Sea buckthorn oil, extraction method and application thereof

Abstract

The invention provides a method for extracting seabuckthorn oil, and belongs to the field of oil processing. The extraction method provided by the invention comprises the following steps: soaking seabuckthorn pomace with water, then stirring evenly, then adding composite enzyme to keep warm, and centrifuging the enzymatic solution; adding 75% ethanol solution to the centrifugal precipitate for heating and reflux extraction, filtering the alcohol extract, combining the filter residue with the centrifugal solution, and then adding n-hexane for extraction, and recovering n-hexane from the extract to obtain crude seabuckthorn oil; adding activated carbon and silica gel powder to the crude seabuckthorn oil in sequence, stirring, placing, and filtering to obtain seabuckthorn oil. The seabuckthorn oil extraction method provided by the invention has a high oil yield, and the obtained seabuckthorn oil has a high content of effective ingredients, a low content of plasticizer and benzopyrene, good quality, and low equipment requirements, and is suitable for large-scale industrial production.

Description

Technical Field

[0001] The invention belongs to the field of oil processing, and in particular relates to sea buckthorn oil and an extraction method and application thereof. Background Art

[0002] Seabuckthorn (Latin name: Hippophae rhamnoides Linn.) is a deciduous shrub of the Elaeagnaceae family and the genus Hippophae. It is also known as sour willow fruit, sour willow, Qicharigacha (Mongolian name), Dapu (Tibetan name), and Jihan (Uyghur name). It is mainly distributed in more than ten provinces and regions in Northwest my country, North China, Northeast China and Southwest China, and is widely planted throughout the country. Seabuckthorn is a medicinal plant containing a variety of active substances such as vitamins, trace elements, amino acids and flavonoids. The oil content of seabuckthorn fruit is about 1.5%, of which pulp oil accounts for about 43% of the total, peel residue oil accounts for about 33%, and seed oil accounts for about 24%. The extracted seabuckthorn oil contains 206 kinds of beneficial active substances, which have many special functions such as repairing mucosal cells, preventing vascular sclerosis, improving immunity, and anti-oxidation. The market prospect is very broad.

[0003] At present, after the whole seabuckthorn fruit is pulped, the pomace (peel, pulp, and seeds) is dried outdoors, and then mechanically separated to obtain pomace (peel and pulp) and seeds, which are stored separately in plastic woven bags. The seeds are extracted with supercritical technology to extract seabuckthorn seed oil, and the pomace (peel and pulp) is used as feed. However, the outdoor drying process of the seabuckthorn pomace and seeds and the storage in plastic bags will increase the content of plasticizers and benzopyrene in the extracted seabuckthorn oil. Therefore, how to extract seabuckthorn oil from the seabuckthorn pomace without drying and storing it, and how to reduce the content of plasticizers and benzopyrene in the seabuckthorn oil has become a technical problem that needs to be solved in this field. Summary of the invention

[0004] In order to solve the above problems, the purpose of the present invention is to provide a sea buckthorn oil extraction method, which has high oil yield, high sea buckthorn oil quality, small solvent residue, simple extraction process, low equipment requirements, and can be used for large-scale industrial production.

[0005] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0006] The present invention provides a sea buckthorn oil extraction method, characterized in that it comprises the following steps:

[0007] (1) soaking seabuckthorn pomace in water, stirring evenly, adding composite enzyme to keep warm, centrifuging the enzymatic solution, and collecting the centrifuge and precipitate respectively; the composite enzyme comprises protease, cellulase and pectinase;

[0008] (2) adding 75% ethanol solution to the centrifugal precipitate for heating and refluxing extraction, filtering the ethanol extract, and mixing the filter residue with the centrifugal liquid obtained in step (1) to obtain a mixture;

[0009] (3) adding n-hexane to the mixture for extraction, and recovering n-hexane from the extract to obtain crude sea buckthorn oil;

[0010] (4) Add activated carbon and silica gel powder to the crude sea buckthorn oil in sequence, stir thoroughly, allow to stand, and filter to obtain sea buckthorn oil.

