Tagetes erecta extract and preparation method thereof

Abstract

The invention relates to the technical field of substance extraction, and particularly discloses a marigold extract and a preparation method thereof. The method for preparing the marigold extract comprises the following steps: (1) taking marigold particles as a raw material, extracting with C6 alkane, and concentrating to obtain a concentrate I with the solid content of 25-40%; (2) fully mixing low-carbon alcohol at 55-65 DEG C, an alkaline solution with the concentration of 18-22% and the concentrate I at 50-60 DEG C, and separating the upper layer to obtain a solvent layer subjected to primary impurity removal; the volume ratio of the concentrate I to the low-carbon alcohol with the temperature of 55-65 DEG C to the aqueous alkali is 1: 1: (0.1-0.2); (3) fully mixing the solvent layer subjected to primary impurity removal with a salt solution at 20-30 DEG C, and separating the upper layer to obtain a solvent layer subjected to secondary impurity removal; (4) concentrating the solvent layer subjected to secondary impurity removal to obtain a concentrate II; and (5) fully mixing the concentrate II with low-carbon alcohol at 80-85 DEG C at 50-65 DEG C, and separating the lower layer to obtain an extract layer. The extract disclosed by the invention is free from special smell and high in yield.

Description

Technical Field

[0001] The invention relates to the technical field of material extraction, in particular to a marigold extract and a preparation method thereof. Background Art

[0002] Lutein, also known as "plant lutein", is an oxygen-containing carotenoid that is widely found in natural plants such as marigold, banana, kiwi and corn. It has good antioxidant activity, is non-toxic and harmless, and is an important natural nutrient, food colorant and feed additive raw material.

[0003] Natural lutein is mainly extracted from marigold flowers. After fermentation, marigold flowers are physically squeezed to remove some water, dried, crushed, and finally made into marigold granules. Marigold granules generally use vegetable oil extraction solvents or alkanes such as subcritical butane as extraction solvents. After extraction, filtration, evaporation and removal of solvents, marigold extract is obtained. At room temperature, marigold extract is in a solidified state and has an unpleasant odor, which greatly limits the application of marigold extract in high-end fields such as food and medicine. Due to the inconvenience of application, marigold extract needs to undergo complex refining treatment. The commonly used treatment methods in the industry include saponification, crystallization and purification to make free lutein crystals, and then preparation and embedding technology to prepare related products for application; in addition, lutein ester crystals are prepared by washing, filtering and drying with a mixed solvent of low-carbon alcohol and alkane, and then preparation and embedding technology is used to make terminal application products for application. Both of the above technical solutions require in-depth processing of marigold extract, and both require preparation technology processing in the later stage. The yield of lutein in the entire processing process is difficult to reach 90%, and most of them are within the range of 70-80%. After a lengthy processing process, the production cost increases a lot, and the effective lutein component is wasted a lot. In addition, there are also some technical attempts to directly deodorize marigold extract. Usually, the preparation of food-grade marigold extract currently adopts refining methods such as supercritical CO2 and molecular distillation. For example, Chinese patent CN201910138486.8 first adds a blending agent to marigold extract, and then performs molecular distillation. The peculiar smell in marigold extract can be removed, and it will not affect the coloring or health care effect of marigold extract. The marigold extract after removing the peculiar smell can be directly used as a food pigment or food additive. However, molecular distillation needs to be carried out under high temperature conditions. Although the time is short, the color of the extract after high temperature treatment becomes darker and the brightness decreases, and the coloring effect becomes worse. In addition, there is the problem of gradual carbonization of the material, which makes the system cleaning cumbersome and there is a risk of entrained carbides in the product. Chinese patent CN202010882928.2 uses a water-soluble emulsifier to emulsify the odorous substances in the marigold extract and dilute it with water, and then uses a non-polar solvent to extract the marigold extract, concentrate the non-polar solvent layer, and remove the solvent residue to obtain a marigold extract with a good smell. However, this method cannot be produced continuously, and the production efficiency is low. In addition, studies have found that when the non-polar solvent back-extracts the aqueous phase, there are still more flavor components that will be extracted into the extract again. The smell of the resulting extract is indeed reduced, but there is still a unique smell of marigold.

[0004] Therefore, according to market demand, it is urgent to invent a method for preparing a food-grade marigold extract that can remove the special smell of marigold, has good fluidity, is not solidified, is not stratified, has a high yield, is simple in process, is easy to operate, and can be produced on a large scale and continuously in an industrialized manner. Summary of the invention

[0005] One of the purposes of the present invention is to provide a method for preparing marigold extract which can effectively remove the odor of marigold extract and has a high yield.

[0006] The present invention provides a method for preparing marigold extract, which comprises: (1) Using marigold granules obtained after fermentation, drying and granulation of marigold as raw materials, extracting with C6 alkane, concentrating the obtained extract to obtain a concentrate I with a solid content of 25-40%; (2) at 50-60°C, fully mixing a 55-65° low-carbon alcohol, an alkali solution having a concentration of 18-22%, and the concentrate I, separating the upper layer to obtain a solvent layer for primary impurity removal; The volume ratio of the concentrate I, 55-65° low carbon alcohol and alkaline solution is 1:1:(0.1-0.2); (3) fully mixing the solvent layer obtained by the primary impurity removal with the salt solution at 20-30° C., separating the upper layer, and obtaining the solvent layer obtained by the secondary impurity removal; (4) concentrating the solvent layer obtained by the secondary impurity removal to obtain a concentrate II; (5) Fully mix the concentrate II with low-carbon alcohol at 80-85°C at 50-65°C, separate the lower layer, and obtain an extract layer.

[0007] Traditional marigold extract is made from marigold as raw material through fermentation, drying, granulation, extraction and other processes. The product has a unique smell of fermented marigold (a sour and astringent taste produced during fermentation) and is in a solidified, non-fluid extract state at room temperature. Its smell affects the application of marigold extract in the fields of food, medicine, etc. In order to solve this problem, the present invention has repeatedly explored the preparation method of marigold extract and finally obtained a solution with an ideal deodorizing effect.

