Method for extracting sea cucumber oil

Abstract

The invention relates to the technical field of biological resource utilization, in particular to an extraction method of sea cucumber oil. According to the extraction method provided by the invention, by-products of sea cucumber processing are fully utilized, and the sea cucumber oil rich in sea cucumber saponin is efficiently extracted through ethanol extraction, vacuum concentration, two-aqueous-phase extraction and impurity removal, ethanol redissolution and vacuum concentration, so that nutrient substances of the sea cucumber oil are well reserved, impurities such as proteoglycan in the sea cucumber oil are effectively removed, the purity of the sea cucumber oil is improved, and the sea cucumber oil is suitable for industrial production. The health-care value of the sea cucumber oil is improved. The method is simple in process, green, economical and suitable for industrial popularization.

Description

Technical Field

[0001] The invention relates to the technical field of biological resource utilization, and in particular to a method for extracting sea cucumber oil. Background Art

[0002] Sea cucumber oil is rich in phospholipids, unsaturated fatty acids and other nutrients. In particular, sea cucumber saponins have multiple biological activities such as anti-tumor, anti-fungal, anti-viral, cytotoxic, immunomodulatory, and hemolytic activities, and have multiple beneficial effects on human health. At present, the main raw material for traditional sea cucumber oil extraction is sea cucumber. At the same time, sea cucumber flowers, which are one of the by-products of the primary processing of sea cucumbers, are often discarded or used as flower fertilizers during the processing. Studies have shown that sea cucumber flowers also contain a variety of active substances including sea cucumber saponins, which have strong application potential in delaying aging, maintaining reproductive system health, and improving cognitive ability.

[0003] At present, the technical research field of sea cucumber oil extraction is still immature. Usually, the sea cucumber oil is extracted by adding biological enzymes after high-temperature heating. However, high-temperature heating often causes some components in the sea cucumber oil to be destroyed, and the nutrients are lost, reducing the original nutritional value of the sea cucumber oil. Among them, the high-value sea cucumber saponins are easily lost during the enzymatic extraction process, resulting in a huge waste of resources.

[0004] Therefore, it is urgent to develop a sea cucumber oil extraction process that is reasonable, suitable for large-scale production, and rich in sea cucumber saponins, which will be of reference significance for the in-depth development and utilization of sea cucumber flower resources. Summary of the invention

[0005] In order to solve the above technical problems, the present invention provides a method for extracting sea cucumber oil. The method for extracting sea cucumber oil provided by the present invention has reasonable process and simple operation, can extract sea cucumber oil with high sea cucumber saponin content and high purity, improves the health value of sea cucumber oil, is green and economical, and is suitable for industrial promotion.

[0006] In a first aspect, the present invention provides a method for extracting sea cucumber oil, comprising the following steps:

[0007] (I) taking sea cucumber viscera, adding ethanol to extract sea cucumber oil, and obtaining a first mixture;

[0008] (II) separating the first mixture into solid and liquid and retaining the filtrate;

[0009] (III) concentrating the filtrate under reduced pressure to remove water and ethanol to obtain crude sea cucumber oil;

[0010] (IV) subjecting the crude sea cucumber oil to aqueous two-phase extraction to separate the oil phase;

[0011] (V) adding ethanol to the oil phase to dissolve it, thereby obtaining a second mixture;

[0012] (VI) concentrating the second mixture under reduced pressure to remove water and ethanol to obtain sea cucumber oil.

[0013] The present invention uses ethanol as the extraction solvent. On the one hand, it is because sea cucumber saponins are easily soluble in ethanol. Using ethanol extraction can increase the dissolution amount of sea cucumber saponins, which is beneficial to increasing the extraction amount of sea cucumber saponins in subsequent processes. On the other hand, it avoids the destruction of some components in the sea cucumber oil and the loss of nutrients caused by adding biological enzymes for enzymatic hydrolysis after high-temperature heating, thereby reducing the nutritional value of the sea cucumber oil. In particular, sea cucumber saponins are easily lost in the process of extracting sea cucumber oil by enzymatic hydrolysis.

[0014] The main purpose of the present invention using the two-phase aqueous extraction method is to remove impurities such as proteoglycans. After the two-phase aqueous extraction, sea cucumber oil is enriched in the upper layer. Proteoglycans and the like are mainly distributed in the middle and lower two-phase aqueous layers and can be effectively separated.