[0011] Preferably, in step (1), water 2 to 5 times the mass of the pomace is added and the mixture is soaked for 1 to 3 hours at a soaking temperature of 30 to 35°C.

[0012] Preferably, in step (1), the amount of protease added is 200-300 U / kg, the amount of cellulase added is 400-600 U / kg, and the amount of pectinase added is 400-600 U / kg.

[0013] Preferably, the insulation time of step (1) is 4 to 6 hours, and the temperature is 37 to 39°C.

[0014] Preferably, the centrifugation conditions in step (1) are 3000-5000 rpm, 1-3 min.

[0015] Preferably, the heating reflux extraction temperature in step (2) is 70 to 80° C. and the time is 10 to 30 minutes.

[0016] Preferably, in step (3), 80 to 100% of the volume of the mixture is added with n-hexane for extraction, the extraction temperature is 30 to 40° C., and the extraction time is 25 to 40 min.

[0017] Preferably, in step (4), the amount of activated carbon added is 2-6% of the mass of the sea buckthorn oil; and the amount of silica gel powder added is 5-8% of the mass of the sea buckthorn oil.

[0018] The invention also provides sea buckthorn oil prepared by the method.

[0019] The present invention also provides application of the seabuckthorn oil in preparing health products or cleaning products.

[0020] Beneficial effects of the present invention:

[0021] The invention adds water to seabuckthorn pomace (peel, pulp, seeds) to directly pulp and perform enzymolysis to extract oil without airing and storage, thereby avoiding the influence of plasticizers and benzopyrene, shortening the oil extraction process, and reducing production costs. Seabuckthorn oil is extracted from pomace (peel and pulp) used as feed in the prior art, thereby increasing the added value of the seabuckthorn pomace.

[0022] The extraction and refining method of the whole seabuckthorn fruit oil provided by the invention has high oil yield and simple operation steps, and does not need to separate the seabuckthorn seeds from the seabuckthorn peel and pulp. The prepared seabuckthorn oil has bright color and high transparency, and the organic solvent residue in the oil is small, and the plasticizer and benzopyrene contents are both low, so that the seabuckthorn oil is more in line with health standards.

[0023] The seabuckthorn oil prepared by the invention has high nutrient content, and the process steps cause less damage to the nutrients. The obtained seabuckthorn oil contains a large amount of unsaturated fatty acids and has excellent quality.

[0024] The extractant in the extraction method of the present invention can be recycled, which greatly reduces the consumption of the extractant and the generation of waste liquid, and the production process is more environmentally friendly. In addition, the method of the present invention has the advantages of simple operation, low equipment requirements, low cost, and is suitable for factory-scale large-scale production. DETAILED DESCRIPTION

[0025] The present invention provides a method for extracting seabuckthorn oil, comprising the following steps:

[0026] (1) soaking seabuckthorn pomace in water, stirring evenly, adding composite enzyme to keep warm, centrifuging the enzymatic solution, and collecting the centrifuge and precipitate respectively; the composite enzyme comprises protease, cellulase and pectinase;

[0027] (2) adding 75% ethanol solution to the centrifugal precipitate for heating and refluxing extraction, filtering the ethanol extract, and mixing the filter residue with the centrifugal liquid obtained in step (1) to obtain a mixture;

[0028] (3) adding n-hexane to the mixture for extraction, and recovering n-hexane from the extract to obtain crude sea buckthorn oil;

[0029] (4) Add activated carbon and silica gel powder to the crude sea buckthorn oil in sequence, stir thoroughly, allow to stand, and filter to obtain sea buckthorn oil.