[0008] Specifically, the present invention extracts the marigold particles obtained by fermentation and granulation with an extraction solvent, concentrates the extract to a specific solid content (retains a certain amount of extractant), and then performs a saponification reaction on the concentrate at a specific temperature and a specific alcohol concentration to achieve both effective separation and removal of impurities and the yield of total carotenoids. The saponification system of the present invention can effectively remove part of the special smell of marigold and part of the impurity components that easily cause the extract to thicken and harden, and avoid the loss of the content of beneficial components such as lutein esters. In this saponification system, the concentration of alcohol has a greater impact on the treatment effect. If the concentration of alcohol is too high, the yield of total carotenoid content is reduced. If the concentration of alcohol is too low, the impurity separation and removal effect and the treatment efficiency are reduced.

[0009] In addition, the present invention has also been found that washing with salt water under the conditions of the present invention can remove impurities that have not been separated in the previous steps and a small amount of special odors, thereby reducing impurity components that affect the fluidity of the product. In particular, after the first impurity removal is achieved by saponification, the temperature is first lowered and washed with salt water at 20-30°C, which can better remove the odor. And after that, the impurities are removed again at 50-65°C with an alcohol solution of a specific concentration, which can remove the remaining odor components, and finally obtain an ideal deodorization effect, and obtain a product without the special smell of marigold. If the concentration of alcohol is too high during the second impurity removal, it will affect the yield of the total carotenoid content. If the concentration of alcohol is too low or the temperature is not within the limits of the present invention, the ideal treatment effect cannot be achieved.

[0010] The marigold granules of the present invention are commercially available conventional fermentation granulation products. Those skilled in the art can also prepare marigolds by fermentation with lactic acid bacteria according to conventional methods in the art. For example, the preparation method can be: pick marigold flowers in the mature stage, put them into a fermentation tank, spray lactic acid bacteria liquid evenly layer by layer, compact and seal them, and ferment them rapidly. The lactic acid bacteria liquid can use commercially available mature marigold green storage agent, such as Taiwan Asia core marigold green storage agent, add 40-80kg water per 100g green storage agent, control the water temperature to 20-30℃, evenly spray it on 15-20 tons of fresh chrysanthemums, seal the pool, ferment for 2-3 weeks, centrifuge or squeeze dehydrate the chrysanthemums, and hot air dry the dehydrated chrysanthemums (60-80℃), control the moisture content to be less than 12%, and then crush the dried chrysanthemums, and ensure that the crushing particle size ensures that the pass rate of 40 meshes reaches more than 90%. After crushing, the chrysanthemum powder enters the extrusion granulator to prepare marigold granules with a hardness of 3-5.0.

[0011] In steps (2), (3) and (5) of the method of the present invention, the method for fully mixing can be conventional methods such as fully stirring or circulating with a circulating pump for 0.5-1 hour, and the method for separation can be conventional methods such as static or centrifugal.

[0012] In the method of the present invention, the C6 alkane is one or more of a vegetable oil extraction solvent, n-hexane, 2-methylpentane, 3-methylpentane, methylcyclopentane, and cyclohexane, preferably a vegetable oil extraction solvent (the vegetable oil extraction solvent is a commercially available product, which is mainly n-hexane and also contains 2-methylpentane, 3-methylpentane, methylcyclopentane, cyclohexane, etc.); the low-carbon alcohol is one or more of methanol, ethanol, and isopropanol, preferably ethanol; In the method of the present invention, the alkaline solution is an aqueous solution of sodium hydroxide and / or potassium hydroxide; and the salt solution is an aqueous solution of sodium chloride and / or potassium chloride.

[0013] In step (3) of the method of the present invention, the volume ratio of the solvent layer for primary impurity removal to the salt solution is 1:(0.34-0.36); the concentration of the salt solution is 4-6%.

[0014] In step (5) of the method of the present invention, the mass volume ratio of the concentrate II to the 80-85° low-carbon alcohol is 1: (2-4) g / mL.

[0015] In steps (1) and (4) of the method of the present invention, the concentration is carried out by heating vacuum concentration, the concentration temperature is 55-65°C, and the pressure is -0.05 ~ -0.08MPa; and / or, in step (4), the residual solvent of the concentrate II is 500-2000ppm.

[0016] The present invention can preferably use a rapid continuous evaporation method such as a lifting film or a thin film suitable for the industry for concentration, so as to reduce the loss of lutein components.

[0017] In step (1) of the method of the present invention, during extraction, the mass volume ratio of the raw material to the C6 alkane is 1: (4-5) g / mL.

[0018] In the method of the present invention, step (2) is repeated once, step (3) is repeated 1-3 times, and step (5) is repeated 2-4 times.

[0019] In the method of the present invention, after step (5), the method further includes a step of concentrating and removing the solvent in the extract layer, or after step (5), the method further includes a step of mixing the extract layer with vegetable oil and then concentrating and cooling the extract layer.

[0020] After the extract layer prepared in step (5) of the present invention is desolventized, the obtained product has no bad taste and has a high yield of total carotenoid content (content yield ≥ 95%).

[0021] The technicians in this field can also add an appropriate amount of vegetable oil to dilute the raw material according to the lutein content and the content required for the finished product, and then heat to remove the solvent residue to obtain the finished product. The equipment for concentrating and removing the solvent residue can be a vacuum deodorization reactor type equipment.

[0022] In the method of the present invention, the vegetable oil is preferably soybean oil and / or sunflower oil, and other vegetable oils may also be selected according to product requirements; the mass ratio of the extract layer to the vegetable oil is 1:(0.5-1), wherein if the amount of oil added is too large, the unit content of the obtained extract is low, and the cost of commercial application is increased, and if the amount of oil added is too low, the product fluidity is poor and the convenience of application is reduced.

[0023] The preferred cooling method is: in the first stage, stirring and cooling from 50-55°C to 40±2°C, the cooling rate is 4-6°C / h, and the stirring speed is 18-22 rpm; in the second stage, stirring and cooling to 30±2°C is continued, and the stirring speed is controlled to be completed within 10 minutes, the stirring speed is not less than 60 rpm, and the preferred stirring speed is 60 rpm, and then the mixture is kept warm and stirred for 5.5-6.5h, and the stirring speed during the insulation period is 38-42 rpm; in the third stage, stirring and cooling to 20±2°C is continued, the cooling rate is 4-6°C / h, and the stirring speed is 28-32 rpm.