[0015] The oil phase of the sea cucumber oil after the two-phase aqueous extraction contains ethanol, water and sea cucumber oil. By adding ethanol for redissolution and then concentrating and distilling under reduced pressure again, the ethanol and water in the oil phase can be further removed to obtain purified red liquid sea cucumber oil.

[0016] In summary, the method for extracting sea cucumber oil provided by the present invention can avoid the loss of sea cucumber saponins during the extraction process of sea cucumber oil, while effectively removing impurities such as proteoglycans, extracting sea cucumber oil with high sea cucumber saponin content and high purity, thereby improving the health value of sea cucumber oil, being green and economical, and being suitable for industrial production.

[0017] In some embodiments of the present invention, the sea cucumber viscera are fresh sea cucumber viscera.

[0018] In some embodiments of the present invention, the sea cucumber viscera are sea cucumber flowers.

[0019] In some embodiments of the present invention, the extraction method further comprises: before adding ethanol in step I, cleaning the sea cucumber viscera and draining the water.

[0020] The fresh sea cucumber viscera of the present invention contains bound water itself and does not need to be processed by crushing, homogenizing and the like, and the operation is simple.

[0021] In some embodiments of the present invention, the weight ratio of sea cucumber viscera to ethanol in step I is 1:4-8, preferably 1:6-8, for example 1:6.5, 1:7, 1:7.5, etc.

[0022] In the extraction method of the present invention, if the proportion of ethanol added is too low, the sea cucumber oil will not be completely extracted; if the proportion of ethanol added is too high, the workload of filtering and recycling will be too large. The amount of ethanol added specified by the present invention can not only ensure the extraction effect of the sea cucumber oil, but also avoid the increase of the recycling cost.

[0023] In some embodiments of the present invention, in step I, stirring is performed after adding ethanol.

[0024] In some embodiments of the present invention, the stirring time is 30-90 min, for example, 40 min, 50 min, 60 min, 70 min, 80 min, etc.

[0025] In some embodiments of the present invention, the solid-liquid separation method in step II is vacuum filtration.

[0026] In some embodiments of the present invention, the air pressure of the vacuum filtration is 0.06-0.1 atmosphere, for example, 0.07 atmosphere, 0.08 atmosphere, or 0.09 atmosphere.

[0027] In some embodiments of the present invention, the vacuum filtration time is 20-40 min, such as 25 min, 30 min, 35 min, etc.

[0028] In some embodiments of the present invention, the pressure of the reduced pressure concentration in step III is 0.08-0.1 atmosphere, for example, 0.085 atmosphere, 0.09 atmosphere, 0.095 atmosphere.

[0029] In some embodiments of the present invention, the temperature for reduced pressure concentration in step III is 30-60°C, preferably 50-60°C, such as 52°C, 54°C, 56°C, 58°C, etc.

[0030] In some embodiments of the present invention, the ethanol concentrated under reduced pressure in step III is collected in a condenser and recycled in step I.

[0031] In some embodiments of the present invention, the time for the reduced pressure concentration in step III is when no more ethanol vapor is condensed into liquid ethanol in the condenser.

[0032] In some embodiments of the present invention, the extractant used in the aqueous two-phase extraction includes ethanol, sodium chloride and water.

[0033] In some embodiments of the present invention, the mass percentage of ethanol in the extractant is 50-80%, preferably 50-60%, for example 52%, 54%, 56%, 58%, etc., the mass percentage of sodium chloride is 1.5-3%, for example 1.7%, 2%, 2.3%, 2.7%, etc., and the balance is water.

[0034] The ratio of ethanol to sodium chloride content affects the extraction effect. The ratio of ethanol to sodium chloride content within the scope of the present invention has a better effect on removing impurities from sea cucumber oil.

[0035] In some embodiments of the present invention, the volume ratio of the extractant to the crude sea cucumber oil is 1:2-4, for example, 1:2, 1:3, 1:4, etc.

[0036] In some embodiments of the present invention, the time of the two-phase aqueous extraction is 1-3 h, such as 1.5 h, 2 h, 2.5 h, etc.

[0037] As the extraction time increases, the sea cucumber oil extraction rate first increases and then tends to stabilize. If the extraction time is too short, it will affect the separation effect of the crude sea cucumber oil and reduce the purity of the sea cucumber oil. If the extraction time is too long, the extraction rate of the sea cucumber oil will not increase, but will increase the time cost and reduce the extraction efficiency of the sea cucumber oil. The extraction time within the scope of the present invention can effectively remove impurities and obtain high-purity sea cucumber oil, and can also ensure a high extraction efficiency of the sea cucumber oil.

