A green deodorization method suitable for ultra-micro sea cucumber powder

By improving the gas distributor and ultra-micro physical crushing technology of the supercritical fluid extractor, the problem of fishy smell in ultra-micro sea cucumber powder was solved, achieving efficient deodorization and high-quality production, while avoiding pipeline blockage and loss of nutritional value.

CN119655407BActive Publication Date: 2025-11-04DALIAN POLYTECHNIC UNIVERSITY +1
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Patent Information

Application Number
CN202411662708.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-11-20
Publication Date
2025-11-04
Estimated Expiration
2044-11-20

AI Technical Summary

Technical Problem

The fishy smell of ultrafine sea cucumber powder intensifies after grinding, affecting its flavor and quality. Traditional deodorization methods can reduce nutritional value or cause pipeline blockage, which is difficult to solve effectively with existing technology.

Method used

The gas distributor of the supercritical fluid extractor was improved by adding a second orifice plate design and combining it with ultra-micro physical fragmentation technology to perform carbon dioxide extraction and secondary extraction, thereby reducing the risk of odorous substances being carried out and clogging.

Benefits of technology

It achieves efficient deodorization of ultrafine sea cucumber powder, simplifies the operation process, maintains high product quality, requires no additives, and is suitable for industrial production.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a kind of green deodorization methods suitable for supermicro sea cucumber powder, belong to the field of food processing.The method includes the following steps: S1, sea cucumber coarse powder is placed in the extraction kettle of supercritical extraction instrument, and the deodorization of sea cucumber powder is carried out using;S2, the sea cucumber powder of deodorization in step S1 is crushed using supermicro grinder, and sea cucumber powder body is obtained, the bulk density of powder body is controlled to be 0.65~0.7g / mL, and the tap density is 0.70~0.80g / mL;S3, the sea cucumber powder after supermicro crushing in step S2 is placed in the extraction kettle of supercritical extraction instrument and is deodorized.The second hole disc is added on the gas distributor in the supercritical extraction instrument in the application, so that carbon dioxide fluid backflow is extracted, the pressure when carbon dioxide fluid is discharged from material basket is slowed down, the material is prevented from being taken out, so that the pipeline blockage problem of supermicro powder is solved, and the extraction efficiency and production efficiency are improved.
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Description

TECHNICAL FIELD

[0001] The present application relates to a green deodorization method suitable for ultra-micro sea cucumber powder, belonging to the field of food processing. BACKGROUND

[0002] Sea cucumber belongs to Echinodermata and Holothuroidea, has the characteristics of high protein, low fat and low cholesterol, and is rich in various trace elements and polyunsaturated fatty acids and other active substances, and has very high nutritional value. However, sea cucumber has the phenomenon of autolysis, which significantly increases the difficulty of fresh sea cucumber in transportation and preservation. Therefore, in order to prevent the occurrence of autolysis of sea cucumber, most sea cucumbers need to be processed after being harvested. Among them, powder products have the advantages of fast absorption, convenient eating and easy storage, so sea cucumber is often processed into powder products. In sea cucumber powder products, ultra-micro sea cucumber powder has greatly improved powder fineness, which is more beneficial to the human body to absorb active ingredients and nutritional ingredients in sea cucumber powder after eating, so it has better market prospects and research and development value.

[0003] However, due to the influence of the living environment of sea cucumber, the body wall of sea cucumber itself has a fishy smell, and the crushing process during the processing of sea cucumber powder will increase the specific surface area of the powder, thereby causing the sea cucumber powder to have a heavier fishy smell, affecting the flavor and quality of the finished sea cucumber powder product. Moreover, this situation will be further aggravated when preparing ultra-micro sea cucumber powder, because the specific surface area of the powder is increased more, which ultimately affects the market prospects of ultra-micro sea cucumber powder.

[0004] At present, for the deodorization of sea cucumber powder, the traditional methods are flavor masking and molecular embedding deodorization technology. Flavor masking is to mask the fishy smell of sea cucumber products by adding flavorings, and molecular embedding deodorization technology is to embed sea cucumber powder with wall materials to mask the fishy smell. However, these two methods have the following problems: first, they increase the use of auxiliary materials, which reduces the nutritional value of sea cucumber powder products; second, they are more suitable for deodorization of conventional sea cucumber powder (10-20 mesh), and the deodorization effect of ultra-micro sea cucumber powder (100 mesh or more) is poor.