[0024] The present invention has found through research that if the extract after adding vegetable oil and desolventizing is cooled in the preferred manner of the present invention, the balance between lutein esters, other monoesters and diesters and vegetable oils in the marigold extract can be controlled, the requirements of fluidity and long-term stability can be met, and stable and uniform lutein fine particles can be obtained. The final product is fluid and stable, without stratification, precipitation, and odor, and can be conveniently applied to food coloring to provide food with a colorful golden color.

[0025] In the method of the present invention, the conditions for concentrating the extract layer after mixing with the vegetable oil are a temperature of 50-55° C. and a vacuum degree of -0.08 to -0.1 MPa; and / or the residual solvent after the extract layer after mixing with the vegetable oil and concentrating is less than 50 ppm.

[0026] The invention also provides a marigold extract, which is prepared by the method.

[0027] The marigold extract obtained by the invention has no special smell and good fluidity.

[0028] The marigold extract added with vegetable oil and cooled in a special preferred manner after desolventizing is placed at room temperature for 6 months without any special smell, and is in a non-solidified state, flowable, stable, and without stratification and precipitation.

[0029] The beneficial effects of the present invention are at least: The marigold extract prepared by the invention has ideal odor removal effect, high production and processing yield, simple process, convenient operation, and can be continuously industrialized for large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 This is the electronic nose analysis spectrum of the common marigold extract prepared from Yanshan granules.

[0031] Figure 2 This is the electronic nose analysis spectrum of the marigold extract prepared in Example 1.

[0032] Figure 3 This is the electronic nose analysis spectrum of the marigold extract prepared in Example 2.

[0033] Figure 4 This is the electronic nose analysis spectrum of the marigold extract prepared in Example 3.

[0034] Figure 5 This is the electronic nose analysis spectrum of the marigold extract prepared in Example 4.

[0035] Figure 6 This is the electronic nose analysis spectrum of the marigold extract prepared in Comparative Example 1.

[0036] Figure 7 This is the electronic nose analysis spectrum of the marigold extract prepared in Comparative Example 2.

[0037] Figure 8 This is the electronic nose analysis spectrum of the marigold extract prepared in Comparative Example 3.

[0038] Fig. 9 This is the electronic nose analysis spectrum of the marigold extract prepared in Comparative Example 4.

[0039] Fig.10 Electronic nose analysis spectrum of common marigold extract prepared for Shache granules.

[0040] Fig.11 This is the electronic nose analysis spectrum of the marigold extract prepared in Example 5.

[0041] Fig.12 This is the electronic nose analysis spectrum of the marigold extract prepared in Example 6.

[0042] Fig.13 This is the electronic nose analysis spectrum of the marigold extract prepared in Example 7.

[0043] Fig.14 This is the electronic nose analysis spectrum of the marigold extract prepared in Example 8.

[0044] Fig.15 This is the electronic nose analysis spectrum of the marigold extract prepared in Comparative Example 5.

[0045] Fig.16 This is the electronic nose analysis spectrum of the marigold extract prepared in Comparative Example 6.

[0046] Fig.17 This is the electronic nose analysis spectrum of the marigold extract prepared in Comparative Example 7.

[0047] Fig.18 This is the electronic nose analysis spectrum of the marigold extract prepared in Comparative Example 8.

[0048] The unit of the horizontal axis in each figure is second, the vertical axis has no actual unit, and the numerical value represents the peak height. DETAILED DESCRIPTION

[0049] The preferred embodiments of the present invention will be described in detail below in conjunction with examples. It should be understood that the following examples are provided only for the purpose of illustration and are not intended to limit the scope of the present invention. Those skilled in the art may make various modifications and substitutions to the present invention without departing from the purpose and spirit of the present invention.

[0050] The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, etc. used in the following examples are commercially available or prepared according to conventional methods in the art unless otherwise specified.

[0051] In the present invention, the vegetable oil extraction solvent is purchased from Liaoning Yufeng Chemical Co., Ltd.

[0052] The detection of total carotenoid content in the extract refers to the China Food Additives and Ingredients Association group standard T / CFAA0005-2021 Lutein raw material marigold oleoresin.

[0053] The content yield is calculated as follows: final product unit content × product weight / (input raw material weight × raw material unit content) × 100%. In the present invention, unit content refers to the total carotenoid content.

[0054] Example 1 This embodiment relates to a food-grade marigold extract, and the preparation steps are as follows: 1) Weigh 1.0 kg of marigold granules with a unit content of 25.0 g / kg (purchased from Yanshan County Huafeng Agricultural Development Co., Ltd.), add 4500 ml of vegetable oil extraction solvent to fully extract, and concentrate the extract by thin film evaporation at 65°C and -0.05 MPa to obtain 935.8 ml of concentrate I with a solid content of 25%; 2) At 55°C, add 935.8 ml of 60° ethanol and 93.58 ml of 20% sodium hydroxide aqueous solution, stir and mix thoroughly for 30 minutes. During the reaction, open the vent tube to condense water to prevent the loss of solvent due to heat and volatilization. Separate and collect the upper alkane layer at a static temperature under insulation; repeat the above operation once for the alkane layer to obtain 926.5 ml of the first impurity-free alkane layer; 3) After the primary deionized alkane layer was cooled to 25°C, 324.3 ml of 5% sodium chloride aqueous solution (the ratio of brine to alkane layer was approximately 0.35:1) was added, and the mixture was stirred for 15 min, and the upper alkane layer was obtained by static separation; the alkane layer was collected and the above operation was repeated once, and finally 922.6 ml of the secondary deionized alkane layer was obtained; 4) The secondary alkane layer after impurity removal was concentrated at 60°C and -0.07MPa to obtain 169.2g of concentrate II with a residual solvent of 1385ppm; 5) At 60°C, add 423.0 ml of 80° ethanol to the concentrate II at a weight-to-volume ratio of 1:2.5, mix and stir thoroughly for 30 min, separate statically, and collect the lower extract layer; repeat the above operation twice to obtain 173.3 g of ethanol extract layer; 6) Add 130.0g soybean oil to the ethanol extract layer, concentrate and desolventize at 55°C and -0.08MPa for 2.0h until the residual solvent is less than 50ppm, turn on the coolant for stirring and cooling, control the cooling rate to 5°C / h, and uniformly cool to 40°C, during which the stirring rate is 20 rpm; continue stirring and cooling, control the uniform cooling to 30°C within 10 minutes, during which the stirring speed is 60 rpm; after the temperature drops to 30°C, keep warm and stir for 6.0h, during which the stirring rate is 40 rpm; continue stirring and uniformly cool to 20°C, the cooling rate is 5°C / h, and the stirring rate is 30 rpm; finally, 296.1g of food-grade marigold extract with a unit content of 83.0g / kg is obtained, and the content yield is 98.31%; The food-grade marigold extract is placed at room temperature for 6 months in a non-solidified state with good fluidity, no stratification and no special smell of marigold extract.