[0038] In some embodiments of the present invention, the mass ratio of the oil phase to ethanol in step V is 1:1-3, for example, 1:1.5, 1:2, 1:2.5, etc.

[0039] In some embodiments of the present invention, the pressure of the reduced pressure concentration in step VI is 0.06-0.1 atmosphere, for example, 0.07 atmosphere, 0.08 atmosphere, or 0.09 atmosphere.

[0040] In some embodiments of the present invention, the temperature for reduced pressure concentration in step VI is 30-60°C, preferably 30-40°C, such as 31°C, 33°C, 35°C, 37°C, 39°C, etc.

[0041] In some embodiments of the present invention, the ethanol concentrated under reduced pressure in step VI is collected in a condenser and recycled in step I.

[0042] In some embodiments of the present invention, the time for the reduced pressure concentration in step VI is such that no more ethanol vapor is condensed into liquid ethanol in the condenser.

[0043] The ethanol evaporated by the reduced pressure concentration in step III and step VI of the present invention can be recycled to step I for reuse, saving process costs. The time of reduced pressure concentration in step III and step VI of the present invention is not limited, as long as it is ensured that no ethanol is generated in the condenser after reduced pressure concentration.

[0044] In a second aspect, the present invention provides a sea cucumber oil extracted by the extraction method described in the first aspect, wherein the sea cucumber oil has a sea cucumber saponin content of ≥8 mg·g -1 .

[0045] The sea cucumber oil extracted by the extraction method provided by the invention has a higher relative content of sea cucumber saponins than that of sea cucumber oil extracted by high-temperature enzymatic hydrolysis under the condition of the same raw materials, thereby improving the health care effect on human body.

[0046] The technical solution provided by the embodiment of the present invention has the following advantages compared with the prior art:

[0047] The extraction method provided by the present invention makes full use of the byproducts of sea cucumber processing, can efficiently extract sea cucumber saponins, and effectively removes impurities such as proteoglycans in sea cucumber oil to obtain high-purity sea cucumber oil. The sea cucumber oil prepared by the extraction method provided by the present invention has a high content of sea cucumber saponins, better retains the nutrients of the sea cucumber oil, and improves the health value of the sea cucumber oil. The process of the present invention is reasonable, simple to operate, green and economical, improves the return on investment of the sea cucumber industry, and is conducive to large-scale promotion in industry. BRIEF DESCRIPTION OF THE DRAWINGS

[0048] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and, together with the description, serve to explain the principles of the invention.

[0049] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.

[0050] Figure 1 The present invention is a process flow chart of the method for extracting sea cucumber oil. DETAILED DESCRIPTION

[0051] In order to more clearly understand the above-mentioned objectives, features and advantages of the present invention, the scheme of the present invention will be further described below. It should be noted that the embodiments of the present invention and the features in the embodiments can be combined with each other without conflict.

[0052] In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention may also be implemented in other ways different from those described herein; it is obvious that the embodiments in the specification are only part of the embodiments of the present invention, rather than all of the embodiments.

[0053] Unless otherwise specified, the mass of the sea cucumber flowers used in the embodiments of the present invention is 1 kg per time.

[0054] Example 1

[0055] This embodiment provides a method for extracting sea cucumber oil, and the specific steps are as follows:

[0056] (I) washing and draining fresh sea cucumber flowers, adding ethanol 8 times the weight of the fresh sea cucumber flowers, stirring at room temperature for 60 minutes to extract sea cucumber oil, and obtaining a first mixture;

[0057] (II) evacuating the first mixture to 0.08 atmospheres and filtering for 40 minutes, removing the filter residue and retaining the filtrate;

[0058] (III) at 50° C., evacuating the filtrate to 0.09 atmospheres for reduced pressure concentration until no more ethanol vapor is present in the condenser and condensing into liquid ethanol to obtain crude sea cucumber oil;

[0059] (IV) subjecting the crude sea cucumber oil to an aqueous two-phase extraction using an ethanol-sodium chloride system, wherein the mass percentage of ethanol in the extractant is 50%, the mass percentage of sodium chloride is 2%, the balance is water, the volume ratio of the extractant to the crude sea cucumber oil is 0.5:1, the extraction time is 3 h, and the oil phase is separated;

[0060] (V) adding ethanol in an amount 1.5 times the mass of the oil phase to dissolve the oil phase to obtain a second mixture;

[0061] (VI) At 40° C., the second mixture is evacuated to 0.1 atmospheres for reduced pressure concentration until no ethanol vapor is left in the condenser and condensed into liquid ethanol to obtain sea cucumber oil.