[0005] There are other methods for deodorizing sea cucumber powder in the prior art. For example, Chinese patent CN 115918770 A (Preparation method of marine biological health-care peptide preparation) uses biological enzymatic hydrolysis method, which converts small molecule fishy smell substances into large molecule substances without fishy smell through the metabolic action of microorganisms, but this method is still relatively complex, and the metabolic action is difficult to control, making it difficult to ensure the quality of industrial production.

[0006] As used in Chinese Patent CN 116491632 A (Preparation method of low-smell and low-salt sea cucumber powder), endogenous enzyme moderate regulation treatment, supercritical carbon dioxide extraction separation and other means are used to prepare a low-smell and low-salt sea cucumber powder. The scheme has many steps and the operation is complex, and the method is still aimed at the deodorization of ordinary sea cucumber powder, wherein a conventional supercritical extractor is used, and the gas distributor thereof is not improved, which may cause pipe blockage during subsequent processing of the ultrafine sea cucumber powder, affecting production. The problem of pipe blockage of fine powder is also mentioned in the last paragraph on the left column on page 49 of "Supercritical extraction of sea cucumber cerebrosides and HPLC detection and analysis", which is "Too fine material can also cause the blockage of the sintering plate in the extraction kettle and the pipe under high pressure, which will be detrimental to the extraction of … …".

[0007] Therefore, it is necessary to explore how to achieve simple and effective deodorization of ultrafine sea cucumber powder without adding auxiliary materials. SUMMARY

[0008] TECHNICAL PROBLEM

[0009] Sea cucumber powder produces a fishy smell after being crushed, and the fishy smell of ultrafine sea cucumber powder is particularly serious, which affects its flavor and quality and hinders the market application of ultrafine sea cucumber powder. The traditional deodorization method reduces the nutritional value of sea cucumber powder by using auxiliary materials; the enzymatic method is complex and difficult to control; and the use of conventional supercritical extractors for deodorization may cause pipe blockage. Therefore, it is necessary to provide a method for simply and effectively deodorizing ultrafine sea cucumber powder without adding auxiliary materials.

[0010] TECHNICAL CONTENT

[0011] The purpose of the present application is to solve the problem of increased fishy smell of sea cucumber powder after being crushed, and to provide a deodorization method suitable for ultrafine sea cucumber powder. The present application improves the gas distributor in the supercritical extractor and combines physical ultrafine physical crushing technology to develop a high-quality ultrafine sea cucumber powder product.

[0012] In order to achieve the above purpose, the present application provides a method for deodorizing ultrafine sea cucumber powder, comprising the following steps:

[0013] S1, placing sea cucumber coarse powder in the extraction kettle of a supercritical extractor for supercritical carbon dioxide extraction to deodorize the sea cucumber powder;

[0014] S2, crushing the sea cucumber powder deodorized in step S1 using an ultrafine crusher to obtain sea cucumber powder, controlling the bulk density of the sea cucumber powder to be 0.65-0.7 g / mL, and the tap density to be 0.70-0.80 g / mL;

[0015] S3, placing the sea cucumber powder after step S2 through ultrafine pulverization in the extraction kettle of the supercritical extraction instrument to perform supercritical carbon dioxide extraction, finally completing the deodorization of the ultrafine sea cucumber powder.

[0016] Further, the sea cucumber coarse powder in step S1 is a sea cucumber coarse powder of 5-20 meshes.

[0017] Further, the sea cucumber coarse powder is prepared by the following method:

[0018] Fresh sea cucumber is placed in warm water at 50-60℃ for temporary cultivation for 4-8h, the temporarily cultivated sea cucumber is opened at the abdomen, the contents in the body cavity of the sea cucumber are removed, and the body wall of the sea cucumber is washed with water, then the sea cucumber is dried by a vacuum freeze-drying machine for 20-24h, and finally the sea cucumber dry product is crushed into a sea cucumber coarse powder of 5-20 meshes in a pulverizer.

[0019] Further, the parameters of the extraction kettle of the supercritical extraction instrument in step S1 are set to 30-40℃, the extraction pressure is 25-30MPa, the CO2 flow is 25-30L / h, and the extraction time is 2-2.5h.