[0055] Example 2 This embodiment relates to a food-grade marigold extract, and the preparation steps are as follows: 1) Weigh 1.0 kg of marigold granules with a unit content of 25.0 g / kg (purchased from Yanshan County Huafeng Agricultural Development Co., Ltd.), add 5000 ml of vegetable oil extraction solvent to fully extract, and the extract is concentrated by thin film evaporation at 55°C and -0.08 MPa to obtain 935.8 ml of concentrate I with a solid content of 25%; 2) At 50°C, add 935.8 ml of 60° methanol and 93.58 ml of 20% sodium hydroxide aqueous solution, stir and mix thoroughly for 30 minutes. During the reaction, open the vent tube to condense water to prevent the loss of solvent due to heat and volatilization. Separate and collect the upper alkane layer at a static temperature. Repeat the above operation once for the alkane layer to obtain 928.3 ml of the first decontaminated alkane layer. 3) After the primary deionized alkane layer is cooled to 20°C, 324.9 ml of 5% sodium chloride aqueous solution (the ratio of brine to alkane layer is about 0.35:1) is added, and the mixture is stirred for 15 minutes, and the upper alkane layer is obtained by static separation; the alkane layer is collected and the above operation is repeated once, and finally 924.2 ml of the secondary deionized alkane layer is obtained; 4) The secondary alkane-removed layer was concentrated at 60°C and -0.07 MPa to obtain 170.4 g of concentrate II with a residual solvent of 1510 ppm; 5) At 65°C, add 681.6 ml of 80° methanol to the concentrate II, with a weight-to-volume ratio of 1:4, mix and stir thoroughly for 30 min, separate statically, and collect the lower extract layer; repeat the above operation twice to obtain 178.2 g of the methanol-containing extract layer; 6) 130.0 g soybean oil was added to the methanol extract layer, and the residual solvent was less than 50 ppm after concentration and desolventization at 55° C. and −0.08 MPa for 2.0 h. The cooling liquid was turned on and the temperature was lowered according to the method described in Example 1. Finally, 299.0 g of odorless marigold extract with a unit content of 82.6 g / kg was obtained, and the content yield was 98.79%; The food-grade marigold extract is placed at room temperature for 6 months in a non-solidified state with good fluidity, no stratification and no special smell of marigold extract.

[0056] Example 3 This embodiment relates to a food-grade marigold extract, and the preparation steps are as follows: 1) Weigh 1.0 kg of marigold granules with a unit content of 25.0 g / kg (purchased from Yanshan County Huafeng Agricultural Development Co., Ltd.), add 4500 ml of vegetable oil extraction solvent to fully extract, and concentrate the extract (under the same conditions as in Example 1) to obtain 935.8 ml of concentrate I with a solid content of 25%; 2) At 55°C, add 935.8 ml of 60° isopropanol and 93.58 ml of 20% sodium hydroxide aqueous solution, stir and mix thoroughly for 30 minutes. During the reaction, open the vent tube to condense water to prevent the loss of solvent due to heat and volatilization. Separate and collect the upper alkane layer at a static state under heat preservation; repeat the above operation once for the alkane layer to obtain 920.8 ml of the first decontaminated alkane layer; 3) After the primary deionized alkane layer was cooled to 25°C, 322.3 ml of 5% sodium chloride aqueous solution (the ratio of brine to alkane layer was approximately 0.35:1) was added, and the mixture was stirred for 15 min, and then the upper alkane layer was obtained by static separation. The alkane layer was collected and the above operation was repeated once, and finally 918.5 ml of the secondary deionized alkane layer was obtained. 4) The secondary alkane-removed layer was concentrated at 60°C and -0.07 MPa to obtain 167.7 g of concentrate II with a residual solvent of 1558 ppm; 5) At 55°C, add 335.4 ml of 80° isopropanol to the concentrate II, with a weight-to-volume ratio of about 1:4, mix and stir thoroughly for 30 minutes, separate statically, and collect the lower extract layer; repeat the above operation twice to obtain 171.6 g of the isopropanol extract layer; 6) 130.0 g of soybean oil was added to the isopropanol extract layer, and the residual solvent was less than 50 ppm after concentration and desolventization at 55° C. and −0.08 MPa for 2.0 h. The cooling liquid was turned on and the temperature was lowered according to the method described in Example 1. Finally, 286.9 g of food-grade marigold extract with a unit content of 84.7 g / kg was obtained, and the content yield was 97.2%; The food-grade marigold extract is placed at room temperature for 6 months in a non-solidified state with good fluidity, no stratification and no special smell of marigold extract.

[0057] Example 4 This embodiment relates to a food-grade marigold extract, and the preparation steps are as follows: 1) Weigh 1.0 kg of marigold granules with a unit content of 25.0 g / kg (purchased from Yanshan County Huafeng Agricultural Development Co., Ltd.), add 4000 ml of vegetable oil extraction solvent to fully extract, and concentrate the extract (the same concentration conditions as in Example 1) to obtain 576.8 ml of concentrate I with a solid content of 40%; 2) At 60°C, add 576.8 ml of 60° ethanol and 115.4 ml of 20% sodium hydroxide aqueous solution (the volume ratio of concentrate I: 60° ethanol: alkaline water is about 1:1:0.2), stir and mix thoroughly for 30 minutes, open the vent tube during the reaction to condense water to prevent the loss of solvent due to heat and volatilization, and separate and collect the upper alkane layer under static separation under heat preservation; repeat the above operation once for the alkane layer to obtain 571.2 ml of the primary decontaminated alkane layer; 3) After the primary deionized alkane layer was cooled to 30°C, 199.9 ml of 5% sodium chloride aqueous solution (the ratio of brine to alkane layer was approximately 0.35:1) was added, and the mixture was stirred for 15 min, and then the upper alkane layer was obtained by static separation; the alkane layer was collected and the above operation was repeated once, and finally 567.3 ml of the secondary deionized alkane layer was obtained; 4) The secondary alkane layer after impurity removal was concentrated at 60°C and -0.07MPa to obtain 164.3g of concentrate II with a residual solvent content of 1450ppm; 5) At 65°C, add 410.8 ml of 80° ethanol to the concentrate II, with a weight-to-volume ratio of about 1:2.5, mix and stir thoroughly for 30 minutes, separate statically, and collect the lower extract layer; repeat the above operation twice to obtain 170.1 g of the ethanol extract layer; 6) 130.0 g of sunflower seed oil was added to the ethanol extract layer, and the residual solvent was less than 50 ppm after concentration and desolventization at 55° C. and −0.08 MPa for 2.0 h. The cooling liquid was turned on and the temperature was lowered according to the method described in Example 1. Finally, 277.1 g of food-grade marigold extract with a unit content of 85.9 g / kg was obtained, and the content yield was 95.21%; The food-grade marigold extract is placed at room temperature for 6 months in a non-solidified state with good fluidity, no stratification and no special smell of marigold extract.

