A production method and application of marigold extract

Abstract

The present invention relates to the technical field of natural product extraction, and specifically discloses a production method and application of marigold extract. The production method of the present invention comprises: (1) mixing marigold flowers with porous fiber materials, crushing and then squeezing and dehydrating to a water content of 40% to 60%, to obtain a first material; (2) adding the porous fiber material again, mixing with the first material, to obtain a second material, heating and drying the second material to dehydrate it to a water content of 20% to 30%, to obtain a third material; (3) crushing the third material and extracting it with an extraction solvent to obtain an extract. Compared with the traditional marigold processing technology, the method of the present invention avoids the cost investment and environmental pollution problems caused by fermentation, does not require the preparation of particles, stabilizes the production process, improves product quality and production efficiency, and has outstanding characteristics such as high content yield and environmental friendliness.

Description

Technical Field

[0001] The invention relates to the technical field of natural product extraction, in particular to a production method and application of a marigold extract. Background Art

[0002] Marigold extract is widely used in food, feed, nutritional supplements, medicine and other aspects as a colorant and nutritional supplement. Marigold flower is the main raw material of lutein. The traditional processing technology of marigold flower requires fermentation, drying, granulation and then extraction with vegetable oil extraction solvent. Generally, the marigold fermentation process takes 2 to 3 weeks, and there are strict requirements for the tank filling, pressing, and silage agent configuration and spraying of marigold flowers; the fermentation process will produce a large amount of wastewater, and the organic acid produced in the fermentation process makes the wastewater acidic and has an unpleasant odor, which has high requirements for subsequent sewage treatment and poses a greater environmental pollution problem; marigold extract produced by fermentation technology has poor fluidity and a sour smell due to the decomposition of some oil components by microorganisms during the fermentation process. The product is prone to residual thermophilic acid-resistant bacteria, which poses a food safety risk. During the marigold pressing process, some lutein in the tissue will be lost and difficult to recover, resulting in a low yield; during the drying process, in order to ensure the subsequent granulation effect, the moisture content needs to be controlled below 15%, resulting in the loss of lutein components and the conversion of trans components to cis components, causing a decline in product quality indicators. If granulation is not performed, the solvent will not be able to fully penetrate in the subsequent solvent extraction process, making it impossible to achieve full and effective extraction.

[0003] Sun Baoguo et al. (Chinese patent: CN112175871A) eliminated fermentation odor and shortened the fermentation cycle of fresh flower silage by using a coupled wall-breaking treatment method of multiple functional bacteria + composite enzyme preparations. Hui Bodi et al. (Chinese patent: CN109400512A) applied a combination of enzymes (including cellulase, pectinase and protease) to improve the extraction efficiency of carotenoid compounds (mainly lutein esters and zeaxanthin esters) from marigold flowers. However, the above-mentioned method using enzymes only improved the marigold silage process and only improved some of the problems caused by fermentation. Dang Yanyan et al. (Chinese patent: CN108929255B) shortened the extraction process by drying and crushing the flowers and then enzymatically hydrolyzing and salting out, but it is not convenient for large-scale industrial production.

[0004] If marigold is processed directly without silage, the cell wall cannot be destroyed, the lutein extraction efficiency is low, and the production cost is high. There will also be problems such as sticking to the furnace and blockage, and lutein cis-trans conversion, and the product yield and quality are difficult to guarantee.

[0005] Therefore, further research is needed on the industrial production method of marigold extract. Summary of the invention

[0006] The invention provides a production process of high-quality marigold extract with high economic feasibility and environmental friendliness.

[0007] In order to achieve this object, the technical solution of the present invention is as follows:

[0008] A method for producing a marigold extract, comprising:

[0009] (1) mixing marigold flowers with a porous fiber material, crushing them, and then pressing and dehydrating them to a water content of 40% to 60% to obtain a first material;

[0010] (2) adding the porous fiber material again and mixing it with the first material (breaking up and mixing it) to obtain a second material, heating and drying the second material to dehydrate it to a moisture content of 20% to 30% (preferably 25% to 30%) to obtain a third material;

[0011] (3) The third material is crushed and then extracted using an extraction solvent to obtain an extract.

