Method for extracting lycopene

Abstract

The invention relates to the technical field of extraction, and discloses a method for extracting lycopene, which comprises the following steps: extracting a sample to be treated to obtain crude lycopene extract; performing chromatographic membrane purification treatment on the crude lycopene extracting solution to obtain a lycopene extract; wherein the chromatography membrane comprises a lysine modified cellulose membrane. According to the extraction method, specific adsorption of lycopene is achieved by introducing the cellulose membrane of lysine, meanwhile, the extraction method has the advantages of being high in extraction efficiency and recovery efficiency, mild in operation condition and the like, and is wide in application range and suitable for large-scale industrial production.

Description

Technical Field

[0001] The invention belongs to the technical field of extraction, and in particular relates to a method for extracting lycopene. Background Art

[0002] Lycopene is a natural red open-chain hydrocarbon carotenoid with poor stability. It is mainly found in tomatoes, tomato products, watermelon, grapefruit and other fruits. Lycopene appears as dark red needle-shaped crystals, soluble in chloroform, benzene and oils but not in water. It has strong antioxidant effects, protects the skin, prevents cardiovascular and cerebrovascular diseases, and improves immunity. It is usually used as a pigment additive and antioxidant raw material in food processing.

[0003] At present, the market demand for high-purity lycopene is growing, especially in the food industry and health care products. Traditional lycopene extraction methods usually include organic solvent extraction, chromatography, crystallization and drying. These methods can achieve the extraction and purification of lycopene to a certain extent, but often have problems such as low extraction efficiency, low purity, complex operation or high cost.

[0004] Therefore, there is an urgent need to develop a method for extracting lycopene that is simple to operate, has high extraction efficiency, mild operating conditions, and is suitable for large-scale industrial production to meet the needs of large-scale industrial production of lycopene. Summary of the invention

[0005] The present invention aims to solve at least one of the technical problems existing in the prior art to a certain extent. To this end, the present invention provides a method for extracting lycopene. The extraction method of the present invention achieves specific adsorption of lycopene by introducing lysine into a cellulose membrane, and has the advantages of high extraction efficiency, high recovery efficiency, mild operating conditions, etc., and has a wide range of applications and is suitable for large-scale industrial production.

[0006] The present invention proposes a method for extracting lycopene. According to an embodiment of the present invention, the method comprises: subjecting a sample to be processed to extraction treatment to obtain a crude lycopene extract; subjecting the crude lycopene extract to chromatography membrane purification treatment to obtain a lycopene extract; wherein the chromatography membrane comprises a lysine-modified cellulose membrane. According to the extraction method of the embodiment of the present invention, the specific adsorption of lycopene is achieved by introducing a lysine-modified cellulose membrane, and the method has the advantages of high extraction efficiency, high recovery efficiency, mild operating conditions, etc., and has a wide range of applications and is suitable for large-scale industrial production.

[0007] According to an embodiment of the present invention, the above method for separating and purifying lycopene may also have the following additional technical features:

[0008] According to an embodiment of the present invention, the extraction process comprises the following steps: (1) mixing a sample to be processed and a first organic solvent to obtain an organic solvent extraction mixture, subjecting the organic solvent extraction mixture to solid-liquid separation, and collecting a filtrate and a solid residue; (2) mixing the solid residue and a second organic solvent, and collecting a filtrate and a solid residue; repeating step (2) 1 to 4 times, combining all filtrates, and obtaining the lycopene crude extract.

[0009] According to an embodiment of the present invention, the mass volume ratio of the sample to be processed and the first organic solvent is 1:(3-10), expressed in kg / L; the mass volume ratio of the solid residue and the second organic solvent is 1:(3-10), expressed in kg / L.

[0010] According to an embodiment of the present invention, the mixing time in step (1) is 3 to 6 hours and the temperature is 20 to 40°C.

[0011] According to an embodiment of the present invention, the mixing time in step (2) is 3 to 6 hours and the temperature is 20 to 40°C.

[0012] According to an embodiment of the present invention, the first organic solvent and the second organic solvent independently include one or more of ethyl acetate, ethanol, methanol, and acetone.

[0013] According to an embodiment of the present invention, the chromatographic membrane purification treatment comprises: adding the crude lycopene extract to a chromatographic column provided with the chromatographic membrane, adding an eluent to the chromatographic column, collecting the effluent, and obtaining the lycopene extract; before performing the chromatographic membrane purification treatment, the crude lycopene extract is concentrated.