[0030] In the present invention, the seabuckthorn pomace is obtained by mechanically crushing the whole seabuckthorn fruit and removing the juice. As an optional embodiment, the present invention selects the picked seabuckthorn fruits, removes the bad fruits, then rinses the seabuckthorn fruits with running water to remove the dirt on the surface, dries the surface moisture of the peel, puts them into a grinder for mechanical crushing, filters out the seabuckthorn juice, and directly obtains the standby seabuckthorn pomace.

[0031] The present invention adds water 2 to 5 times the weight of the seabuckthorn pomace, soaks for 1 to 3 hours, and the soaking temperature is 30 to 35° C. The amount of water added is preferably 3 to 4 times, the water is preferably deionized water, the soaking time is preferably 1.5 to 2 hours, and the soaking temperature is preferably 32 to 34° C. The present invention can make the seabuckthorn fruit seeds absorb water and swell, soften the seed cells, facilitate enzymolysis, extract the seabuckthorn oil, and improve the oil yield of the whole seabuckthorn fruit by adding water to the seabuckthorn pomace and soaking it.

[0032] The method stirs the soaked seabuckthorn pomace evenly, disperses the seabuckthorn peel, pulp and seeds that are statically soaked and precipitated by stirring, and then adds a composite enzyme for enzymolysis.

[0033] The present invention adds a composite enzyme to the sea buckthorn pomace for enzymolysis treatment, wherein the added amount of the protease is 200-300 U / kg of the mass of the sea buckthorn pomace, preferably 250-280 U / kg, more preferably 260 U / kg, the added amount of the cellulase is 400-600 U / kg of the mass of the sea buckthorn pulp, preferably 450-550 U / kg, more preferably 500 U / kg; the added amount of the pectinase is 400-600 U / kg of the mass of the sea buckthorn pulp, preferably 420-520 U / kg, more preferably 480 U / kg.

[0034] The present invention performs heat preservation enzymolysis on the seabuckthorn pomace-water mixture after adding the complex enzyme, the temperature is 37-39° C., preferably 38° C., and the heat preservation time is 4-6 hours, preferably 5 hours. During the heat preservation enzymolysis process of the seabuckthorn pomace-water mixture, the seabuckthorn pomace-water mixture can be placed in a constant temperature shaking incubator, or slowly mechanically stirred to avoid a large amount of precipitation of pulp cells.

[0035] The invention can demulsify the fruit pulp by adding protease to the seabuckthorn pomace-water mixture, so that the oil can be easily released from the seabuckthorn fruit cells, thereby improving the oil yield of the seabuckthorn fruit pulp; the invention can effectively degrade the crude fiber and pectin in the pomace by adding cellulase and pectinase to the seabuckthorn pomace-water mixture, thereby making the seabuckthorn oil more easily released.

[0036] The present invention centrifuges the enzymatically hydrolyzed seabuckthorn pomace-water mixture at 3000-5000 rpm for 1-3 min, preferably 4500 rpm for 3 min. The present invention uses a centrifuge to separate the enzymatic hydrolyzate of the seabuckthorn pomace-water mixture, and collects the centrifuge and the precipitate separately.

[0037] The present invention adds 75% ethanol solution to the precipitate obtained by the above centrifugation, stirs and then performs heating reflux extraction, wherein the ethanol solution is added in an amount of 5 to 15 mL / g (precipitate mass), preferably 10 to 12 mL / g. The heating reflux extraction temperature is 70 to 80° C., the time is 10 to 30 min, the extraction temperature is preferably 75° C., and the extraction time is preferably 15 to 20 min.

[0038] In the present invention, the heating reflux extraction process can be repeated 1 to 3 times. As an optional embodiment, the present invention adds 10 to 12 mL / g of 75% ethanol solution to the filter residue of the first alcohol extract for reflux extraction. The present invention can effectively remove the plasticizer in the seabuckthorn pomace through the heating reflux extraction process, so that the plasticizer content in the extracted seabuckthorn oil is significantly reduced.