[0012] The present invention has been found that by adding porous fiber materials respectively in the pressing and heating drying stages of the production method and combining the moisture content control of each dehydration step, the cell walls of fresh marigold flowers can be effectively destroyed and the lutein components can be fully released without using traditional enzymatic fermentation and drying granulation methods. While ensuring the extraction effect, the loss of active ingredients due to excessive drying and dehydration is avoided, and there is no problem of residual fermentation bacteria. The product has no sour and rancid smell, good fluidity and high yield.

[0013] In the production method of the present invention, the porous fiber material is one or more of coconut shell fiber, peanut shell fiber, and cotton stalk fiber. Preferably, the porous fiber material is a mixed fiber obtained by mixing coconut shell fiber and cotton stalk fiber in a mass ratio of (1.8-2.2):1. The preparation method of the porous fiber material comprises:

[0014] 1) crushing the raw material, sieving and retaining particles with a particle size of 1.0 mm to 5.0 mm, preferably 3 mm to 5 mm (screening out fine powder and large particles); the raw material is coconut shell, peanut shell or cotton stalk;

[0015] 2) Soaking with alkane reagents, ester reagents, and alcohol reagents in turn, and evaporating (evaporating and recovering the solvent) after soaking;

[0016] 3) Soaking with alkali and acid respectively;

[0017] 4) After eluting again with an alkane reagent, an ester reagent, and an alcohol reagent, the mixture is evaporated to dryness (evaporation, solvent recovery, and cooling).

[0018] The preferred porous fiber material of the present invention is compounded by two specific fibers, which can better ensure the processing and extraction effect.

[0019] The coconut shell in the raw material is preferably the inner husk of coconut.

[0020] The porous fiber material of the present invention is prepared by a specific method. The impurities and non-fiber components of the specific fiber material treated in sequence with the above-mentioned various reagents can be effectively removed, which can better ensure that the components of the fiber itself are not precipitated after entering the extraction process with marigold, thereby avoiding affecting the lutein content in the extract. When the fiber particles are within the preferred range, the lutein yield can be better guaranteed.

[0021] In the production method of the present invention, the alkane reagent is one of n-hexane, isopentane, cyclopentane, and a plant extraction solvent; the ester reagent is one of ethyl acetate and methyl acetate; the alcohol reagent is one of methanol, ethanol, and propanol; preferably, the alkane reagent is a plant extraction solvent, the ester reagent is ethyl acetate, and the alcohol reagent is ethanol, which can better ensure the lutein content and yield.

[0022] In the production method of the present invention, the acid is one or more of citric acid, acetic acid, and phosphoric acid, and the alkali is sodium hydroxide. Preferably, the acid is citric acid with a concentration of 0.4-0.6% (more preferably 0.5%), and the alkali is NaOH with a concentration of 0.15-0.25% (more preferably 0.2%).

[0023] In the method of the present invention, the fiber is first treated with a strong base and then with a weak acid, which can effectively remove various impurities and stabilize the pH value of the treated fiber between 4 and 6 to better cooperate with the subsequent extraction process and avoid affecting the extraction effect.

[0024] The material-liquid ratio during soaking in step 2) of the production method of the present invention is 1:(2.8-3.2), and each soaking takes 2 to 4 hours;

[0025] In the production method of the present invention, the material-liquid ratio during soaking in step 3) is 1:(1.5-2.5), the soaking time of the alkali is 1 to 6 hours, and the soaking time of the acid is 1 to 6 hours.

[0026] The present invention cooperates with the reagents used and performs soaking under the above soaking conditions to better ensure the treatment effect.