[0020] Further, pre-cooling is performed before pulverization in step S2 using an ultrafine pulverizer; the pre-cooling is pre-cooling using dry ice, liquid nitrogen, or pre-cooling by standing in a frozen environment; the pre-cooling temperature is below-20℃.

[0021] Further, the pulverization in step S2 using an ultrafine pulverizer is performed at a rotational speed of 8000-12000rpm with a 0.3-0.6mm aperture screen.

[0022] Further, the parameters of the extraction kettle of the supercritical extraction instrument in step S3 are set to 30-40℃, the extraction pressure is 25-30MPa, the CO2 flow is 25-30L / h, and the extraction time is 2-2.5h.

[0023] Further, the supercritical extraction instrument in step S1 and step S3 is a supercritical extraction instrument equipped with a gas disperser.

[0024] Further, the gas disperser in the supercritical extraction instrument is an improved gas disperser.

[0025] Further, the improved gas disperser comprises a mounting pipe (1), a connecting flange (2), a first hole disc (3), a filter screen (4), a support column (5), a baffle (6), a telescopic rod (7), a spring (70), a pressing plate (8), and a second hole disc (9).

[0026] Wherein, the installation pipe (1) is transparent material, facilitate observation inside situation, installation pipe (1) upper and lower two department outside are connected with the connecting flange (2), facilitate external pipeline, installation pipe (1) middle inside and lower inside are connected with the first hole disc (3), the first hole disc (3) downside are connected with filter screen (4), the first hole disc (3) between connection has four support columns (5), support column (5) upside are connected with baffle (6), baffle (6) all with installation pipe (1) contact, baffle (6) all are connected with telescopic rod (7), telescopic rod (7) fixed end and telescopic end between all are connected with spring (70), telescopic rod (7) telescopic end all are rotatably connected with pressure plate (8), baffle (6) between the placement has second hole disc (9), pressure plate (8) all with second hole disc (9) contact cooperation, the shape of first hole disc (3) and second hole disc (9) is same, second hole disc (9) upside is equipped with twelve conical parts, facilitate backflow.

[0027] The beneficial effects of the present application are:

[0028] 1、The gas distributor of conventional supercritical extraction instrument lacks the design of the second hole disc, which will carry out the material from the material basket when extracting some relatively delicate materials, blow into the carbon dioxide pipeline, cause the blockage of the carbon dioxide pipeline, and cannot normally complete the extraction. Therefore, the second hole disc is added to the gas distributor, so that the carbon dioxide fluid backflows, slows down the pressure when the carbon dioxide fluid is discharged from the material basket, prevents the carrying out of the material, thereby solving the problem of pipeline blockage of super-fine powder; at the same time, the backflow of the carbon dioxide fluid can also carry out secondary extraction, thereby improving the extraction efficiency and production efficiency.

[0029] 2、The supercritical extraction instrument equipped with the improved gas distributor is used to extract the superfine sea cucumber powder, realizes the deodorization of the superfine sea cucumber powder, the whole process is simple and easy to operate, does not involve complex processes such as enzymolysis, and is particularly suitable for process production; and the prepared superfine sea cucumber powder has greatly reduced fishy smell and high food quality, and has great market value. BRIEF DESCRIPTION OF DRAWINGS

[0030] Figure 1 It is a schematic diagram of the improved gas distributor; wherein, 1, installation pipe, 2, connecting flange, 5, support column, 7, telescopic rod, 8, pressure plate, 9, second hole disc;

[0031] Figure 2 It is a schematic diagram of the improved gas distributor; wherein, 1, installation pipe, 2, connecting flange, 3, first hole disc, 4, filter screen, 5, support column, 6, baffle, 7, telescopic rod, 8, pressure plate, 9, second hole disc;

[0032] Figure 3Figure 6 is a schematic view of the improved gas distributor in a perspective view from A in Figure 5; wherein 1, mounting tube, 5, support column, 6, baffle, 7, telescopic rod, 70, spring, 8, pressing plate, 9, second hole disc;

[0033] Figure 4 Figure 7 is a supercritical extraction device installed with the gas distributor, wherein the red arrow is the installation position of the gas distributor;