[0014] According to an embodiment of the present invention, the eluent comprises petroleum ether and ethyl acetate, and the volume ratio of the petroleum ether to ethyl acetate is (5-15):1.

[0015] According to an embodiment of the present invention, based on 1 kg of the sample to be processed, the amount of the eluent used is 8 to 30 L.

[0016] According to an embodiment of the present invention, the elution flow rate of the eluent is 4 to 7 L / h.

[0017] According to an embodiment of the present invention, the method further comprises: subjecting the lycopene extract to recrystallization to obtain a purified lycopene; subjecting the purified lycopene to washing to obtain crude lycopene; subjecting the crude lycopene to drying to obtain refined lycopene; wherein the recrystallization temperature is 0 to 40°C, the drying temperature is 37 to 50°C, and the drying time is 12 to 24 hours.

[0018] According to an embodiment of the present invention, the cleaning process comprises: cleaning the purified lycopene with a cleaning solution to obtain crude lycopene; wherein the cleaning solution comprises at least one of ethanol, methanol, acetone and ethyl acetate.

[0019] According to an embodiment of the present invention, the preparation method of the lysine-modified cellulose membrane includes: a first mixing of a cellulose membrane, a strong oxidant and a catalyst to obtain a cellulose membrane having an aldehyde group; a second mixing of the cellulose membrane having an aldehyde group and lysine to obtain a cellulose membrane introduced with lysine; and a third mixing of the cellulose membrane introduced with lysine, a strong reducing agent and a buffer to obtain a lysine-modified cellulose membrane.

[0020] According to an embodiment of the present invention, the strong oxidant includes at least one of potassium periodate and sodium periodate.

[0021] According to an embodiment of the present invention, the catalyst is a strong acid solution, including at least one of a sulfuric acid solution, a hydrochloric acid solution, and a nitric acid solution.

[0022] According to an embodiment of the present invention, the strong reducing agent is a strong alkaline solution, including at least one of potassium borohydride and sodium hydride.

[0023] According to an embodiment of the present invention, the buffer comprises at least one of sodium carbonate and sodium bicarbonate.

[0024] According to an embodiment of the present invention, the concentration of the strong oxidant is 20-30 g / L.

[0025] According to an embodiment of the present invention, the concentration of the catalyst is 15-25 ml / L.

[0026] According to an embodiment of the present invention, the time for the first mixing, the second mixing and the third mixing is 8 to 24 hours.

[0027] According to an embodiment of the present invention, the concentration of the strong reducing agent is 10-15 g / L.

[0028] According to an embodiment of the present invention, the concentration of lysine is 30-35 g / L.

[0029] According to an embodiment of the present invention, the pH of the buffer solution is 9-10. DETAILED DESCRIPTION

[0030] The embodiments of the present invention are described in detail below. The embodiments described below are exemplary and are only used to explain the present invention, and should not be understood as limiting the present invention.

[0031] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

[0032] In this document, the terms “include” or “comprising” are open expressions, that is, including the contents specified in the present invention but not excluding other contents.

[0033] The present invention proposes a method for extracting lycopene. According to an embodiment of the present invention, the method comprises: subjecting a sample to be processed to extraction treatment to obtain a crude lycopene extract; subjecting the crude lycopene extract to chromatography membrane purification treatment to obtain a lycopene extract; wherein the chromatography membrane comprises a lysine-modified cellulose membrane. According to the extraction method of the embodiment of the present invention, the specific adsorption of lycopene is achieved by introducing a lysine-modified cellulose membrane, and the method has the advantages of high extraction efficiency, high recovery efficiency, mild operating conditions, etc., and has a wide range of applications and is suitable for large-scale industrial production.

[0034] According to an embodiment of the present invention, the extraction process comprises the following steps: (1) mixing a sample to be processed with a first organic solvent to obtain an organic solvent extraction mixture, subjecting the organic solvent extraction mixture to solid-liquid separation, and collecting a filtrate and a solid residue; (2) mixing the solid residue with a second organic solvent, and collecting a filtrate and a solid residue; repeating step (2) 1 to 4 times, combining all filtrates, and obtaining the lycopene crude extract. First, an organic solvent is used to extract the sample to be processed, so that the lycopene in the sample to be processed can be separated, impurities can be removed, and subsequent chromatographic membrane treatment can be facilitated; if a chromatographic membrane is used directly for treatment, impurities in the sample to be processed can easily cause damage to the chromatographic membrane, affecting its service life.