[0027] In the production method of the present invention, the extraction solvent includes a vegetable oil extraction solvent and acetone, the volume ratio of the vegetable oil extraction solvent to acetone is (3-10):1, preferably (5-8):1, and more preferably 5:1, and the pH value of the extraction solvent is 4-6 (preferably adjusted using citric acid).

[0028] The extraction solvent of the present invention is used for extraction, which can better ensure the extraction effect and has a high content of trans-lutein.

[0029] In the production method of the present invention, the mass volume ratio of the third material to the extraction solvent is 1: (5-15) kg / L, preferably 1: (7-8) kg / L, more preferably 1: 6 kg / L, and the extraction temperature is 30-45°C; preferably, a countercurrent continuous extraction method is adopted under an inert gas (such as nitrogen).

[0030] Preferably, the material (third material) after heating, drying and dehydration is crushed and then transported to an extraction device, and an acidic extraction solvent is used for extraction while an inert gas is introduced from the bottom.

[0031] In step (1) of the production method of the present invention, the mass ratio of the fresh marigold flowers to the porous fiber material is (9-11):1, preferably 10:1.

[0032] The present invention has studied the amount of fiber material added and found that when the fiber material is used in the above ratio, the cell walls of fresh marigold flowers can be effectively broken in step (1) without affecting the effective dehydration, which is conducive to taking into account both the yield and the production capacity. If too much fiber is added, the production capacity will be seriously affected.

[0033] In step (2) of the production method of the present invention, the mass ratio of the first material to the porous fiber material is (9-11):1.5, preferably 10:1.5.

[0034] Adding a specific proportion of fiber material again before drying in the above proportion can not only help improve the drying efficiency, but also prevent marigold from adhering to the drying equipment. It can be beneficial to quickly reduce the moisture content at the drying temperature, avoid long-term drying to reduce the content of active ingredients, and at the same time help to take into account both yield and production capacity.

[0035] In step (2) of the production method of the present invention, the heating and drying dehydration method is segmented heating and dehydration, specifically, firstly infrared heating is used to raise the temperature of the second material to 30-40°C, and then drying and heating dehydration is adopted, and the heating time of the second material during drying and heating is controlled to be ≤2min; preferably, the inlet air temperature during drying is 200-260°C, and the outlet air temperature is 40-70°C.

[0036] A drum dryer can be used for drying and heating. By adjusting the drum speed and fan frequency, the material can reach the target moisture content within ≤2 minutes with the help of the predetermined temperature and cellulose.

[0037] The present invention can better ensure the rapid drying of materials through a specific step-by-step heating method, thereby reducing the impact on the content of active ingredients.

[0038] The degree of crushing in step (1) of the production method of the present invention is such that the particle size of the fresh marigold flower is 1 mm to 10 mm. In step (3), the particle size of the third material after crushing is 20-30 meshes.

[0039] The production method of the present invention also includes the steps of filtering and concentrating the extract to remove the residual solvent.

[0040] In the production method of the present invention, the filtering method is multi-stage filtration, specifically, cross-flow filtration is first performed, the filter mesh number is 40 mesh, and then filtration is performed using a filter mesh number of 200 mesh;

[0041] And / or, the concentration method is vacuum concentration, the vacuum degree is maintained at 0-0.08 MPa, the concentration temperature is maintained at 30-50° C., and the residual solvent is removed to below 25 ppm.

[0042] As a specific embodiment of the present invention, the production method comprises the following steps:

[0043] (1) The raw materials for preparing the porous fiber material are crushed and sieved to retain particles with a particle size between 3 and 5 mm. The raw materials are soaked in plant extract solvent, ethyl acetate, and ethanol for 4 hours in sequence, and the solvent is evaporated and recovered. The raw materials are then soaked in 0.2% NaOH and 0.5% citric acid water for 4 hours in sequence, and finally rinsed in plant extract solvent, ethyl acetate, and ethanol in sequence, and the solvent is evaporated and cooled to recover.