[0058] Example 5 This embodiment relates to a food-grade marigold extract, and the preparation steps are as follows: 1) Weigh 1.0 kg of marigold granules with a unit content of 24.3 g / kg (purchased from Shache Co., Ltd. of Chenguang Biotechnology Group), add 4500 ml of vegetable oil extraction solvent to fully extract, and concentrate the extract by thin film evaporation at 65°C and -0.05 MPa to obtain 927.7 ml of concentrate I with a solid content of 25%; 2) At 55°C, add 927.7 ml of 60° ethanol and 92.77 ml of 20% sodium hydroxide aqueous solution, stir and mix thoroughly for 30 minutes. During the reaction, open the vent tube to condense water to prevent the loss of solvent due to heat and volatilization. Separate and collect the upper alkane layer at a static temperature. Repeat the above operation once for the alkane layer to obtain 919.9 ml of the first impurity-free alkane layer. 3) After the primary decontaminated alkane layer was cooled to 25°C, 322.0 ml of 5% sodium chloride aqueous solution (the ratio of brine to alkane layer was approximately 0.35:1) was added, and the mixture was stirred for 15 min. The upper alkane layer was obtained by static separation. The alkane layer was collected and the above operation was repeated once, and finally 916.2 ml of the secondary decontaminated alkane layer was obtained. 4) The secondary alkane layer after impurity removal was concentrated at 60°C and -0.07MPa to obtain 167.1g of concentrate II with a residual solvent of 1322ppm; 5) At 60°C, add 417.8 ml of 80° ethanol to the concentrate II at a weight-to-volume ratio of 1:2.5, mix and stir thoroughly for 30 min, separate statically, and collect the lower extract layer; repeat the above operation twice to obtain 171.3 g of ethanol extract layer; 6) 130.0 g soybean oil was added to the ethanol extract layer, and the residual solvent was less than 50 ppm after concentration and desolventization at 50° C. and −0.08 MPa for 2.0 h. The cooling liquid was turned on and the temperature was lowered according to the method described in Example 1. Finally, 294.2 g of food-grade marigold extract with a unit content of 80.9 g / kg was obtained, and the content yield was 97.95%; The food-grade marigold extract is placed at room temperature for 6 months in a non-solidified state with good fluidity, no stratification and no special smell of marigold extract.

[0059] Example 6 This embodiment relates to a food-grade marigold extract, and the preparation steps are as follows: 1) Weigh 1.0 kg of marigold granules with a unit content of 24.3 g / kg (purchased from Shache Co., Ltd. of Chenguang Biotechnology Group), add 4500 ml of vegetable oil extraction solvent to fully extract, and concentrate the extract by thin film evaporation at 65°C and -0.05 MPa to obtain 927.7 ml of concentrate I with a solid content of 25%; 2) At 55°C, add 927.7 ml of 55° ethanol and 92.77 ml of 20% sodium hydroxide aqueous solution, stir and mix thoroughly for 30 minutes. During the reaction, open the vent tube to condense water to prevent the loss of solvent due to heat and volatilization. Separate and collect the upper alkane layer at a static temperature. Repeat the above operation once for the alkane layer to obtain 921.8 ml of the first decontaminated alkane layer. 3) After the primary decontaminated alkane layer was cooled to 25°C, 322.0 ml of 5% sodium chloride aqueous solution (the ratio of brine to alkane layer was approximately 0.35:1) was added, and the mixture was stirred for 15 min, and the upper alkane layer was obtained by static separation; the alkane layer was collected and the above operation was repeated 3 times, and finally 919.1 ml of the secondary decontaminated alkane layer was obtained; 4) The secondary alkane-removed layer was concentrated at 60°C and -0.07 MPa to obtain 169.5 g of concentrate II with a residual solvent of 1701 ppm; 5) At 60°C, add 423.8 ml of 80° ethanol to the concentrate II at a weight-to-volume ratio of 1:2.5, mix and stir thoroughly for 30 min, separate statically, and collect the lower extract layer; repeat the above operation twice to obtain 173.9 g of the ethanol extract layer; 6) Add 130.0g soybean oil to the ethanol extract layer, concentrate and desolventize for 2.0h at 53°C and -0.08MPa until the residual solvent is less than 50ppm, turn on the coolant for stirring and cooling, control the cooling rate to 5°C / h, and cool to 38°C at a uniform rate, with a stirring rate of 20 rpm; after the temperature drops to 38°C, keep stirring for 6.0h, with a stirring rate of 40 rpm; continue stirring and cooling to 20°C, control the cooling rate to 5°C / h, with a stirring rate of 30 rpm; finally, obtain 295.9g of food-grade marigold extract with a unit content of 80.7g / kg, and a content yield of 98.27%; The marigold extract was placed at room temperature for 6 months in a non-solidified state with acceptable fluidity and an oil layer on the upper layer.