[0035] According to an embodiment of the present invention, the mass volume ratio of the sample to be processed and the first organic solvent is 1:(3-10), in kg / L. Exemplarily, the mass volume ratio of the sample to be processed and the first organic solvent (in kg:L) is 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, preferably 1kg:(5-8)L, more preferably 1kg:(5-6)L. Thus, the organic solvent fully extracts the lycopene in the sample to be processed, further improving the extraction rate of lycopene.

[0036] According to an embodiment of the present invention, the mass volume ratio of the solid residue to the second organic solvent is 1:(3-10), in kg / L. Exemplarily, the mass volume ratio of the solid residue to the second organic solvent in step (2) (in kg:L) is 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, preferably 1kg:(5-8)L, more preferably 1kg:(5-6)L. Thus, the organic solvent fully extracts the lycopene remaining in the solid residue, further improving the extraction rate of lycopene.

[0037] According to an embodiment of the present invention, the mixing time in step (1) is 3 to 6 hours. Exemplarily, the mixing time in step (1) is 3 hours, 4 hours, 5 hours, 6 hours, preferably 4 hours. Thus, the organic solvent and the sample to be processed are fully mixed, which can further improve the extraction rate of lycopene.

[0038] According to an embodiment of the present invention, the temperature in step (1) is 20-40° C. Exemplarily, the temperature of the stirring treatment in step (1) is 20° C., 25° C., 30° C., 35° C., 40° C., preferably 30° C. Therefore, using an organic solvent to extract lycopene from the sample to be treated within this temperature range can protect lycopene and further improve the extraction rate of lycopene.

[0039] According to an embodiment of the present invention, the mixing time in step (2) is 3 to 6 hours. Exemplarily, the mixing time in step (2) is 3 hours, 4 hours, 5 hours, 6 hours, preferably 4 hours. Thus, the organic solvent and the solid residue are fully mixed, which can further improve the extraction rate of lycopene.

[0040] According to an embodiment of the present invention, the temperature in step (2) is 20-40° C. Exemplarily, the temperature of the stirring treatment in step (2) is 20° C., 25° C., 30° C., 35° C., 40° C., preferably 30-40° C. Therefore, using an organic solvent to extract lycopene from the solid residue within this temperature range can protect lycopene and further improve the extraction rate of lycopene.

[0041] According to an embodiment of the present invention, the first organic solvent and the second organic solvent independently include one or more of ethyl acetate, ethanol, methanol, and acetone. Thus, the method is applicable to a variety of organic solvents.

[0042] According to an embodiment of the present invention, the chromatographic membrane purification process comprises: adding the crude lycopene extract to a chromatographic column provided with the chromatographic membrane, adding an eluent to the chromatographic column, collecting the effluent, and obtaining the lycopene extract. Thus, the crude lycopene extract is purified by the eluent, and the lycopene content in the lycopene extract is further increased.

[0043] As used herein, the terms "eluent" and "eluent" are used synonymously.

[0044] According to an embodiment of the present invention, the eluent includes petroleum ether and ethyl acetate, and the volume ratio of the petroleum ether to ethyl acetate is (5-15): 1. Exemplarily, the volume ratio of the petroleum ether to ethyl acetate is 5: 1, 7: 1, 9: 1, 10: 1, 12: 1, 15: 1, preferably 10: 1. Thus, by optimizing the volume ratio of petroleum ether to ethyl acetate, the elution effect of the crude lycopene extract is optimized, and the extraction rate of lycopene is further improved.

[0045] According to an embodiment of the present invention, based on 1 kg of the sample to be processed, the amount of the eluent used is 8 to 30 L. Exemplarily, the amount of the eluent used is 8 L, 10 L, 15 L, 20 L, 25 L, 30 L, preferably 9 to 24 L, and more preferably 11 to 16 L. Thus, the eluent can fully elute the lycopene crude extract, further increasing the content of lycopene in the lycopene extract.