[0044] (2) Adding the treated porous fiber material to fresh marigold flowers at a ratio of 10:1, and squeezing and dehydrating the fresh marigold flowers until the water content is between 40% and 60%.

[0045] (3) adding the dehydrated flowers to the porous fiber material again at a ratio of 10:1.5, breaking and mixing, and further heating and dehydrating until the moisture content is 25% to 30%.

[0046] (4) After drying and crushing, the mixture is extracted with a plant extraction solvent and acetone mixed solvent, filtered, concentrated, and the solvent residue is removed to obtain a marigold extract.

[0047] The present invention preferably adds the treated porous fiber material to the marigold flowers, and achieves a faster and more effective dehydration effect by combining preliminary crushing, extrusion dehydration and multi-step drying dehydration, thereby avoiding the loss of active ingredients.

[0048] Specifically, the porous fiber material and the fresh flower are squeezed together to partially destroy the cell wall, and the loss of lutein is reduced during the squeezing process (during the squeezing of fresh flowers, the outflow of cell fluid will take away part of the lutein. The specific fiber material added in the present invention has a certain adsorption capacity, which can reduce the loss of lutein). The porous fiber material is added again after squeezing to avoid the problem of sticking to the furnace during the heating process of sugar in the fresh flower. At the same time, the process avoids granulation, the drying process is gentle, and the moisture content after drying is maintained between 20% and 30%, avoiding the loss of active ingredient content and cis-trans conversion during the drying process. Finally, an acidic mixed solvent is used for extraction to ensure high yield and high trans content. The method of the present invention avoids the problems of environmental pollution and storage capacity limitation caused by traditional silage processes, reduces the sour and rancid taste of the extract, does not have the food safety risks of acidophilic thermotolerant bacteria, and has high economic feasibility and environmental friendliness.

[0049] The material-liquid ratio described in the present invention is a mass-to-volume ratio. In the mass-to-volume ratio described in the present invention, both mass and volume are standard units, and in the process of the ratio, grams correspond to milliliters, and kilograms correspond to liters.

[0050] The present invention also provides an application of the production method in preparing a lutein-containing product.

[0051] The beneficial effects of the present invention are at least:

[0052] The process of the invention reduces the cost of dehydrating fresh marigold flowers, and at the same time, completes the partial wall breaking of fresh flowers and reduces the loss of lutein in cell effluent during the dehydration process, avoids granulation, and allows the drying moisture content to be 20% to 30%, thereby reducing the quality problem of cis-trans conversion and avoiding the loss of lutein content, thereby improving the yield, and at the same time solves the process problems of oven sticking and clogging in non-silage drying, thereby reducing the production cost. The method of the invention has high economic feasibility and environmental friendliness, and is suitable for industrial large-scale production.

[0053] By adopting the method of the present invention, the lutein content yield can reach more than 99%, which is significantly higher than the traditional marigold processing method. The marigold extract has no sour smell and acidophilic thermotolerant bacteria, has a high trans ratio, good fluidity and good quality. DETAILED DESCRIPTION

[0054] 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.

[0055] 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.

[0056] Example 1

[0057] This embodiment provides a method for producing a marigold extract, comprising the following steps:

[0058] 1) Coconut shells and cotton stalks are crushed and sieved respectively, and particles with a particle size between 3.0 mm and 5.0 mm are retained. They are soaked in plant extraction solvent, ethyl acetate, and ethanol for 4 hours respectively, and the material-liquid ratio is 1:3 kg / L each time. After the soaking, the solvent is evaporated and recovered. Then, they are soaked in 0.2% NaOH and 0.5% citric acid water for 4 hours respectively, and the material-liquid ratio is 1:2 kg / L each time. The pH after the treatment is 4.5. Finally, they are washed with plant extraction solvent, ethyl acetate, and ethanol respectively, air-dried, and cooled to obtain coconut shell fibers and cotton stalk fibers.

