Method for separating ceramide from hydration degumming byproduct

Abstract

The invention discloses a method for separating ceramide from a hydration degumming byproduct, which comprises the following steps: (1) adding an organic solvent into the hydration degumming byproduct containing ceramide, extracting, separating and concentrating an organic phase to obtain a concentrated solution; (2) adding water into the concentrated solution, extracting and separating, and concentrating a water phase to obtain a ceramide product; the organic solvent in the step (1) is any one or more of diethyl ether, dichloromethane and trichloromethane; the content of solid matters in the concentrated solution is 20%-40%. The content of ceramide separated by the method can reach 9.5% or above, efficient conversion of byproducts is achieved, and the comprehensive utilization rate of resources is greatly increased.

Description

Technical Field

[0001] The invention relates to a method for separating ceramide from hydration degumming by-products. Background Art

[0002] As a bioactive substance with important physiological functions, ceramide has attracted wide attention and been studied in depth in recent years. In the field of dermatology, it plays a key role in maintaining the skin barrier function. It can enhance the skin's moisturizing ability, prevent water loss, resist the invasion of harmful substances from the outside world, and help the skin stay healthy, smooth and elastic. The market demand for skin care products containing ceramide continues to rise. In the medical field, ceramide can regulate cell growth, differentiation and apoptosis, and has potential therapeutic value for certain skin diseases, nervous system diseases and cancer. In the food field, it also has health care functions, such as regulating intestinal flora and enhancing immunity.

[0003] At present, the preparation methods of ceramide mainly include natural extraction, chemical synthesis and microbial fermentation. The natural extraction method generally obtains ceramide from animal tissues or plants, but there are problems such as limited sources, low yields, high costs, and possible risks of animal-borne diseases. Although the chemical synthesis method can produce ceramide on a large scale, toxic and harmful chemical reagents may be used in the synthesis process, which poses potential hazards to the environment and human health. The microbial fermentation method is relatively environmentally friendly and the product safety is relatively high, but the fermentation process control is more complicated, and the separation and purification of the product is also difficult.

[0004] In the oil processing process, hydration degumming will produce by-products. In the past, these by-products were often regarded as waste and were not fully utilized. With the continuous advancement of technology and the increasing emphasis on comprehensive resource utilization, people have begun to explore the separation and purification of high-value substances from hydration degumming by-products. Ceramide may contain a certain amount of ceramide in the by-products of hydration degumming. If ceramide can be effectively separated and purified from these by-products, it can not only achieve high-value utilization of by-products and improve the comprehensive utilization rate of resources, but also open up a new way for the production of ceramide. Summary of the invention

[0005] The present invention aims to provide a method for separating ceramide from hydration degumming by-products, wherein the ceramide content can reach more than 9.5%, thereby achieving efficient conversion of the by-products and greatly improving the comprehensive utilization rate of resources.

[0006] To achieve the above purpose, the technical solution of the present invention is as follows: A method for separating ceramide from hydration degumming by-products comprises the following steps: (1) adding an organic solvent to the hydrated degumming byproduct containing ceramide, extracting and separating, and concentrating the organic phase to obtain a concentrated solution; (2) adding water to the concentrated solution, extracting and separating, and concentrating the aqueous phase to obtain a ceramide product.

[0007] Furthermore, the raw material sources of the hydration degumming by-products of the present invention include but are not limited to soybeans, rice bran, camellia seeds, and peppers.

[0008] Furthermore, the organic solvent in step (1) of the present invention is one or more of diethyl ether, dichloromethane and chloroform.

[0009] Furthermore, in step (1) of the present invention, the volume ratio of the hydrated degumming byproduct to the organic solvent is 1:1-20.

[0010] Furthermore, the solid content of the concentrated solution in step (1) of the present invention is 20%-40%.

[0011] Furthermore, in step (2) of the present invention, the volume ratio of the concentrate to water is 1:1-5.

[0012] Furthermore, in step (1) and step (2) of the present invention, the extraction temperature is 20 to 40° C., and the extraction time is 0.5 to 1 h.

[0013] Furthermore, in the present invention, the concentration temperature in step (1) is 20°C-30°C; and the concentration temperature in step (2) is 60°C-70°C.

[0014] The beneficial technical effects of the technical solution of the present invention are: The present invention can realize the separation of ceramide by bidirectionally controlling the extraction and separation solvents, the solid content in the concentrated solution, etc. The content of the separated ceramide is greater than 9.5%, and the yield is greater than 50%.