[0046] According to an embodiment of the present invention, the elution flow rate of the eluent is 4 to 7 L / h. Exemplarily, the elution flow rate of the eluent is 4 L / hour, 5 L / hour, 6 L / hour, 7 L / hour, preferably 5 to 6 L / hour, and more preferably 5 L / hour. Thus, the eluent is in full contact with the lycopene crude extract to fully elute the lycopene, further increasing the content of lycopene in the lycopene extract.

[0047] According to an embodiment of the present invention, the method further comprises: subjecting the lycopene extract to recrystallization to obtain a purified lycopene, thereby removing water from the lycopene extract and further improving the purity of the lycopene.

[0048] According to an embodiment of the present invention, the method further comprises: washing the purified lycopene to obtain crude lycopene, thereby removing impurities from the purified lycopene and further improving the purity of the lycopene.

[0049] According to an embodiment of the present invention, the method further comprises: drying the crude lycopene to obtain refined lycopene, thereby removing the washing liquid in the crude lycopene to obtain dry, high-purity refined lycopene.

[0050] According to an embodiment of the present invention, the temperature of the recrystallization treatment is 0-40° C. Exemplarily, the temperature of the recrystallization treatment is 0° C., 5° C., 10° C., 15° C., 20° C., 25° C., 30° C., 35° C., 40° C., preferably 0-10° C., more preferably 0-5° C. Thus, the water in the lycopene extract is removed, and the purity of the lycopene is further improved.

[0051] According to an embodiment of the present invention, the temperature of the drying treatment is 37-50° C. Exemplarily, the temperature of the drying treatment is 37° C., 38° C., 39° C., 40° C., 41° C., 42° C., 43° C., 44° C., 45° C., 46° C., 47° C., 48° C., 49° C., 50° C., preferably 37-42° C., more preferably 40° C. Thus, while ensuring the biological activity of lycopene, the washing liquid in the crude lycopene is removed to obtain dry, highly pure refined lycopene.

[0052] According to an embodiment of the present invention, the drying time is 12 to 24 hours. Exemplarily, the drying time is 12 hours, 14 hours, 16 hours, 18 hours, 20 hours, 22 hours, 24 hours, preferably 18 to 24 hours, and more preferably 18 hours. Thus, the washing liquid in the crude lycopene is fully removed to obtain dry, high-purity refined lycopene.

[0053] According to an embodiment of the present invention, the cleaning process includes: cleaning the purified lycopene with a cleaning solution to obtain crude lycopene; wherein the cleaning solution includes at least one of ethanol, methanol, acetone and ethyl acetate. Thus, the purified lycopene is cleaned with a cleaning solution such as ethanol to remove impurities from the purified lycopene and further improve the purity of the lycopene.

[0054] According to an embodiment of the present invention, the lycopene crude extract is concentrated before the chromatographic membrane purification process, thereby shortening the chromatographic membrane purification process time and improving the efficiency of the extraction work.

[0055] According to an embodiment of the present invention, the method for preparing the lysine-modified cellulose membrane comprises: first mixing a cellulose membrane, a strong oxidant and a catalyst to obtain a cellulose membrane having aldehyde groups. Thus, aldehyde groups are introduced into the cellulose membrane, making the surface of the cellulose membrane more active, providing active sites for the subsequent binding of the cellulose membrane with lysine.

[0056] According to an embodiment of the present invention, the cellulose membrane having aldehyde groups and lysine are mixed for a second time to obtain a cellulose membrane introduced with lysine, thereby introducing lysine into the cellulose membrane having carboxyl groups, which can specifically adsorb lycopene, further improving the lycopene extraction efficiency.

[0057] According to an embodiment of the present invention, the cellulose membrane into which lysine is introduced, a strong reducing agent and a buffer are subjected to a third mixing to obtain a lysine-modified cellulose membrane. Thus, by mixing with a strong reducing agent and a buffer, it is ensured that lysine reacts completely with the carboxyl groups on the cellulose membrane to form a stable lysine-modified cellulose membrane.

[0058] According to an embodiment of the present invention, the strong oxidant comprises at least one of potassium periodate and sodium periodate. Thus, the cellulose film is effectively oxidized to introduce carboxyl groups into the cellulose film.

[0059] According to an embodiment of the present invention, the catalyst is a strong acid solution, including at least one of a sulfuric acid solution, a hydrochloric acid solution, and a nitric acid solution, thereby accelerating the oxidation reaction of the cellulose membrane, improving the oxidation reaction efficiency, and ensuring the rapid introduction of carboxyl groups into the cellulose membrane.