[0039] The present invention combines the filter residue obtained by heating reflux extraction and the centrifugal liquid after enzymatic hydrolysis to obtain a mixture. Then, a n-hexane solution of 80 to 100% of the volume of the mixture is added for extraction, and the amount of the extractant added is preferably 85 to 95% of the volume of the mixture; the extraction temperature is 30 to 40° C., preferably 35 to 36° C.; and the extraction time is 25 to 40 minutes, preferably 30 to 32 minutes.

[0040] The present invention collects the extract and recovers the n-hexane to obtain the crude seabuckthorn oil. As an optional embodiment, the present invention recovers and removes the solvent by rotary evaporation to obtain the crude seabuckthorn oil.

[0041] The invention adds 2-6% activated carbon by weight of the sea buckthorn oil to the crude sea buckthorn oil, stirs it fully, leaves it for 10-40 minutes, filters it to remove the activated carbon, then adds 5-8% silica gel powder by weight of the sea buckthorn oil, stirs it fully, leaves it for 15-30 minutes, filters it to remove the silica gel powder, and obtains the sea buckthorn oil. The addition amount of the activated carbon in the invention is preferably 3-5%, and the addition amount of the silica gel powder is preferably 6-7%.

[0042] The present invention decolorizes and clarifies the crude seabuckthorn oil obtained by extraction by sequentially adding activated carbon and silica gel powder, thereby effectively removing impurities in the seabuckthorn oil, improving the clarity and quality of the seabuckthorn oil, and also effectively removing benzopyrene in the seabuckthorn oil.

[0043] The present invention also provides seabuckthorn oil prepared by the extraction method. The seabuckthorn oil has pure color, high transparency, high content of effective ingredients, low solvent residue, and low content of benzopyrene.

[0044] The present invention also provides the use of the seabuckthorn oil in preparing health products or cleaning products. When preparing health products, the seabuckthorn oil can be used to prepare health products with functions such as regulating the stomach and intestines, protecting blood vessels, protecting liver functions, and improving body immunity; when preparing cleaning products, the seabuckthorn oil can be used to prepare fine products with functions such as whitening, moisturizing, and repairing.

[0045] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0046] Example 1

[0047] This embodiment provides a method for extracting seabuckthorn oil, comprising the following steps:

[0048] (1) picking fresh seabuckthorn fruits and selecting them, removing bad fruits, then washing the seabuckthorn fruits with running water to remove dirt on the surface, drying the surface moisture of the peel, putting them into a grinder for mechanical crushing, filtering out the seabuckthorn juice, and setting aside the seabuckthorn pomace;

[0049] (2) Add water 3 times the weight of the pomace to the crushed seabuckthorn pomace and soak at 32°C for 1.5 h;

[0050] (3) The soaked seabuckthorn pulp is stirred evenly, and a composite enzyme is added, including 280 U / kg of protease, 450 U / kg of cellulase, and 500 U / kg of pectinase;

[0051] (4) keeping the mixture at 38°C for 5 h for enzymatic hydrolysis, centrifuging the seabuckthorn pulp at 4500 rpm for 3 min at room temperature, and collecting the centrifuge liquid and the centrifugal precipitate;

[0052] (5) Add 75% ethanol solution to the centrifugal precipitate and heat reflux extraction twice: first add 15 mL / g (precipitate mass) of ethanol solution, stir to dissolve, heat reflux extraction at 75°C for 15 min, filter the ethanol extract, add 12 mL / g ethanol solution to the residue again, heat reflux extraction at 75°C for 10 min, filter the ethanol extract, and take the residue;

[0053] (6) adding 90% of the volume of n-hexane to the combined mixture of the filter residue and the centrifuge liquid for extraction at a temperature of 36° C. for 32 min, and recovering the extract by rotary evaporation and removing the solvent to obtain crude sea buckthorn oil;

[0054] (7) Add activated carbon in an amount of 5% by weight of the sea buckthorn oil to the crude sea buckthorn oil, stir thoroughly, let stand for 25 minutes, and then filter to remove the activated carbon. Then, add silica gel powder in an amount of 6% by weight of the sea buckthorn oil, stir thoroughly, let stand for 20 minutes, and then filter to remove the silica gel powder to obtain sea buckthorn oil.