[0059] 2) adding 500 kg of processed mixed fiber material (coconut shell fiber and cotton stalk fiber mixed in a mass ratio of 2:1) to 5000 kg of fresh marigold flowers, crushing the fresh flowers to a particle size of 5 mm to 10 mm, and squeezing and dehydrating the fresh flowers to a moisture content of 50%.

[0060] 3) Add 750 kg of the processed mixed fiber material to the squeezed and dehydrated material, break it up and mix it. First, use infrared heating to heat the material to 40°C, and then use a drum dryer to heat and dehydrate it. The drum dryer has an air inlet temperature of 230°C and an air outlet temperature of 60°C. By adjusting the drum speed and fan frequency to control the material heating time in the drum to 1.5 minutes, the material with a moisture content of 30% is obtained.

[0061] 4) After the dried material is crushed to 20 mesh, it is transported to the extraction equipment, and while nitrogen is filled from the bottom, a countercurrent continuous extraction method is used to extract with an extractant, the extractant is a mixed solvent of a plant extraction solvent and acetone adjusted to pH 4.5 with citric acid, filtered, concentrated, and the solvent residue is removed to obtain a marigold extract. The volume ratio of the plant extraction solvent and acetone in the mixed solvent is 5:1, the material-liquid ratio during extraction is 1:6kg / L, and the extraction temperature is 45°C. The filtration method is multi-stage filtration, first cross-flow filtration is performed, the filter mesh is 40 mesh, and then a stainless steel filter is used for filtration, and the filter mesh is 200 mesh. The concentration method is vacuum concentration, the vacuum degree is maintained at 0.08MPa, the concentration temperature is maintained at 40°C, and the solvent residue is removed to less than 25ppm.

[0062] Example 2

[0063] This embodiment provides a method for producing marigold extract. Compared with Embodiment 1, the difference lies in that in the step 1), after the fiber raw material is crushed and sieved, particles with a particle size of 1 mm to 3 mm are retained.

[0064] Example 3

[0065] This embodiment provides a method for producing marigold extract. Compared with Embodiment 1, the difference is that in step 1), only coconut shell is used as the raw material for fiber preparation, and in subsequent steps, only coconut shell fiber is used instead of mixed fiber material.

[0066] Example 4

[0067] This embodiment provides a method for producing marigold extract. Compared with Embodiment 1, the difference is that in step 1), only cotton stalks are used as raw materials for fiber preparation, and in subsequent steps, only coconut shell fibers are used instead of mixed fiber materials.

[0068] Example 5

[0069] This embodiment provides a production method of marigold extract. Compared with Example 1, the difference is that in step 1), peanut shells are used instead of cotton stalks as one of the fiber preparation raw materials, and the mixed fiber material in the subsequent steps is a mixed fiber of coconut shell fiber and peanut shell fiber (mass ratio is 2:1).

[0070] Example 6

[0071] This embodiment provides a production method of marigold extract. Compared with Example 1, the difference is that in step 1), peanut shells are used instead of coconut shells as one of the raw materials for fiber preparation, and the mixed fiber material in the subsequent steps is a mixed fiber of peanut shell fiber and cotton stalk fiber (mass ratio is 2:1).

[0072] Example 7

[0073] This embodiment provides a method for producing marigold extract. Compared with embodiment 1, the difference lies in that in step 2), the water content of the third material is controlled to 30% by squeezing and dehydrating to 40% by pressing, and in the subsequent step 3), the air inlet temperature is lowered to 200° C. and the drying time is shortened to 1.2 minutes.

[0074] Example 8

[0075] This embodiment provides a method for producing marigold extract. Compared with embodiment 1, the difference lies in that in step 3), the air inlet temperature is 260° C., and the moisture content of the third material is controlled to be 30% by shortening the drying time to 1 minute.