[0062] Example 2

[0063] This embodiment provides a method for extracting sea cucumber oil, and the specific steps are as follows:

[0064] (I) washing and draining fresh sea cucumber flowers, adding ethanol 6 times the weight of the fresh sea cucumber flowers, stirring at room temperature for 60 minutes to extract sea cucumber oil, and obtaining a first mixture;

[0065] (II) evacuating the first mixture to 0.08 atmospheres and filtering for 40 minutes, removing the filter residue and retaining the filtrate;

[0066] (III) at 50° C., evacuating the filtrate to 0.09 atmospheres for reduced pressure concentration until no more ethanol vapor is present in the condenser and condensing into liquid ethanol to obtain crude sea cucumber oil;

[0067] (IV) subjecting the crude sea cucumber oil to an aqueous two-phase extraction using an ethanol-sodium chloride system, wherein the mass percentage of ethanol is 50%, the mass percentage of sodium chloride is 2%, the balance is water, the volume ratio of the extractant to the crude sea cucumber oil is 0.5:1, the extraction time is 3 h, and the oil phase is separated;

[0068] (V) adding ethanol in an amount 1.5 times the mass of the oil phase to dissolve the oil phase to obtain a second mixture;

[0069] (VI) At 40° C., the second mixture is evacuated to 0.1 atmospheres for reduced pressure concentration until no ethanol vapor is left in the condenser and condensed into liquid ethanol to obtain sea cucumber oil.

[0070] Example 3

[0071] This embodiment provides a method for extracting sea cucumber oil, which differs from Embodiment 1 in that the stirring time in step I is 30 minutes.

[0072] Example 4

[0073] This embodiment provides a method for extracting sea cucumber oil, which is different from Embodiment 1 in that the mass percentage of ethanol in the extractant of step IV is 60%, and the mass percentage of sodium chloride is 2%.

[0074] Example 5

[0075] This embodiment provides a method for extracting sea cucumber oil, which is different from Embodiment 1 in that the mass percentage of ethanol in the extractant of step IV is 50%, and the mass percentage of sodium chloride is 1.5%.

[0076] Example 6

[0077] This embodiment provides a method for extracting sea cucumber oil, which is different from Embodiment 1 in that the mass percentage of ethanol in the extractant of step IV is 50%, and the mass percentage of sodium chloride is 3%.

[0078] Example 7

[0079] This embodiment provides a method for extracting sea cucumber oil, which is different from Example 1 in that the time for the two-phase aqueous extraction in step IV is 2 hours.

[0080] Example 8

[0081] This embodiment provides a method for extracting sea cucumber oil, which is different from Embodiment 1 in that the mass percentage of the extractant ethanol in step IV is 40%.

[0082] Example 9

[0083] This embodiment provides a method for extracting sea cucumber oil, which is different from Embodiment 1 in that:

[0084] The mass percentage of the extractant ethanol in step IV is 85%.

[0085] Example 10

[0086] This embodiment provides a method for extracting sea cucumber oil, which is different from Embodiment 1 in that:

[0087] The mass percentage of the extractant sodium chloride in step IV is 1%.

[0088] Embodiment 11

[0089] This embodiment provides a method for extracting sea cucumber oil, which is different from Embodiment 1 in that:

[0090] The mass percentage of the extractant sodium chloride in step IV is 4%.

[0091] Comparative Example 1

[0092] This comparative example provides a method for extracting sea cucumber oil, and the specific steps are as follows:

[0093] (I) taking fresh sea cucumber flowers, washing them, and heating them at 90° C. for 30 min;

[0094] (II) cooling to 55°C and adding biological enzymes for enzymatic hydrolysis;

[0095] (III) evacuating the enzymatic hydrolyzate to 0.08 atmospheres and filtering for 40 minutes, removing the filter residue and retaining the filtrate;

[0096] (III) At 50° C., the filtrate is evacuated to 0.09 atmospheres for reduced pressure concentration to obtain sea cucumber oil.

[0097] Comparative Example 2

[0098] This comparative example provides a method for extracting sea cucumber oil, which differs from Example 1 in that the two-aqueous phase extraction in step IV is not performed.

[0099] Detection of sea cucumber oil ingredients

[0100] The test results of the extraction amount and purity of the sea cucumber oil prepared in the embodiment and the comparative example and the sea cucumber saponin content are shown in Table 1.