[0060] According to an embodiment of the present invention, the strong reducing agent is a strong alkaline solution, including at least one of potassium borohydride and sodium hydride, thereby terminating the oxidation reaction of the cellulose membrane and ensuring the stability of the lysine-modified cellulose membrane.

[0061] According to an embodiment of the present invention, the buffer solution includes at least one of sodium carbonate and sodium bicarbonate. Thus, the buffer solution is used to provide suitable environmental conditions for the modification of the cellulose membrane.

[0062] According to an embodiment of the present invention, the concentration of the strong oxidant is 20 to 30 g / L. Exemplarily, the concentration of the strong oxidant is 20 g / L, 21 g / L, 22 g / L, 23 g / L, 24 g / L, 25 g / L, 26 g / L, 27 g / L, 28 g / L, 29 g / L, 30 g / L, preferably 23 to 27 g / L, more preferably 26 g / L. Thus, the cellulose film is effectively oxidized to introduce aldehyde groups into the cellulose film.

[0063] According to an embodiment of the present invention, the concentration of the catalyst is 15-25 ml / L. Exemplarily, the concentration of the catalyst is 15 mL / L, 16 mL / L, 17 mL / L, 18 mL / L, 19 mL / L, 20 mL / L, 21 mL / L, 22 mL / L, 23 mL / L, 24 mL / L, 25 mL / L, preferably 18-23 mL / L, more preferably 20 mL / L. Thus, the oxidation reaction of the cellulose film is accelerated, the oxidation reaction efficiency is improved, and the rapid introduction of aldehyde groups in the cellulose film is ensured.

[0064] According to an embodiment of the present invention, the time of the first mixing, the second mixing, and the third mixing is 8 to 24 hours. Exemplarily, the time of the first mixing, the second mixing, and the third mixing is 8 hours, 12 hours, 16 hours, 20 hours, and 24 hours. Thus, the cellulose membrane, the strong oxidant, and the catalyst fully react; the cellulose membrane with aldehyde groups and lysine fully react; and the cellulose membrane with lysine introduced, the strong reducing agent, and the buffer fully react.

[0065] According to an embodiment of the present invention, the concentration of the strong reducing agent is 10 to 15 g / L. Exemplarily, the concentration of the strong reducing agent is 10 g / L, 11 g / L, 12 g / L, 13 g / L, 14 g / L, 15 g / L, preferably 11 to 13 g / L, more preferably 12 g / L. Thus, the oxidation reaction of the cellulose membrane is terminated, ensuring the stability of the lysine-modified cellulose membrane.

[0066] According to an embodiment of the present invention, the concentration of lysine is 30-35 g / L. Exemplarily, the concentration of lysine is 30 g / L, 31 g / L, 32 g / L, 33 g / L, 34 g / L, 35 g / L, preferably 32.4 g / L. Thus, sufficient lysine is introduced to specifically adsorb lycopene more efficiently, further improving the lycopene extraction efficiency.

[0067] According to an embodiment of the present invention, the pH of the buffer solution is 9 to 10. Thus, the buffer solution is used to provide more suitable environmental conditions for the modification of the cellulose membrane.

[0068] The scheme of the present invention will be explained below in conjunction with the embodiments. It will be appreciated by those skilled in the art that the following embodiments are only used to illustrate the present invention and should not be considered as limiting the scope of the present invention. Where specific techniques or conditions are not indicated in the embodiments, the techniques or conditions described in the literature in this area or the product specifications are used. The reagents or instruments used are not indicated by the manufacturer and are all conventional products that can be obtained commercially.

[0069] Example 1: Preparation of lysine-modified cellulose membrane

[0070] 1. Weigh 13 g of KIO4, add it to 500 mL of deionized water, add 10 ml of concentrated sulfuric acid (98%, w / w), stir evenly, put in 10 g of cut cellulose membrane (60 um thick), react at room temperature for 12 hours, wash with deionized water to obtain a cellulose membrane with aldehyde groups.

[0071] 2. Weigh 16.2 g of lysine and dissolve it in water. Add it to the cellulose membrane with aldehyde groups. After reacting at room temperature for 12 hours, wash it with deionized water to obtain a cellulose membrane with lysine introduced.