[0060] Example 7 This embodiment relates to a food-grade marigold extract, and the preparation steps are as follows: 1) Weigh 1.0 kg of marigold granules with a unit content of 24.3 g / kg (purchased from Shache Co., Ltd. of Chenguang Biotechnology Group), add 4500 ml of vegetable oil extraction solvent to fully extract, and concentrate the extract by thin film evaporation at 65°C and -0.05 MPa to obtain 927.7 ml of concentrate I with a solid content of 25%; 2) At 55°C, add 927.7 ml of 65° ethanol and 92.77 ml of 20% sodium hydroxide aqueous solution, stir and mix thoroughly for 30 minutes. During the reaction, open the vent tube to condense water to prevent the loss of solvent due to heat and volatilization. Separate and collect the upper alkane layer at a static temperature. Repeat the above operation once for the alkane layer to obtain 916.3 ml of the first decontaminated alkane layer. 3) After the primary deionized alkane layer was cooled to 25°C, 320.7 ml of 5% sodium chloride aqueous solution (the ratio of brine to alkane layer was approximately 0.35:1) was added, and the mixture was stirred for 15 min, and then the upper alkane layer was obtained by static separation; the alkane layer was collected and the above operation was repeated once, and finally 913.5 ml of the secondary deionized alkane layer was obtained; 4) The secondary alkane layer after impurity removal was concentrated at 60°C and -0.07MPa to obtain 164.8g of concentrate II with a residual solvent of 1277ppm; 5) At 60°C, add 412 ml of 85° ethanol to the concentrate II at a weight-to-volume ratio of 1:2.5, mix and stir thoroughly for 30 min, separate statically, and collect the lower extract layer; repeat the above operation twice to obtain 172.7 g of the ethanol extract layer; 6) Add 130.0g soybean oil to the ethanol extract layer, concentrate and desolventize at 50℃ and -0.08MPa for 2.0h until the residual solvent is less than 50ppm, turn on the coolant for stirring and cooling, control the cooling rate to 5℃ / h, and uniformly cool to 38℃, during which the stirring rate is 20 rpm; continue stirring and cooling, control the uniform cooling to 30℃ within 10 minutes, during which the speed is 60 rpm; after the temperature drops to 30℃, keep warm and stir for 6.0h, during which the stirring rate is 40 rpm; continue stirring and cooling to 20℃, control the cooling rate to 5℃ / h, during which the stirring rate is 30 rpm; finally, 292.3g of food-grade marigold extract with a unit content of 80.1g / kg is obtained, and the content yield is 96.35%; The food-grade marigold extract is placed at room temperature for 6 months in a non-solidified state with good fluidity, no stratification and no special smell of marigold extract.

[0061] Example 8 This embodiment relates to a marigold extract, the first five steps of which are the same as those of Example 5, and step 6) the ethanol extract layer is not added with vegetable oil, and the residual solvent is less than 50 ppm after 4.0 hours of concentration and desolventization at 55°C and -0.08MPa, and the cooling liquid is turned on for stirring and cooling, and the cooling rate is controlled to be 5°C / h, and the temperature is uniformly reduced to 20°C, and the stirring rate is 20 rpm; finally, 170.2g of marigold extract with a unit content of 140.4g / kg is obtained, and the content yield is 98.34%; the product has a good smell. The marigold extract is placed at room temperature for 6 months, and the product solidifies and has no fluidity.

[0062] The extract layers obtained in step 5) of Examples 1-7 of the present invention were directly used to prepare marigold extract according to the method of Example 8, and the products finally obtained also had good smell.

[0063] Comparative Example 1 This comparative example relates to a marigold extract, and its preparation steps are as follows: 1) Weigh 1.0 kg of marigold granules with a unit content of 25.0 g / kg (purchased from Yanshan County Huafeng Agricultural Development Co., Ltd.), add 4500 ml of vegetable oil extraction solvent to fully extract, and the extract is concentrated by thin film evaporation at 55°C and -0.08 MPa to obtain 461.4 ml of concentrate I with a solid content of 50%; 2) At 55°C, add 461.4 ml of 60° ethanol and 46.1 ml of 20% sodium hydroxide aqueous solution (the volume ratio of concentrate I: 60° ethanol: alkaline water is about 1:1:0.1), stir and mix thoroughly for 30 minutes. During the reaction, open the vent tube to condense water to prevent the loss of solvent due to heat and volatilization. Separate and collect the upper alkane layer under static separation under heat preservation; repeat the above operation once for the alkane layer to obtain 430.2 ml of the primary decontaminated alkane layer; 3) After the primary deionized alkane layer was cooled to 25°C, 150.6 ml of 5% sodium chloride aqueous solution (the ratio of brine to alkane layer was approximately 0.35:1) was added, and the mixture was stirred for 15 min, and then the upper alkane layer was obtained by static separation. The alkane layer was collected and the above operation was repeated once, and finally 421.3 ml of the secondary deionized alkane layer was obtained. 4) The secondary de-doped alkane layer was concentrated at 60°C and -0.07 MPa to obtain 147.6 g of concentrate II with a residual solvent of 1428 ppm; 5) At 60°C, add 369 ml of 80° ethanol to the concentrate II, with a weight-to-volume ratio of 1:2.5, mix and stir thoroughly for 30 min, separate statically, and collect the lower extract layer; repeat the above operation twice to obtain 151.8 g of the ethanol extract layer; 6) 113.9 g of soybean oil was added to the ethanol extract layer, and the residue was concentrated and desolventized at 55° C. and −0.08 MPa for 2.0 h. Then, the cooling liquid was turned on and the temperature was lowered according to the method described in Example 1. Finally, 241.4 g of marigold extract with a unit content of 95.96 g / kg was obtained, and the content yield was 92.66%. The product had a good smell, but the yield was significantly reduced.

[0064] The marigold extract was placed at room temperature for 6 months in a non-solidified state, with slightly viscous fluidity, no obvious stratification and no special smell of marigold extract.