[0034] Figure 5 Figure 8 is a GC-IMS two-dimensional difference topography of Example 1;

[0035] Figure 6 Figure 9 is a GC-IMS two-dimensional difference topography of Comparative Example 1;

[0036] Figure 7 Figure 10 is a GC-IMS two-dimensional difference topography of Comparative Example 2;

[0037] Figure 8 Figure 11 is the content of different kinds of volatile substances of Example 1, Comparative Example 1 and Comparative Example 2 (different letters indicate significance);

[0038] Figure 9 Figure 12 is the content of key volatile substances of Example 1, Comparative Example 1 and Comparative Example 2 (different letters indicate significance). DETAILED DESCRIPTION

[0039] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the scope of protection of the present application.

[0040] In the present application, unless otherwise explicitly specified and limited, the terms "connected", "connected", "fixed" should be understood broadly, for example, can be fixedly connected, or can be detachably connected, or integrated; can be mechanically connected, or electrically connected; can be directly connected, or indirectly connected through an intermediate medium, can be the internal communication of two elements or the interaction relationship between two elements. For those of ordinary skill in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0041] In the present application, unless otherwise explicitly specified and limited, the first feature is "on" or "under" the second feature can include that the first and second features are in direct contact, or can include that the first and second features are not in direct contact but are in contact through another feature between them. Moreover, the first feature is "on", "above" and "over" the second feature includes that the first feature is directly above and obliquely above the second feature, or only indicates that the first feature is higher in horizontal height than the second feature. The first feature is "under", "below" and "underneath" the second feature includes that the first feature is directly below and obliquely below the second feature, or only indicates that the first feature is lower in horizontal height than the second feature.

[0042] Experimental apparatus

[0043] The supercritical extraction instrument with improved gas distributor used in the examples and comparative examples is produced by Jiangsu Gaokeli Pharmaceutical Equipment Co., Ltd., and the model is GKSCFE220-40-30L. Among them, the gas distributor of the supercritical extraction instrument is improved, and the improved gas distributor is shown in Figures 1-3 .

[0044] The improved gas distributor includes a mounting pipe 1, a connecting flange 2, a first hole disc 3, a filter screen 4, a support column 5, a baffle 6, an extension rod 7, a spring 70, a pressing plate 8 and a second hole disc 9.

[0045] The mounting pipe 1 is of transparent material, facilitating observation of the internal situation. The upper and lower outer sides of the mounting pipe 1 are connected with the connecting flanges 2, facilitating external connection of pipes. The inner sides of the middle and lower parts of the mounting pipe 1 are connected with the first hole discs 3. The lower sides of the first hole discs 3 are connected with the filter screens 4. Four support columns 5 are connected between the first hole discs 3. The upper sides of the support columns 5 are connected with the baffles 6, which are in contact with the mounting pipe 1. The extension rods 7 are connected with the baffles 6. The springs 70 are connected between the fixed ends and the extension ends of the extension rods 7. The extension ends of the extension rods 7 are rotatably connected with the pressing plates 8. The second hole disc 9 is placed between the baffles 6. The pressing plates 8 are in contact with the second hole disc 9. The first hole disc 3 and the second hole disc 9 are of the same shape. Twelve conical pieces are arranged on the upper side of the second hole disc 9, facilitating reflux.

[0046] When the supercritical carbon dioxide extraction is carried out, the improved gas distributor is used to drive the place where the extracted ingredients are needed, the connecting flange 2 at the lower part of the installation pipe 1 is connected with the feeding pipe, the installation pipe 1 is made of transparent material, which is convenient for observing the internal situation, then the pressing plate 8 is pulled to move and rotate, so that the telescopic rod 7 is elongated, the spring 70 is stretched, then the second hole disc 9 is in contact with the baffle 6, then the pressing plate 8 is reset by reverse rotation, then the spring 70 rebounds, the telescopic rod 7 is retracted and restored, so that the pressing plate 8 is in contact with the second hole disc 9, thereby the second hole disc 9 can be fixed, preventing the second hole disc 9 from falling due to the flow of carbon dioxide fluid, then the upper connecting flange 2 is connected with the feeding port of the extraction tank, the carbon dioxide fluid is added into the feeding pipe, so that the carbon dioxide fluid enters the installation pipe 1, flows through the first hole disc 3, the filter screen 4 and the second hole disc 9, and then flows into the extraction tank to extract the material, the first hole disc 3 and the second hole disc 9 are the same shape, thereby the carbon dioxide fluid can be uniformly fed, the extraction efficiency and production efficiency are improved, meanwhile the device can be placed in the extraction tank, the carbon dioxide can achieve the effect of reflux under the action of the conical part, so that the carbon dioxide fluid is refluxed under the action of the conical part on the second hole disc 9, secondary extraction is carried out, the material is conveniently extracted twice, the pressure when the carbon dioxide fluid is discharged from the material basket is reduced, the material is prevented from being taken out, and the extraction effect is improved.