[0055] The oil yield of seabuckthorn oil was calculated based on the quality of seabuckthorn oil and the quality of raw materials used. The oil yield of seabuckthorn oil in this embodiment was 1.24% of the quality of fresh seabuckthorn fruit. The residual solvent in the obtained seabuckthorn oil was measured by gas chromatography. The residual solvent content of seabuckthorn oil in this embodiment was 11.4ppm (<100ppm).

[0056] Example 2

[0057] This embodiment provides a method for extracting seabuckthorn oil, comprising the following steps:

[0058] (1) picking fresh seabuckthorn fruits and selecting them, removing bad fruits, then washing the seabuckthorn fruits with running water to remove dirt on the surface, drying the surface moisture of the peel, putting them into a grinder for mechanical crushing, filtering out the seabuckthorn juice, and setting aside the seabuckthorn pomace;

[0059] (2) Add water 4 times the weight of the pomace to the crushed seabuckthorn pomace and soak at 32°C for 1 h;

[0060] (3) The soaked seabuckthorn pulp is stirred evenly, and a composite enzyme is added, including 260 U / kg of protease, 500 U / kg of cellulase, and 480 U / kg of pectinase;

[0061] (4) keeping the mixture at 39° C. for 5 h for enzymatic hydrolysis, centrifuging the seabuckthorn pulp at 4500 rpm for 2 min at room temperature, and collecting the centrifuge and precipitate respectively;

[0062] (5) First add 12 mL / g (precipitate mass) of 75% ethanol solution to the centrifugal precipitate, stir to dissolve, heat and reflux at 72°C for 20 min, and filter the ethanol extract;

[0063] (6) combining the filter residue and the centrifuged liquid to obtain a mixture, adding 85% of the volume of n-hexane to the mixture for extraction, the extraction temperature is 35° C., the extraction time is 30 min, and the extract is recovered by rotary evaporation and the solvent is removed to obtain crude sea buckthorn oil;

[0064] (7) Add activated carbon in an amount of 3% by weight of the sea buckthorn oil to the crude sea buckthorn oil, stir thoroughly, let stand for 30 minutes, and then filter to remove the activated carbon. Then, add silica gel powder in an amount of 7% by weight of the sea buckthorn oil, stir thoroughly, let stand for 25 minutes, and then filter to remove the silica gel powder to obtain sea buckthorn oil.

[0065] The oil yield of seabuckthorn oil was calculated based on the quality of seabuckthorn oil and the quality of raw materials used. The oil yield of seabuckthorn oil in this embodiment was 1.16% of the quality of fresh seabuckthorn fruit. The residual solvent in the obtained seabuckthorn oil was measured by gas chromatography. The residual solvent content of seabuckthorn oil in this embodiment was 14.1ppm (<100ppm).

[0066] Comparative Example 1

[0067] The only difference from Example 1 is that the soaking treatment in step (2) is discarded, and the complex enzyme is directly added after adding water for enzymolysis. The rest is the same as Example 1.

[0068] Comparative Example 2

[0069] The only difference from Example 1 is that the addition of cellulase and pectinase in step (3) is discarded and replaced with an equal amount of protease, and the rest is the same as Example 1.

[0070] Comparative Example 3

[0071] The only difference from Example 1 is that the enzymatic hydrolysis in steps (4)-(5) is discarded and centrifugation is performed directly. The rest is the same as Example 1.

[0072] Comparative Example 4

[0073] The only difference from Example 1 is that the reflux extraction process of the ethanol solution is abandoned in step (5), and the rest is the same as Example 1.