[0065] Comparative Example 2 This comparative example relates to a marigold extract, and its preparation steps are as follows: 1) Weigh 1.0 kg of marigold granules with a unit content of 25.0 g / kg (purchased from Yanshan County Huafeng Agricultural Development Co., Ltd.), add 4500 ml of vegetable oil extraction solvent to fully extract, and the extract is concentrated by thin film evaporation at 55°C and -0.08 MPa to obtain 1169.8 ml of concentrate I with a solid content of 20%; 2) At 55°C, add 1169.8 ml of 60° ethanol and 117.0 ml of 20% sodium hydroxide aqueous solution (the volume ratio of concentrate I: 60° ethanol: alkaline water is about 1:1:0.1), stir and mix thoroughly for 30 minutes. During the reaction, open the vent tube to condense water to prevent the loss of solvent due to heat and volatilization. Separate and collect the upper alkane layer at a static temperature under insulation; repeat the above operation once for the alkane layer to obtain 1107.2 ml of the primary decontaminated alkane layer; 3) After the primary deionized alkane layer was cooled to 25°C, 387.5 ml of 5% sodium chloride aqueous solution (the ratio of brine to alkane layer was approximately 0.35:1) was added, and the mixture was stirred for 15 min, and then the upper alkane layer was obtained by static separation; the alkane layer was collected and the above operation was repeated once, and finally 1098.3 ml of the secondary deionized alkane layer was obtained; 4) The secondary alkane-removed layer was concentrated at 60°C and -0.07 MPa to obtain 176.8 g of concentrate II with a residual solvent of 1653 ppm; 5) At 60°C, add 442 ml of 80° ethanol to the concentrate II at a weight-to-volume ratio of 1:2.5, mix and stir thoroughly for 30 min, separate statically, and collect the lower extract layer; repeat the above operation twice to obtain 173.8 g of ethanol extract layer; 6) 130.0 g of soybean oil was added to the ethanol extract layer, and the residue was concentrated and desolventized at 55° C. and −0.08 MPa for 2.0 h. Then, the cooling liquid was turned on and the temperature was lowered according to the method described in Example 1. Finally, 300.5 g of marigold extract with a unit content of 82.1 g / kg was obtained, and the content yield was 98.68%. The product had a slight odor.

[0066] The marigold extract was placed at room temperature for 6 months in a non-solidified state, with slightly viscous fluidity, stratification, and a slight special smell of marigold extract.

[0067] Comparative Example 3 This comparative example relates to a marigold extract, and its preparation steps are as follows: 1) Weigh 1.0 kg of marigold granules with a unit content of 25.0 g / kg (purchased from Yanshan County Huafeng Agricultural Development Co., Ltd.), add 4500 ml of vegetable oil extraction solvent to fully extract, and the extract is concentrated by thin film evaporation at 65°C and -0.08 MPa to obtain 166.5 g of extract with a residual solvent of 1500 ppm; 2) At 55°C, add 416.3 ml of 80° ethanol to the extract at a weight-to-volume ratio of about 1:2.5, mix and stir thoroughly for 30 min, separate statically, and collect the lower extract layer; repeat the above operation and separate the extract layer once to obtain 170.3 g of ethanol-containing extract layer.

[0068] 3) 130.0 g of soybean oil was added to the ethanol extract layer, and the mixture was concentrated and desolventized at 55° C. and −0.08 MPa for 2.0 h. Then, the cooling liquid was turned on and the temperature was lowered according to the method described in Example 1. Finally, 300.7 g of marigold extract with a unit content of 81.8 g / kg was obtained, and the content yield was 98.40%. The product had good fluidity but had a certain unique marigold smell.

[0069] The marigold extract was placed at room temperature for 6 months in a non-solidified state, with slightly viscous fluidity, stratification, and a certain special smell of marigold extract.

[0070] Comparative Example 4 This comparative example provides a marigold extract, the preparation method of which is basically the same as that of Example 1, except that in step 2), 935.8 ml of 50° ethanol and 62.4 ml of 30% sodium hydroxide aqueous solution are added instead. The remaining steps are the same. Finally, 299.7 g of food-grade marigold extract with a unit content of 82.5 g / kg is obtained, and the content yield is 98.90%; The food-grade marigold extract is placed at room temperature for 6 months in a non-solidified state, with average fluidity, stratification, and a certain special smell of marigold extract.

[0071] Comparative Example 5 This comparative example provides a marigold extract, the preparation method of which is basically the same as that of Example 5, except that in step 2), 927.7 ml of 70° ethanol and 123.7 ml of 15% sodium hydroxide aqueous solution are added instead. The remaining steps are the same. Finally, 264.4 g of food-grade marigold extract with a unit content of 82.8 g / kg is obtained, and the content yield is 90.09%; the yield loss is relatively obvious.

[0072] The food-grade marigold extract is placed at room temperature for 6 months in a non-solidified state, has good fluidity, no stratification phenomenon, and no special smell of marigold extract.

[0073] Comparative Example 6 This comparative example provides a marigold extract, the preparation method of which is basically the same as that of Example 5, except that in step 3), the temperature is not lowered, and salt water is directly added for mixing and stirring. Finally, 295.6 g of food-grade marigold extract with a unit content of 81.0 g / kg is obtained, and the content yield is 98.53%; The food-grade marigold extract was left at room temperature for 6 months in a non-solidified state, with slightly viscous fluidity and stratification, and without the special smell of marigold extract.

[0074] Comparative Example 7 This comparative example provides a marigold extract, the preparation method of which is basically the same as that of Example 5, except that in step 5), anhydrous ethanol is added for mixing and stirring. Finally, 266.4 g of food-grade marigold extract with a unit content of 84.9 g / kg is obtained, and the content yield is 93.08%; there is a significant yield loss.

[0075] The food-grade marigold extract is placed at room temperature for 6 months in a non-solidified state, has good fluidity, has stratification, and has no special smell of marigold extract.

[0076] Comparative Example 8 This comparative example provides a marigold extract, the preparation method of which is basically the same as that of Example 1, except that in step 5), 75° ethanol is added for mixing and stirring. Finally, 301.8 g of food-grade marigold extract with a unit content of 79.2 g / kg is obtained, and the content yield is 95.61%; The food-grade marigold extract is placed at room temperature for 6 months in a non-solidified state, has good fluidity, has stratification, and has a certain special smell of marigold extract.

[0077] Experimental Example 1 In this experimental example, the marigold extract prepared in each example and the ordinary marigold extract without special treatment were analyzed by ultra-fast electronic nose. The statistical results are shown in Table 1. The spectra of each group are shown in Figures 1 to 18 It can be seen that the total volatile odor (unpleasant odor) of the marigold extract prepared by the method of the present invention is low.