[0101] Table 1. Extraction amount and purity of prepared sea cucumber oil and sea cucumber saponin content

[0102]

[0103]

[0104] From the comparison between Examples 1-7 and Comparative Example 1, it can be seen that the sea cucumber oil prepared by the sea cucumber oil extraction method provided by the present invention avoids the destruction of sea cucumber saponins by biological enzymes compared to the high-temperature enzymatic extraction method, and the content of sea cucumber saponins is significantly improved.

[0105] From the comparison between Example 1 and Comparative Example 2, it can be seen that the sea cucumber oil prepared by the sea cucumber oil extraction method provided by the present invention can significantly reduce the proteoglycan content in the sea cucumber oil through the two-phase aqueous extraction step, and the purity of the sea cucumber oil is significantly improved.

[0106] From the comparison between Example 1 and Examples 8-11, it can be seen that the ratio of ethanol and sodium chloride in the two-phase extraction system in the sea cucumber oil extraction method provided by the present invention is maintained within the range specified by the present invention, which can improve the removal rate of impurities such as proteoglycans and improve the purity of sea cucumber oil while ensuring the extraction amount of sea cucumber oil.

[0107] In summary, the method for extracting sea cucumber oil provided by the present invention can prepare high-purity sea cucumber oil with a high sea cucumber content, and the overall process is simple, green and economical, which is conducive to improving the return on investment of the sea cucumber industry.

[0108] It should be noted that, in this article, relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0109] The above description is only a specific embodiment of the present invention, so that those skilled in the art can understand or implement the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments described herein, but should conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for extracting sea cucumber oil, characterized in that: The following steps are involved: (I) taking sea cucumber viscera, adding ethanol to extract sea cucumber oil, and obtaining a first mixture; (II) separating the first mixture into solid and liquid and retaining the filtrate; (III) concentrating the filtrate under reduced pressure to remove water and ethanol to obtain crude sea cucumber oil; (IV) subjecting the crude sea cucumber oil to aqueous two-phase extraction to separate the oil phase; (V) adding ethanol to the oil phase to dissolve it, thereby obtaining a second mixture; (VI) concentrating the second mixture under reduced pressure to remove water and ethanol to obtain sea cucumber oil.

2. The extraction method according to claim 1, characterized in that The sea cucumber viscera are fresh sea cucumber viscera; Preferably, the sea cucumber viscera is sea cucumber flower; Preferably, the extraction method further comprises: before adding ethanol in step I, cleaning the sea cucumber viscera and draining the water.

3. The extraction method according to claim 1 or 2, characterized in that The weight ratio of sea cucumber viscera to ethanol in step I is 1:4-8, preferably 1:6-8; Preferably, in step I, stirring is performed after adding ethanol; Preferably, the stirring time is 30-90 min.

4. The extraction method according to any one of claims 1 to 3, characterized in that The solid-liquid separation method in step II is vacuum filtration; Preferably, the air pressure of the vacuum filtration is 0.06-0.1 atmosphere; Preferably, the vacuum filtration time is 20-40 min.

5. The extraction method according to any one of claims 1 to 4, characterized in that The pressure of the reduced pressure concentration in step III is 0.08-0.1 atmosphere; Preferably, the temperature of reduced pressure concentration in step III is 30-60°C, preferably 50-60°C.

6. The extraction method according to any one of claims 1 to 5, characterized in that The extractant used in the two-phase aqueous extraction includes ethanol, sodium chloride and water; Preferably, the mass percentage of ethanol in the extractant is 50-80%, preferably 50-60%, the mass percentage of sodium chloride is 1.5-3%, and the balance is water.

7. The extraction method according to any one of claims 1 to 6, characterized in that The volume ratio of the extractant to the crude sea cucumber oil is 1:2-4; Preferably, the aqueous two-phase extraction time is 1-3 h.

8. The extraction method according to any one of claims 1 to 7, characterized in that In the step V, the mass ratio of the oil phase to the ethanol is 1:1-3.

9. The extraction method according to any one of claims 1 to 8, characterized in that The pressure of the reduced pressure concentration in step VI is 0.06-0.1 atmosphere; Preferably, the temperature of the reduced pressure concentration in step VI is 30-60°C, preferably 30-40°C.

10. A sea cucumber oil prepared by the extraction method according to any one of claims 1 to 9, characterized in that: The sea cucumber oil has a sea cucumber saponin content of ≥8 mg·g -1 .

Images