[0015] Compared with other solutions in the prior art, the method of the present invention has short steps, low cost, and is suitable for industrial large-scale production. In addition, the method of the present invention realizes efficient conversion of by-products, greatly improving the comprehensive utilization rate of resources. DETAILED DESCRIPTION

[0016] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0017] The content of ceramide in the present invention is detected by high performance liquid chromatography tandem time-of-flight mass spectrometry as follows: mobile phase: phase A is 1% formic acid-water solution, phase B is 1% formic acid-50% acetonitrile-50% isopropanol, and gradient elution is used for analysis (gradient elution conditions are shown in Table 1); control flow rate during elution: 0.2 mL / min; column temperature: 40°C; chromatographic column: BEH C18 column (2.1 mm×150 mm, particle size 1.7 μm); injection volume: 2.0 μL. The retention time of the ceramide component appears at 70-85.5 min.

[0018] Table 1 Gradient elution conditions during ceramide content detection

[0019] The content of the ceramide in the present invention is measured using commercially available natural plant-derived ceramide (Shaanxi Yihaochuan Biotechnology Co., Ltd., ceramide content 5%) as a reference substance. Example 1

[0020] 1) Take 10 L of hydrated degumming byproduct containing ceramide, the raw material of the hydrated degumming byproduct is derived from pepper, the mass concentration of solids in the byproduct is 50 g / L, and the mass percentage of ceramide in the solids is 4.8%. Add 50 L of dichloromethane to the byproduct, stir and extract for 1 hour, and let it stand for 2 hours.

[0021] 2) Collect the dichloromethane phase and concentrate it at 25°C to a solid content of 30% to obtain 1 kg of concentrated solution.

[0022] 3) Add 3 L of pure water to the above concentrate, stir and extract for 1 hour, collect the aqueous phase by centrifugation, and concentrate at 65°C to obtain 0.161 kg of ceramide product.

[0023] After testing, the content of ceramide in the ceramide product obtained in this embodiment is 11.2%; after calculation, it can be known that the ceramide extraction rate of this embodiment is 75.1%. Example 2

[0024] Compared with Example 1, the difference is that the amount of dichloromethane added in step 1) is 10 L, and the other operations are the same as Example 1.

[0025] In this example, 0.106 kg of ceramide product was obtained; after testing, the ceramide content in the obtained ceramide product was 12.9%. According to calculation, the ceramide extraction rate in this example was 56.8%. Example 3

[0026] Compared with Example 1, the difference is that the amount of dichloromethane added in step 1) is 200 L, and the other operations are the same as Example 1.

[0027] In this example, 0.185 kg of ceramide product was obtained; after testing, the ceramide content in the obtained ceramide product was 10.5%. According to calculation, the ceramide extraction rate in this example was 80.9%. Example 4

[0028] Compared with Example 1, the difference is that the solid content of the concentrated solution in step 2) is 20%, and the other operations are the same as those in Example 1.

[0029] In this example, 0.131 kg of ceramide product was obtained; after testing, the content of ceramide in the obtained ceramide product was 12.2%. According to calculation, the ceramide extraction rate in this example was 66.5%. Example 5

[0030] Compared with Example 1, the difference is that the solid content of the concentrated solution in step 2) is 40%, and the other operations are the same as those in Example 1.

[0031] In this example, 0.189 kg of ceramide product was obtained; after testing, the ceramide content in the obtained ceramide product was 10.1%. According to calculation, the ceramide extraction rate in this example was 79.7%. Example 6

[0032] Compared with Example 1, the difference is that chloroform is added in step 1), and the other operations are the same as those in Example 1.

[0033] In this example, 0.155 kg of ceramide product was obtained; after testing, the content of ceramide in the obtained ceramide product was 11.5%. According to calculation, the ceramide extraction rate in this example was 74.1%. Example 7

[0034] Compared with Example 1, the difference is that anhydrous ether is added in step 1), and the other operations are the same as those in Example 1.

[0035] In this example, 0.128 kg of ceramide product was obtained; after testing, the content of ceramide in the obtained ceramide product was 9.5%. According to calculation, the ceramide extraction rate in this example was 50.7%. Example 8

[0036] Compared with Example 1, the difference is that 1 L of pure water is added in step 3), and the other operations are the same as those in Example 1.

[0037] In this example, 0.132 kg of ceramide product was obtained; after testing, the ceramide content in the obtained ceramide product was 11.9%. According to calculation, the ceramide extraction rate in this example was 65.4%. Example 9

[0038] Compared with Example 1, the difference is that 5 L of pure water is added in step 3), and the other operations are the same as those in Example 1.

[0039] In this example, 0.197 kg of ceramide product was obtained; after testing, the content of ceramide in the obtained ceramide product was 9.8%. According to calculation, the ceramide extraction rate in this example was 80.3%.

[0040] Comparative Example 1 Compared with Example 1, the difference is that n-hexane is added in step 1), and the other operations are the same as those in Example 1.

[0041] The comparative example obtained 0.033 kg of ceramide product; after testing, the ceramide content in the obtained ceramide product was 9.7%. After calculation, it can be known that the ceramide extraction rate of the comparative example is 13.2%.

[0042] Comparative Example 2 Compared with Example 1, the difference is that ethyl acetate is added in step 1), and the other operations are the same as those in Example 1.