[0078] Table 1 Experimental Example 2 In this experimental example, 8 evaluators conducted sensory evaluation on the odor of the marigold extract prepared in each example and the ordinary marigold extract without special treatment. The evaluation table is shown in Table 2, and the results are shown in Table 3. It can be seen that through the preparation method of the present invention, the unpleasant odors such as sour and astringent taste in the marigold extract can be almost completely removed, and the deodorizing effect is obvious.

[0079] Table 2 Sensory evaluation table Table 3 Sensory evaluation results Experimental Example 3 Accelerated stability and long-term stability evaluation Accelerated stability test: Use the centrifugation method to measure, take 15g of extract, add it into a centrifuge tube at 4000 rpm, centrifuge for 10 minutes, observe whether there is an oil layer on the upper layer of the centrifuge tube, if an oil layer is formed, use a vernier caliper with a precision of 0.1mm to measure the thickness of the oil layer and record it; in addition, take one sample from 1 / 5 of the distance below the liquid surface (upper layer sampling) and one sample from 1 / 5 of the distance above the bottom (lower layer sampling), test the unit content of the two samples, if the content difference does not exceed 2%, the upper and lower layers are determined to be stable.

[0080] Long-term stability test: Take 100L of extract sample and place it in a 100ml glass measuring cylinder. After the sample is placed for 6 months, observe whether stratification occurs. Use a vernier caliper with a precision of 0.1mm to measure the thickness of the oil layer and record it. In addition, use a sampling tube to take 1 sample from 1 / 5 of the distance below the extract liquid surface (upper layer sampling) and 1 sample from 1 / 5 of the distance above the bottom of the extract (lower layer sampling). Detect the unit content of the two samples. If the content difference does not exceed 2.5%, the upper and lower layers are determined to be stable.

[0081] The specific statistical results of each case are shown in Table 4.

[0082] Table 4 Experimental Example 4 Product Fluidity Evaluation The viscosity of the prepared marigold extract and the extract stored at room temperature for six months was tested, and the viscosity unit was mPa•s. The specific test was performed using a viscometer according to the rotation method in the national standard GB / T 10247-2008 viscosity measurement method, and the test temperature was 25°C. The specific statistical results of each case are shown in Table 5.

[0083] Table 5 Although the present invention has been described in detail above with general descriptions and specific embodiments, it is obvious to those skilled in the art that some modifications or improvements may be made thereto based on the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention all fall within the scope of protection claimed by the present invention.

Claims

1. A method for preparing marigold extract, characterized in that: include: (1) Using marigold granules obtained after fermentation, drying and granulation of marigold as raw materials, extracting with C6 alkane, concentrating the obtained extract to obtain a concentrate I with a solid content of 25-40%; (2) at 50-60°C, fully mixing a 55-65° low-carbon alcohol, an alkali solution with a concentration of 18-22% and the concentrate I, separating the upper layer to obtain a solvent layer for primary impurity removal; The volume ratio of the concentrate I, 55-65° low carbon alcohol and alkaline solution is 1:1:(0.1-0.2); (3) fully mixing the solvent layer obtained by the primary impurity removal with the salt solution at 20-30° C., separating the upper layer, and obtaining the solvent layer obtained by the secondary impurity removal; (4) concentrating the solvent layer obtained by the secondary impurity removal to obtain a concentrate II; (5) Fully mix the concentrate II with low-carbon alcohol at 80-85°C at 50-65°C, separate the lower layer, and obtain an extract layer.

2. The method according to claim 1, characterized in that The C6 alkane is one or more of a vegetable oil extraction solvent, n-hexane, 2-methylpentane, 3-methylpentane, methylcyclopentane, and cyclohexane, preferably a vegetable oil extraction solvent; The low-carbon alcohol is one or more of methanol, ethanol, and isopropanol, preferably ethanol; And / or, the alkaline solution is an aqueous solution of sodium hydroxide and / or potassium hydroxide; the salt solution is an aqueous solution of sodium chloride and / or potassium chloride.

3. The method according to claim 1 or 2, characterized in that: In step (3), the volume ratio of the solvent layer for primary impurity removal to the salt solution is 1:(0.34-0.36); the concentration of the salt solution is 4-6%.

4. The method according to any one of claims 1 to 3, characterized in that: In step (5), the mass volume ratio of the concentrate II to the 80-85° low-carbon alcohol is 1:(2-4) g / mL.

5. The method according to any one of claims 1 to 4, characterized in that: In steps (1) and (4), the concentration is carried out by heating vacuum concentration, the concentration temperature is 55-65°C, and the pressure is -0.05~-0.08Mpa; And / or, in step (4), the residual solvent of the concentrate II is 500-2000 ppm.

6. The method according to any one of claims 1 to 5, characterized in that: In step (1), during extraction, the mass volume ratio of the raw material to the C6 alkane is 1: (4-5) g / mL.

7. The method according to any one of claims 1 to 6, characterized in that: Step (2) is repeated once, step (3) is repeated 1-3 times, and step (5) is repeated 2-4 times.

8. The method according to any one of claims 1 to 7, characterized in that: After step (5), the method further includes the step of concentrating and removing the solvent in the extract layer, or after step (5), the method further includes the step of mixing the extract layer with vegetable oil, concentrating the extract layer, and cooling the extract layer.

9. The method according to claim 8, characterized in that The vegetable oil is soybean oil and / or sunflower oil; the mass ratio of the extract layer to the vegetable oil is 1:(0.5-1); And / or, the cooling method is: in the first stage, stirring and cooling from 50-55°C to 40±2°C, the cooling rate is 4-6°C / h, and the stirring speed is 18-22 rpm; in the second stage, stirring and cooling to 30±2°C is continued, and the stirring speed is controlled to be completed within 10 minutes, and the stirring speed is not less than 60 rpm, preferably the stirring speed is 60 rpm, and then the temperature is kept and stirred for 5.5-6.5h, and the stirring speed during the insulation period is 38-42 rpm; in the third stage, stirring and cooling to 20±2°C is continued, the cooling rate is 4-6°C / h, and the stirring speed is 28-32 rpm; And / or, the extract layer is mixed with the vegetable oil and concentrated under the conditions of a temperature of 50-55° C. and a vacuum degree of -0.08 to -0.1 MPa; And / or, the residual solvent after the extract layer is mixed and concentrated with the vegetable oil is less than 50 ppm.

10. A marigold extract, characterized in that: The method is prepared by any one of claims 1 to 9.

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