[0047] Example 1

[0048] S1, physical crushing of sea cucumber powder: fresh sea cucumber is placed in warm water at 60°C for temporary cultivation for 6h, the sea cucumber is opened at the abdomen, the contents in the body cavity of the sea cucumber are removed, and the body wall of the sea cucumber is washed with water, then the sea cucumber is dried by a vacuum freeze-drying machine for 24h, and finally the sea cucumber dry product is crushed into 20-mesh sea cucumber powder in a crusher.

[0049] S2, supercritical treatment: the sea cucumber powder obtained in step S1 is placed in the extraction kettle of the supercritical extraction instrument equipped with an improved gas distributor, the extraction kettle temperature is set to 30°C, the extraction pressure is 30MPa, the CO2 flow rate is 30L / h, and the extraction time is 2.5h, after the extraction is completed, the sea cucumber powder in the extraction kettle is collected.

[0050] S3, super-micronization combined with supercritical: the sea cucumber powder obtained in step S2 was pre-cooled in liquid nitrogen for 1 h, and then was crushed using a super-micronizer at a rotation speed of 10000 rpm and a mesh size of 0.6 mm to obtain a powder, the bulk density of which was controlled to be 0.65 g / mL and the tap density was 0.73 g / mL; the sea cucumber powder was deodorized using a supercritical extraction instrument equipped with an improved gas distributor, the powder crushed by the super-micronizer was placed in the extraction kettle of the supercritical extraction instrument, the extraction kettle temperature was set to 30℃, the extraction pressure was 30 MPa, the CO2 flow rate was 30 L / h, and the extraction time was 2.5 h, after the extraction was completed, the sea cucumber powder in the extraction kettle was collected, and a super-micronized sea cucumber powder was obtained.

[0051] Comparative Example 1

[0052] S1, physical crushing of sea cucumber powder: fresh sea cucumber was incubated in warm water at 60℃ for 6 h, the incubated sea cucumber was opened at the abdomen, the contents in the body cavity of the sea cucumber were removed, and the body wall of the sea cucumber was washed with water, then the sea cucumber was dried by a vacuum freeze-drying machine for 24 h, and finally the dried sea cucumber was crushed into sea cucumber coarse powder with a particle size of 20 mesh.

[0053] S2, supercritical treatment: the sea cucumber coarse powder was deodorized using a supercritical extraction instrument equipped with an improved gas distributor, the sea cucumber coarse powder obtained in step S1 was placed in the extraction kettle of the supercritical extraction instrument, the extraction kettle temperature was set to 30℃, the extraction pressure was 30 MPa, the CO2 flow rate was 30 L / h, and the extraction time was 2.5 h, after the extraction was completed, the sea cucumber powder in the extraction kettle was collected.

[0054] Comparative Example 2

[0055] S1, physical crushing of sea cucumber powder: fresh sea cucumber was incubated in warm water at 60℃ for 6 h, the incubated sea cucumber was opened at the abdomen, the contents in the body cavity of the sea cucumber were removed, and the body wall of the sea cucumber was washed with water, then the sea cucumber was dried by a vacuum freeze-drying machine for 24 h, and finally the dried sea cucumber was crushed into sea cucumber coarse powder with a particle size of 20 mesh.

[0056] S2, supercritical treatment: the sea cucumber coarse powder was deodorized using a supercritical extraction instrument equipped with an improved gas distributor, the sea cucumber coarse powder obtained in step S1 was placed in the extraction kettle of the supercritical extraction instrument, the extraction kettle temperature was set to 30℃, the extraction pressure was 30 MPa, the CO2 flow rate was 30 L / h, and the extraction time was 2.5 h, after the extraction was completed, the sea cucumber powder in the extraction kettle was collected.