[0043] The comparative example obtained 0.056 kg of ceramide product; after testing, the ceramide content in the obtained ceramide product was 8.8%. After calculation, it can be known that the ceramide extraction rate of the comparative example is 20.7%.

[0044] Comparative Example 3 Compared with Example 1, the difference is that n-butanol is added in step 1), and the other operations are the same as those in Example 1.

[0045] The comparative example obtained 0.048 kg of ceramide product; after testing, the ceramide content in the obtained ceramide product was 5.2%. After calculation, it can be known that the ceramide extraction rate of the comparative example is 10.3%.

[0046] Comparative Example 4 Compared with Example 1, the difference is that the solid content of the concentrated solution in step 2) is 5%, and the other operations are the same as those in Example 1.

[0047] The comparative example obtained 0.103 kg of ceramide product; after testing, the ceramide content in the obtained ceramide product was 11.5%. After calculation, it can be known that the ceramide extraction rate of the comparative example is 49.5%.

[0048] Comparative Example 5 Compared with Example 1, the difference is that the solid content of the concentrated solution in step 2) is 90%, and the other operations are the same as those in Example 1.

[0049] The comparative example obtained 0.307 kg of ceramide product; after testing, the ceramide content in the obtained ceramide product was 6.7%. After calculation, it can be known that the ceramide extraction rate of the comparative example is 85.8%.

[0050] Comparative Example 6 Compared with Example 1, the difference is that the volume ratio of the concentrate to water in step (2) is 1:20, and the other operations are the same as those in Example 1.

[0051] The comparative example obtained 0.321 kg of ceramide product; after testing, the ceramide content in the obtained ceramide product was 6.1%. After calculation, it can be known that the ceramide extraction rate of the comparative example is 81.5%.

[0052] Comparative Example 7 1) Take 10 L of hydrated degumming byproduct containing ceramide, the mass concentration of solid in the byproduct is 50 g / L, add 50 L of dichloromethane, stir and extract for 1 hour, and let it stand for 2 hours.

[0053] 2) Collect the dichloromethane phase and concentrate at 25°C to obtain ceramide.

[0054] The comparative example obtained 0.530 kg of ceramide product; after testing, the ceramide content in the obtained ceramide product was 4.3%. After calculation, it can be known that the ceramide extraction rate of the comparative example is 94.9%.

[0055] It can be seen from the above embodiments and comparative examples that the method of the present invention can well separate the ceramide component in the by-product of hydration degumming. If the method of the present invention is not used, such as using n-hexane, ethyl acetate, and n-butanol for extraction in Comparative Examples 1-3, the yield and purity of ceramide are significantly reduced; the solid content of the concentrate in Comparative Example 4 is 5%, and the yield of ceramide is significantly reduced; the solid content of the concentrate in Comparative Example 5 is 90%, the volume ratio of the concentrate to water in Comparative Example 6 is 1:20, and no water is added for extraction and separation in Comparative Example 7, and the purity of the obtained ceramide is significantly reduced. It shows that the technical solution provided by the present invention has outstanding technical effects.

[0056] The above is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily thought of by a person skilled in the art within the technical scope disclosed by the present invention should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the claims.

Claims

1. A method for separating ceramide from hydration degumming by-products, characterized in that: The following steps are involved: (1) adding an organic solvent to the hydrated degumming byproduct containing ceramide, extracting and separating, and concentrating the organic phase to obtain a concentrated solution; (2) adding water to the concentrated solution, extracting and separating, and concentrating the aqueous phase to obtain a ceramide product.

2. A method for separating ceramide from hydration degumming by-products according to claim 1, characterized in that: The raw material sources of the hydration degumming by-products include but are not limited to soybeans, rice bran, camellia seeds, and peppers.

3. The method for separating ceramide from hydration degumming byproducts according to claim 1, characterized in that: The organic solvent in step (1) is one or more of ether, dichloromethane and chloroform.

4. The method for separating ceramide from hydration degumming byproducts according to claim 1, characterized in that: In step (1), the volume ratio of the hydrated degumming byproduct to the organic solvent is 1:1-20.

5. The method for separating ceramide from hydration degumming byproducts according to claim 1, characterized in that: The solid content of the concentrated solution in step (1) is 20%-40%.

6. The method for separating ceramide from hydration degumming byproducts according to claim 1, characterized in that: The volume ratio of the concentrate to water in step (2) is 1:1-5.

7. The method for separating ceramide from hydration degumming byproducts according to claim 1, characterized in that: The extraction temperature in step (1) and step (2) is 20-40° C., and the extraction time is 0.5-1 h.

8. The method for separating ceramide from hydration degumming byproducts according to claim 1, characterized in that: The concentration temperature in step (1) is 20°C-30°C.

9. The method for separating ceramide from hydration degumming byproducts according to claim 1, characterized in that: The concentration temperature in step (2) is 60°C-70°C.

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