[0076] Example 9

[0077] This embodiment provides a method for producing marigold extract. Compared with embodiment 1, the difference is that in step 3), the air inlet temperature is increased to 250° C. and the drying time is extended to 2 minutes, so that the moisture content of the third material after drying is 25%.

[0078] Example 10

[0079] This embodiment provides a method for producing a marigold extract. Compared with Embodiment 1, the difference is that the pulverization particle size in step 4) is 30 mesh.

[0080] Embodiment 11

[0081] This embodiment provides a method for producing a marigold extract. Compared with Embodiment 1, the difference is that in the mixed solvent of step 4), the volume ratio of the vegetable oil extraction solvent to acetone is 3:1.

[0082] Example 12

[0083] This embodiment provides a method for producing a marigold extract. Compared with Embodiment 1, the difference is that the pH value of the mixed solvent in step 4) is 6.

[0084] Comparative Example 1

[0085] 1) Take 5000 kg of fresh marigold flowers, spray them with the Taiwan Asia-core marigold silage agent prepared according to the instruction manual, compact them, seal them with black plastic bags, and ferment them for 20 days.

[0086] 2) The fermented flowers are squeezed to a moisture content of 70%, and then transported to a hot air furnace (250° C.) for air drying to a moisture content of 15%.

[0087] 3) The dried material is crushed through a 40-mesh sieve and granulated.

[0088] 4) Extraction with plant extracting solvent in continuous countercurrent extraction with a solid-liquid ratio of 1:6.

[0089] 5) Filter, concentrate and remove the residual solvent by the method of Example 1 to obtain marigold extract.

[0090] Comparative Example 2

[0091] This comparative example provides a method for producing a marigold extract. Compared with Example 1, the difference is that the soaking sequence in step 1) is changed to ethanol, ethyl acetate, and plant extraction solvent.

[0092] Comparative Example 3

[0093] This comparative example provides a method for producing a marigold extract. Compared with Example 1, the difference is that the acid added in step 1) is changed to 0.5% hydrochloric acid.

[0094] Comparative Example 4

[0095] This comparative example provides a method for producing a marigold extract. Compared with Example 1, the difference is that the alkali added in step 1) is changed to 0.2% ammonia water.

[0096] Comparative Example 5

[0097] This comparative example provides a method for producing marigold extract, which is different from Example 1 in that in step 2), the fresh flower is crushed to a particle size of >10 mm and ≤15 mm.

[0098] Comparative Example 6

[0099] This comparative example provides a method for producing marigold extract. Compared with Example 1, the difference is that infrared preheating is not used in step 3), but the mixed material is directly heated and dehydrated by a drum dryer.

[0100] Comparative Example 7

[0101] This comparative example provides a method for producing a marigold extract, which is different from Example 1 in that the extraction solvent in step 4) only uses a plant extraction solvent.

[0102] Comparative Example 8

[0103] This comparative example provides a method for producing a marigold extract. Compared with Example 1, the difference is that the pH value of the mixed solvent in step 4) is 2.

[0104] Comparative Example 9

[0105] This comparative example provides a method for producing a marigold extract, which is different from Example 1 in that no nitrogen is introduced in step 4).

[0106] Comparative Example 10

[0107] This comparative example provides a method for producing a marigold extract. Compared with Example 1, the difference is that ethanol is used to replace the acetone in the extraction solvent in step 4).

[0108] Comparative Example 11

[0109] This comparative example provides a method for producing marigold extract. Compared with Example 1, the difference is that in step 1), the solvent soaking sequence is changed, and the crushed coconut shells and cotton stalks are soaked in ethanol, ethyl acetate, and plant extraction solvent respectively.

[0110] Comparative Example 12

[0111] This comparative example provides a method for producing marigold extract. Compared with Example 1, the difference lies in that in step 1), the first soaking solvent sequence is changed, and the crushed coconut shells and cotton stalks are soaked in acetone, ethyl acetate and ethanol respectively.

