volume fraction of acetone in the acetone solution is 94 to 99%.

9. The industrial process according to any one of claims 1 to 8, wherein the volume fraction of the alcohol in the solution of the lower alcohol is 80 to 90%; and/or the mass-to-volume ratio of the concentrate to the solution of the lower alcohol is 1: 1 to 10.

10. The lutein product and quercetagetin product obtained by the industrial method according to any one of claims 1 to 9.

Technical Field

The invention relates to the technical field of plant functional component extraction, in particular to a method for extracting lutein and quercetagetin from marigold flowers.

Background

Marigold is one of the main herbaceous potted flowers cultivated in China, and is widely used for indoor and outdoor environment arrangement. With the development of the nutritional health industry, marigold is increasingly demanded internationally. Marigold not only has ornamental value, but also has good medicinal value, and the main components having pharmacological action are flavonoid, carotenoid, terpenoid, glycoside, essential oil, etc.

At present, the extraction method of lutein and flavone mainly comprises the step-by-step extraction, namely, lutein is firstly extracted by normal hexane, and then marigold flower pulp is treated by a solvent to obtain a flavonoid product. In addition, two patents utilize mixed solvent extraction, wherein 201410104645.X adopts aqueous two-phase solvent for extraction; mainly extracts the mixture of lutein and flavone, but does not extract high-purity quercetagetin. Chinese patent 201811188771.2 adopts mixed solvent of petroleum ether and acetone for extraction, and the separation mode selected in the patent is that water is added for separation, the operation is complicated, and high-purity quercetagetin cannot be separated, and only marigold flavone mixture can be obtained.

Disclosure of Invention

The invention relates to an industrial method for simply extracting lutein and quercetagetin, which comprises the following steps:

1) extracting marigold flower particles by using an acetone solution with the volume fraction of 90-99% to obtain an extracting solution;

2) concentrating the extracting solution until the solid content is 60-95%, and extracting the concentrate by using a solution of lower alcohol with the volume fraction of 70-100% to obtain a quercetagetin product and a lutein product.

Research finds that the concentration of acetone is strictly controlled within the range, the quercetin marigold and the lutein can be directly extracted, but in the process of separating the two substances by using a low-alcohol solution, if the extracting solution is directly volatilized and then extracted, the two substances are not easily separated, the purity of the quercetin marigold and the lutein is greatly reduced, and the analysis reason may be that the two substances are extracted by using the acetone solution alone, the two substances exist as uniform solids after being volatilized to be dried, and the two substances are relatively strongly wrapped with each other and are not easily and directly separated. The lower alcohol solution has certain solubility to lutein and quercetagetin, but the solubility of quercetagetin is far greater than that of lutein, which is also the reason why the alcohol solution can extract and separate the two. If the concentration degree is too light, the concentrated extract contains more acetone, and the acetone is easily dissolved in the alcohol solution, so that the mixed solution of the acetone and the alcohol solution can also dissolve a certain degree of lutein in the extraction process, so that the purity of the quercetagetin is reduced, and the lutein yield is reduced. The extractant is concentrated to the degree, and the two still have a certain dispersion degree, so that the alcohol solution can be separated, and the extraction effect cannot be influenced due to mutual solubility of the acetone and the alcohol solution. Further, concentrating the alcohol phase to obtain quercetagetin, and separating the lower layer to obtain xanthophyll extract.

Preferably, the lower alcohol is one or more of alcohols with 1-4 carbon atoms.

Further preferably, the lower alcohol is one or more of methanol, ethanol or propanol.

Preferably, the mass-to-volume ratio of the marigold flower particles to the acetone solution is 1: 4 to 20. Within the above range, lutein and quercetagetin can be extracted sufficiently, and the extraction rate is high.

Further preferably, the mass-to-volume ratio of the marigold flower particles to the acetone solution is 1: 5 to 10. Within the above range, the lutein and quercetagetin can be sufficiently extracted without causing an increase in cost.

Preferably, the extraction is carried out at the temperature of 30-60 ℃, and/or the extraction time is 2-6 h. At the temperature, the two products can be fully and completely extracted, the temperature is too low, the extraction is not sufficient, the yield of the quercetagetin cannot be increased even if the temperature is too high, the yield of the lutein can be reduced on the contrary, and the volatilization of acetone is easy to cause.

Preferably, the concentration is carried out at a temperature of 50-90 ℃. Under the condition, the lutein is not damaged by high-temperature concentration.

Preferably, the volume fraction of acetone in the acetone solution is 94-99%. Under the concentration, the lutein and the quercetagetin can be fully extracted by acetone at the same time.

Preferably, the concentration is carried out until the solid content is 80-90%. Concentrating the solid content to the above range can better realize the separation of lutein and quercetagetin.

Preferably, the volume fraction of the alcohol in the lower alcohol solution is 80-90%. The lower alcohol solution has certain solubility to both lutein and quercetagetin, but the volume fraction of the lower alcohol solution can be adjusted to control better solubility to queretagetin and poorer solubility to lutein, and under the volume fraction, the solubility of lutein in the alcohol solution can be further reduced and the higher solubility of queretagetin can be ensured.

Preferably, in the extraction process, the volume fraction of acetone in the acetone solution is 94-99%, the extracting solution is concentrated to a solid content of 80-90%, and a methanol solution with the volume fraction of 80-90% is used for extraction.

Another purpose of the invention is to protect the lutein product and the quercetagetin product extracted by the method.

The acetone solution is an acetone aqueous solution, the lower alcohol solution is a lower alcohol aqueous solution, the mass and the volume in the mass-volume ratio are standard units, and in the ratio process, g corresponds to ml, and kg corresponds to L.

The invention has the following beneficial effects:

1) the invention provides a method for extracting lutein and quercetagetin by a single solvent method, which only comprises the operations of extraction, concentration and extraction.

2) Aiming at the marigold flower, the invention selects acetone as an extracting agent, can simultaneously extract lutein and quercetagetin, and can reach the highest yield of the two products by strictly controlling the concentration of the acetone. By controlling the concentration degree and the concentration and proportion of the lower alcohol solution, the contents of the two products can be ensured.

3) By adopting the method, the lutein and the quercetagetin can be fully extracted, the yield of the lutein is 98 percent, and the content is more than 19 percent; the yield of the quercetagetin is 90 percent, and the purity is more than 90 percent.

Drawings

FIG. 1 is a liquid chromatogram of quercetagetin extracted by the method described in example 1.

Detailed Description

The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.