[0072] 3. Add 6.0 g KBH4 to 500 mL sodium carbonate buffer with a pH value of 9.0, and then add the cellulose membrane introduced with lysine. After reacting at room temperature for 12 hours, wash with deionized water and dry to obtain a lysine-modified cellulose membrane.

[0073] Example 2: Extraction of lycopene

[0074] (1) Raw material preparation

[0075] 1 kg of food-grade lycopene was selected as the starting material, purchased from Wuhan Noreho Biotechnology Co., Ltd., and the purity of the starting material was 10%.

[0076] (2) Organic solvent extraction

[0077] 1 kg of food-grade lycopene was mixed with 5 L of ethanol (95%, v / v), stirred at room temperature for 3 hours, and then filtered to separate the solid residue, and the filtrate was collected. The solid residue was extracted again with 5 L of ethanol (95%, v / v), and this process was repeated three times to ensure the maximum extraction of lycopene, and the filtrates obtained by the three filtration separations were combined to obtain a crude lycopene filtrate.

[0078] (3) Concentration of lycopene

[0079] The lycopene crude filtrate was concentrated to 3 L at 40° C. to obtain a lycopene concentrated solution.

[0080] (4) Chromatographic membrane adsorption purification

[0081] The above lycopene concentrate was filtered and purified through the lysine-modified cellulose membrane prepared in Example 1, and the lycopene concentrate was loaded for filtration at a flow rate of 5 L / hour. After loading, a mixed solvent of petroleum ether and ethyl acetate (ratio of petroleum ether:ethyl acetate=10:1) was used as an eluent, and the lycopene was eluted with a total amount of 15 L of eluent and an eluent flow rate of 5 L / hour, and the eluate containing lycopene was collected.

[0082] (4) Recrystallization and drying

[0083] The eluate containing lycopene was concentrated at 40°C until solid precipitated, cooled to 0°C and stirred, filtered, and the filter cake was collected. The filter cake was rinsed with cold ethanol (95%, v / v) at 4°C, and vacuum dried at 40°C for 18 hours to collect the lycopene sample.

[0084] Examples 3-12: Optimization of lycopene extraction conditions

[0085] Compared with Example 2, the differences in the extraction conditions in Examples 3 to 12 are shown in Table 1. (Using Example 2 as a reference standard, "same as Example 2" in Table 1 means that the processing conditions in this step are exactly the same as those in Example 2, and "stirring for 5 hours" etc. are the changed condition parameters of this Example)

[0086] Table 1 Extraction parameters of lycopene

[0087]

[0088]

[0089] Example 13 Determination of the yield, recovery rate and purity of lycopene samples

[0090] The lycopene yield, recovery rate and purity of the lycopene extraction methods of Examples 2 to 12 were respectively detected. The specific detection steps are as follows:

[0091] (1) Determination of lycopene production

[0092] Collect the lycopene sample and weigh it with a balance, which is the yield of the lycopene sample in g.

[0093] (2) Determination of lycopene recovery

[0094] The purity of lycopene in the lycopene sample was measured according to GB1886.78-2016, and then the recovery rate was calculated according to Formula 1.

[0095] Recovery rate (%) = yield (g) * purity / (feeding amount (g) * 10%) Formula 1

[0096] The yield is the yield of the lycopene sample measured in step (1), in g; the feed amount is the weight of the food-grade lycopene raw material initially added, in g.

[0097] (3) Purity testing of lycopene

[0098] Take lycopene samples for purity testing, and the testing method is carried out with reference to GB1886.78-2016.

[0099] The yield, recovery rate and purity of lycopene samples are shown in Table 2.

[0100] Table 2 Results of yield, recovery and purity of lycopene samples

[0101]

[0102] The results show that as the amount of eluent increases, the yield of the lycopene sample increases, but at the same time the purity of the lycopene sample decreases. The amount of eluent can be selected according to the demand for lycopene products. When the amount of eluent is 18-24 L, the recovery rate is higher; when the amount of eluent is 9-15 L, the purity is higher; when the extraction is carried out under the conditions of stirring at room temperature for 5 h, the amount of secondary extraction ethanol is 6 L, the sample is loaded at a flow rate of 5 L / hour, the total amount of eluent is 15 L, and the eluent flow rate is 5 L / hour (Example 4), the recovery rate is 85.3% and the purity is 98%. At this time, both the recovery rate and the purity are relatively high.