[0112] Experimental Example 1

[0113] The lutein in the marigold extract obtained in the embodiment and the comparative example was detected by high performance liquid chromatography, and the detection conditions were:

[0114] Mobile phase: n-hexane:acetone=81:19, mobile phase flow rate: 1.0mL / min, column temperature: 28°C; chromatographic column: Kromasil 100~5SIL 150*4.6mm; UV detector wavelength: 474nm; injection volume: 20μL.

[0115] Experimental Example 2

[0116] The marigold extracts obtained in the examples and comparative examples were placed in clean sample bottles, sealed and placed at room temperature in the tasting laboratory. Three inspectors evaluated and described each sample in turn. The odor intensity was divided into 6 levels, 1-2 for grassy smell, 3-4 for sour smell, and 5-6 for sour smell. Each person evaluated no more than 5 samples in a row.

[0117] Experimental Example 3

[0118] Place the marigold extract obtained in the examples and comparative examples in a 40°C water bath for 30 minutes. Take the water-bathed sample out of the water bath and immediately pour it into a 250mL beaker. The sample volume should be sufficient to cover the mark on the rotor of the viscosity tester (NDJ-5S Shanghai Nirun), and the test should be performed immediately. Adjust the viscometer to a horizontal position; screw the rotor protection frame to the right and install it on the viscometer, and screw the selected rotor to the left into the connecting screw. Turn on the machine and press the rotor key to enter the required rotor number. Press the speed key to select the required speed; rotate the lifting frame knob to slowly lower the viscometer, and gradually immerse the rotor in the liquid to be tested until the mark on the rotor is level with the liquid surface. Press the measurement key and read the sample viscosity value after 0.5 minutes; during the measurement process, if the rotor selection is inappropriate and needs to be replaced, press the reset key directly, and re-enter the rotor number, speed, detection, and reading after the replacement is completed.

[0119] The results of the unit content, trans ratio, yield, odor and viscosity of marigold extract are shown in Table 1.

[0120] Table 1 Content and yield of marigold extracts from different processes

[0121]

[0122]

[0123] Compared with the traditional fermentation process, the marigold extract obtained by the process of the invention has no sour smell, better fluidity and does not contain acidophilic and thermotolerant bacteria.

[0124] It can be seen from the above examples that the method of the present invention can be used to obtain marigold lutein with high content, trans ratio and yield.

[0125] 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 producing a marigold extract, characterized in that: include: (1) mixing marigold flowers with a porous fiber material, crushing them, and then pressing and dehydrating them to a water content of 40% to 60% to obtain a first material; (2) adding the porous fiber material again and mixing it with the first material to obtain a second material, and heating and drying the second material to dehydrate it to a moisture content of 20% to 30% to obtain a third material; (3) crushing the third material and extracting it with an extraction solvent to obtain an extract; the extraction solvent comprises a vegetable oil extraction solvent and acetone, the volume ratio of the vegetable oil extraction solvent to the acetone is (3-10):1, and the pH value of the extraction solvent is 4-6; The porous fiber material is one or more of coconut shell fiber, peanut shell fiber, and cotton stalk fiber. The preparation method of the porous fiber material comprises: 1) The raw materials are crushed and sieved to retain particles with a particle size between 1.0 mm and 5.0 mm; The raw materials are coconut shells, peanut shells or cotton stalks; 2) Soaking with alkane reagent, ester reagent and alcohol reagent respectively, and evaporating after soaking; 3) soaking in alkali and acid respectively; the acid is one or more of citric acid, acetic acid and phosphoric acid, and the alkali is sodium hydroxide; 4) Rinse again with alkane reagent, ester reagent and alcohol reagent respectively, and evaporate to dryness.

2. The production method according to claim 1, characterized in that The porous fiber material is a mixed fiber obtained by mixing coconut shell fiber and cotton stalk fiber in a mass ratio of (1.8-2.2):

1.