[0074] Comparative Example 5

[0075] The only difference from Example 1 is that the n-hexane in step (7) is replaced by chloroform, and the rest is the same as Example 1.

[0076] Comparative Example 6

[0077] The only difference from Example 1 is that the activated carbon in step (8) is replaced by diatomaceous earth, and the rest is the same as Example 1.

[0078] Comparative Example 7

[0079] The only difference from Example 1 is that in step (8), the amount of activated carbon added is 10%, and the amount of silica gel powder added is 10%. The rest is the same as Example 1.

[0080] Example 3

[0081] The quality and oil yield of the sea buckthorn oil prepared in Examples 1 to 2 and Comparative Examples 1 to 7 were tested, and the main indicators of product quality standards, VE and iodine value, were used to characterize whether the effective ingredients were lost, and the plasticizer content was based on the phthalate content (DBP is dibutyl phthalate; DEHP is di(2-ethylhexyl) phthalate). The specific test results are shown in Table 1.

[0082] Table 1 Quality of sea buckthorn oil extracted from each group

[0083]

[0084]

[0085] As can be seen from Table 1, the sea buckthorn oil prepared in Examples 1 to 2 is brown-red in color, has high transparency, a high content of effective ingredients, less loss, and low contents of plasticizer and benzopyrene in the oil, and a high oil yield, indicating that the preparation method of the present invention can obtain sea buckthorn oil of good quality and a high oil yield.

[0086] Example 4

[0087] The components of the seabuckthorn oil prepared in Examples 1 and 2 were analyzed, and the main nutrients in the seabuckthorn oil, palmitic acid, palmitoleic acid, oleic acid, linoleic acid, linolenic acid and unsaturated acids were detected, and the total fat content in the seabuckthorn oil was detected. The results are shown in Table 2.

[0088] Table 2 Analysis of sea buckthorn oil components (%)

[0089]

[0090] It can be seen from Table 2 that the seabuckthorn oil prepared in Examples 1-2 has a high total fat content and contains a large amount of unsaturated fatty acids, and has a high nutritional value.

[0091] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for extracting seabuckthorn oil, characterized in that: The following steps are involved: (1) soaking seabuckthorn pomace in water, stirring evenly, adding composite enzyme to keep warm, centrifuging the enzymatic solution, and collecting the centrifuge and precipitate respectively; the composite enzyme comprises protease, cellulase and pectinase; (2) adding 75% ethanol solution to the centrifugal precipitate for heating and refluxing extraction, filtering the ethanol extract, and mixing the filter residue with the centrifugal liquid obtained in step (1) to obtain a mixture; (3) adding n-hexane to the mixture for extraction, and recovering n-hexane from the extract to obtain crude sea buckthorn oil; (4) adding activated carbon and silica gel powder to the crude seabuckthorn oil in sequence, stirring, standing, and filtering to obtain the seabuckthorn oil; In the step (1), water 2 to 5 times the mass of the pomace is added and the mixture is soaked for 1 to 3 hours at a soaking temperature of 30 to 35° C.; In the step (1), the amount of protease added is 200-300 U / kg, the amount of cellulase added is 400-600 U / kg, and the amount of pectinase added is 400-600 U / kg; The insulation time of step (1) is 4 to 6 hours, and the temperature is 37 to 39° C.; The centrifugation condition in step (1) is 3000-5000 rpm, 1-3 min; In the step (2), the heating reflux extraction temperature is 70 to 80° C. and the time is 10 to 30 minutes; In the step (3), 80-100% of the volume of the mixture is added with n-hexane for extraction, the extraction temperature is 30-40° C., and the extraction time is 25-40 min; In the step (4), the amount of activated carbon added is 2-6% of the mass of the seabuckthorn oil; the amount of silica gel powder added is 5-8% of the mass of the seabuckthorn oil.

2. Sea buckthorn oil prepared by the method according to claim 1.

3. Use of the seabuckthorn oil according to claim 2 in the preparation of health products or cleaning products.

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