[0103] The above results show that the lysine-modified cellulose membrane can be used to separate and purify lycopene, providing a new method for preparing high-purity and high-recovery lycopene.

[0104] Although the embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and are not to be construed as limitations of the present invention. A person skilled in the art may change, modify, replace and vary the above embodiments within the scope of the present invention.

Claims

1. A method for extracting lycopene, characterized in that: include: Extracting the sample to be processed to obtain a crude lycopene extract; Purifying the lycopene crude extract with a chromatographic membrane to obtain a lycopene extract; Wherein, the chromatographic membrane comprises a lysine-modified cellulose membrane.

2. The method according to claim 1, characterized in that The extraction process comprises the following steps: (1) mixing a sample to be processed and a first organic solvent to obtain an organic solvent extraction mixture, performing solid-liquid separation on the organic solvent extraction mixture, and collecting a filtrate and a solid residue; (2) mixing the solid residue with a second organic solvent, and collecting the filtrate and the solid residue; Repeat step (2) 1 to 4 times, combine all filtrates, and obtain the lycopene crude extract.

3. The method according to claim 2, characterized in that The mass volume ratio of the sample to be processed and the first organic solvent is 1:(3-10), in kg / L; The mass volume ratio of the solid residue to the second organic solvent is 1:(3-10), in kg / L; Optionally, the mixing time in step (1) is 3 to 6 hours and the temperature is 20 to 40° C.; Optionally, the mixing time in step (2) is 3 to 6 hours and the temperature is 20 to 40° C.; Optionally, the first organic solvent and the second organic solvent independently include one or more of ethyl acetate, ethanol, methanol, and acetone.

4. The method according to claim 1, characterized in that The chromatographic membrane purification process comprises: Adding the lycopene crude extract to a chromatography column provided with the chromatography membrane, then adding an eluent to the chromatography column, and collecting the effluent to obtain the lycopene extract; Before the chromatography membrane purification treatment, the lycopene crude extract is concentrated.

5. The method according to claim 4, characterized in that The eluent comprises petroleum ether and ethyl acetate, and the volume ratio of the petroleum ether to ethyl acetate is (5-15):1; Optionally, based on 1 kg of the sample to be processed, the amount of the eluent used is 8 to 30 L; Optionally, the elution flow rate of the eluent is 4 to 7 L / h.

6. The method according to claim 1, characterized in that The method further comprises: Recrystallizing the lycopene extract to obtain a purified lycopene; washing the purified lycopene to obtain crude lycopene; Drying the crude lycopene to obtain refined lycopene; Wherein, the temperature of the recrystallization treatment is 0-40°C, the temperature of the drying treatment is 37-50°C, and the time of the drying treatment is 12-24h.

7. The method according to claim 6, characterized in that The cleaning process comprises: washing the purified lycopene with a washing solution to obtain crude lycopene; Wherein, the cleaning liquid includes at least one of ethanol, methanol, acetone and ethyl acetate.

8. The method according to claim 1, characterized in that The preparation method of the lysine-modified cellulose membrane comprises: The cellulose film, the strong oxidant and the catalyst are first mixed to obtain the cellulose film having aldehyde groups; The cellulose membrane having an aldehyde group and lysine are mixed for a second time to obtain a cellulose membrane into which lysine is introduced; The cellulose membrane introduced with lysine, a strong reducing agent and a buffer are mixed for the third time to obtain a lysine-modified cellulose membrane.

9. The method according to claim 8, characterized in that The strong oxidant includes at least one of potassium periodate and sodium periodate; Optionally, the catalyst is a strong acid solution, including at least one of a sulfuric acid solution, a hydrochloric acid solution, and a nitric acid solution; Optionally, the strong reducing agent is a strong alkaline solution, including at least one of potassium borohydride and sodium hydride; Optionally, the buffer comprises at least one of sodium carbonate and sodium bicarbonate; Optionally, the concentration of the strong oxidant is 20 to 30 g / L; Optionally, the concentration of the catalyst is 15 to 25 mL / L; Optionally, the time for the first mixing, the second mixing, and the third mixing is 8 to 24 hours; Optionally, the concentration of the strong reducing agent is 10 to 15 g / L; Optionally, the concentration of lysine is 30-35 g / L; Optionally, the pH of the buffer is 9-10.

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