3. The production method according to claim 1, characterized in that In the method for preparing the porous fiber material, in step 1), the raw material is crushed and sieved to retain particles with a particle size between 3 mm and 5 mm.

4. The production method according to claim 1, characterized in that The alkane reagent is one of n-hexane, isopentane, cyclopentane, and plant extraction solvent; the ester reagent is one of ethyl acetate and methyl acetate; the alcohol reagent is one of methanol, ethanol, and propanol; And / or, the acid is 0.4-0.6% citric acid and the base is 0.15-0.25% NaOH.

5. The production method according to claim 4, characterized in that: The alkane reagent is a plant extraction solvent, the ester reagent is ethyl acetate, and the alcohol reagent is ethanol.

6. The production method according to claim 1, characterized in that: The material-liquid ratio during soaking in step 2) is 1:(2.8-3.2), and each soaking takes 2 to 4 hours; And / or, the material-liquid ratio during soaking in step 3) is 1:(1.5-2.5), the soaking time of the alkali is 1 to 6 hours, and the soaking time of the acid is 1 to 6 hours.

7. The production method according to claim 1, characterized in that: The mass volume ratio of the third material to the extraction solvent is 1: (5-15) kg / L, and the extraction temperature is 30-45° C.; And / or, in step (1), the mass ratio of the marigold flowers to the porous fiber material is (9-11):1; And / or, in step (2), the mass ratio of the first material to the porous fiber material is (9-11):1.

5.

8. The production method according to claim 7, characterized in that: The volume ratio of the vegetable oil extraction solvent to acetone is (5-8):1; And / or, the extraction of the third material is carried out under inert gas by countercurrent continuous extraction.

9. The production method according to any one of claims 1 to 8, characterized in that: In step (2), the heating and drying dehydration method is staged heating and dehydration, specifically, infrared heating is first used to raise the temperature of the second material to 30-40° C., and then drying and heating dehydration are used, and the heating time of the second material in the drying and heating is controlled to be ≤2 minutes.

10. The production method according to claim 9, characterized in that: The inlet air temperature during drying is 200-260°C, and the outlet air temperature is 40-70°C.

11. The production method according to any one of claims 1 to 8 and 10, characterized in that: The degree of crushing in step (1) is such that the particle size of the fresh marigold flower is 1 mm to 10 mm; And / or, in step (3), the particle size of the third material after crushing is 20-30 mesh.

12. The production method according to claim 9, characterized in that: The degree of crushing in step (1) is such that the particle size of the fresh marigold flower is 1 mm to 10 mm; And / or, in step (3), the particle size of the third material after crushing is 20-30 mesh.

13. The production method according to any one of claims 1 to 8, 10 and 12, characterized in that: The method also includes the steps of filtering and concentrating the extract to remove residual solvent.

14. The production method according to claim 9, characterized in that: The method also includes the steps of filtering and concentrating the extract to remove residual solvent.

15. The production method according to claim 11, characterized in that: The method also includes the steps of filtering and concentrating the extract to remove residual solvent.

16. The production method according to claim 13, characterized in that: The filtration method is multi-stage filtration, specifically, cross-flow filtration is first performed, the filter mesh number is 40 mesh, and then filtration is performed using a filter mesh number of 200 mesh; And / or, the concentration method is vacuum concentration, the vacuum degree is maintained at 0-0.08 MPa, the concentration temperature is maintained at 30-50° C., and the residual solvent is removed to below 25 ppm.

17. The production method according to claim 14 or 15, characterized in that: The filtration method is multi-stage filtration, specifically, cross-flow filtration is first performed, the filter mesh number is 40 mesh, and then filtration is performed using a filter mesh number of 200 mesh; And / or, the concentration method is vacuum concentration, the vacuum degree is maintained at 0-0.08 MPa, the concentration temperature is maintained at 30-50° C., and the residual solvent is removed to below 25 ppm.

18. Use of the production method according to any one of claims 1 to 17 in the preparation of a lutein-containing product.

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