[0057] S3, ultrafine physical crushing: the sea cucumber powder obtained in step S2 is crushed using an ultrafine crusher, the rotation speed of the ultrafine crusher is 10000 rpm, and the mesh size of the screen is 0.6 mm to obtain sea cucumber powder, the bulk density of the powder is controlled to be 0.65 g / mL, and the tap density is 0.73 g / mL.

[0058] Comparative Example 3

[0059] S1, physical crushing of sea cucumber powder: fresh sea cucumber is placed in warm water at 60°C for temporary cultivation for 6 hours, the contents in the body cavity of the sea cucumber are removed after opening the abdomen, and the body wall of the sea cucumber is washed with water, then the sea cucumber is dried by vacuum freeze-drying machine for 24 hours, and finally the dried sea cucumber is crushed into 20-mesh sea cucumber powder.

[0060] S2, supercritical treatment: the conventional supercritical extraction instrument (without improvement of gas distributor, lack of design of second hole disc) is used to remove the odor of sea cucumber powder, the sea cucumber powder obtained in step S1 is placed in the extraction kettle of the supercritical extraction instrument, the extraction kettle temperature is set to 30°C, the extraction pressure is 30 MPa, the CO2 flow rate is 30 L / h, and the extraction time is 2.5 h, after the extraction is completed, the sea cucumber powder in the extraction kettle is collected.

[0061] S3, ultrafine crushing combined with supercritical: the sea cucumber powder obtained in step S2 is pre-cooled in liquid nitrogen for 1 h, then crushed using an ultrafine crusher, the rotation speed of the ultrafine crusher is 10000 rpm, and the mesh size of the screen is 0.6 mm to obtain the powder, the bulk density of the powder is controlled to be 0.65 g / mL, and the tap density is 0.73 g / mL; then the conventional supercritical extraction instrument (without improvement of gas distributor, lack of design of second hole disc) is used to remove the odor of sea cucumber powder, the powder crushed by the ultrafine crusher is placed in the extraction kettle of the supercritical extraction instrument, the extraction kettle temperature is set to 30°C, the extraction pressure is 30 MPa, the CO2 flow rate is 30 L / h, and the extraction time is 2.5 h.

[0062] The pipeline is blocked during the extraction process, and the extraction cannot be completed normally. This is because the volume of the ultrafine sea cucumber powder is too small, which is easily carried out of the material basket by the carbon dioxide fluid, into the carbon dioxide pipeline, causing the carbon dioxide pipeline to be blocked. The sea cucumber powder that has not been extracted still has a strong odor.

[0063] According to the experimental method of Xu Jialin (Xu Jialin, Peng Jian, Xu Yujuan, et al. Physicochemical and powder properties of mango ultrafine powder with different peel addition amounts [J]. Food and Fermentation Industries, 2024, 1-13.), take the EP tube with a volume of 2 mL, fill the EP tube with sea cucumber powder, record the mass M of the sea cucumber powder in the container, and calculate the bulk density as shown in the formula: bulk density (g / mL) = M / 2. The larger the bulk density value, the smaller the gap between particles and the smaller the particle size.

[0064] Referring to the experimental method of Li Zhenjiang (Li Zhenjiang, Liu Ying, Zhi Li, et al. Effect of ball milling ultrafine grinding on particle characteristics and polysaccharide extraction of inonotus obliquus powder [J]. China Food Additives, 2021, 32(11): 1-8.), take 2 mL of EP tube, fill the EP tube with sea cucumber powder, continuously vibrate the EP tube, and continuously add the sample until the weight of the powder reaches a stable state, record the mass M1 of the sea cucumber powder in the container, and the calculation of the tap density is shown in the formula: tap density (g / mL) = M1 / 2. The greater the tap density, the smaller the gap between the particles, the smaller the total volume, and the smaller the particle size.

[0065] Referring to the experimental method of Qi Baokun (Qi Baokun, Liu Yuwen, Yao Yuxue, et al. Analysis of the effect of protease on the volatile flavor of soybean meal based on HS-GC-IMS and HS-SPME-GC-MS [J]. Transactions of the Chinese Society of Agricultural Machinery, 2024, 1-27.), 0.1 g of sea cucumber powder was added to 1 mL of deionized water and placed in a 20 mL headspace sampling bottle. After incubation at 60°C for 30 min, automatic sampling was performed with a sampling needle temperature of 85°C, a sampling volume of 500 μL, and a non-divided mode.

[0066] The chromatographic conditions are: WAX capillary column, column temperature 60°C, operation time 30 min, carrier gas purity N2≥99.999%, N2purity≥99.999%. The analysis conditions are: 2 mL / min 2 min, 10 mL / min 8 min, 100 mL / min 10 min, 150 mL / min 10 min stop.

[0067] Qualitative analysis of different volatile substances: The drift gas (nitrogen) is set to 150 mL / min. Each spectrum is averaged 12 times. All analyses were performed in triplicate. With N-ketone C4-C9 (Beijing Nation Reagent Co., Ltd.) as an external reference, the retention index (RI) of VC was calculated. Qualitative analysis was performed by comparing the RI and the drift time of the standard in the GC-IMS library.

[0068] The sea cucumber powder prepared in Example 1, the sea cucumber powder prepared in Comparative Example 1 and Comparative Example 2 were detected, and the detection process referred to the above method. Among them, the GC-IMS two-dimensional difference topographic map is as shown in Figures 5-7 The darker the color, the greater the concentration of sample characteristic flavor. As can be seen from the figure, the green deodorization technology provided by the present application effectively removes the fishy substances in the sample, and the overall flavor difference of the sample after deodorization is not large. As can be seen from the results of Comparative Example 1 and Comparative Example 2, the ultrafine grinding process will increase the concentration of volatile substances in the sample, so further deodorization is needed after ultrafine grinding, and the use of a conventional supercritical extractor cannot complete the deodorization of the ultrafine sea cucumber powder.

[0069] The 7 categories of volatile substances, i.e. aldehydes, alcohols, ketones, acids, esters, furans and others, were identified from the topographical map in combination with HNONO 3H IMS2020 database and NIST gas phase database. Aldehydes are the main volatile organic compounds, and aldehyde compounds are usually the main components of the flavor of aquatic products and have been identified as the main source of fishy smell. The results are shown in Table 1. Figures 8-9 Pentanal, butanal, hexanal, heptanal, octanal and benzaldehyde are aldehydes with relatively high content. Among them, it is observed in Example 1 that the key fishy smell substances are significantly reduced (p < 0.05) compared with Comparative Examples 1 and 2.

[0070] The above description is only the preferred specific embodiment of the present application, but the protection scope of the present application is not limited thereto. Any person skilled in the art can make equivalent replacements or changes within the technical range disclosed in the present application according to the technical solution and inventive concept of the present application, which should be covered within the protection scope of the present application.

Claims

1. A method for deodorizing ultra-micro sea cucumber powder, characterized in that, The method comprises the following steps: S1, placing sea cucumber coarse powder in the extraction kettle of a supercritical extraction instrument to perform supercritical carbon dioxide extraction to remove the odor of the sea cucumber powder; the parameters of the extraction kettle of the supercritical extraction instrument are set as 30-40 ℃, the extraction pressure is 25-30 MPa, the CO2 flow rate is 25-30 L / h, and the extraction time is 2-2.5 h; S2, crushing the sea cucumber powder subjected to the odor removal in step S1 by using a supermicro grinder to obtain sea cucumber powder, and controlling the bulk density of the sea cucumber powder to be 0.65-0.7 g / mL and the tap density to be 0.70-0.80 g / mL; S3, placing the sea cucumber powder subjected to the supermicro crushing in step S2 in the extraction kettle of a supercritical extraction instrument to perform supercritical carbon dioxide extraction, and finally completing the odor removal of the supermicro sea cucumber powder; the parameters of the extraction kettle of the supercritical extraction instrument are set as 30-40 ℃, the extraction pressure is 25-30 MPa, the CO2 flow rate is 25-30 L / h, and the extraction time is 2-2.5 h; The supercritical extraction instrument in steps S1 and S3 is a supercritical extraction instrument provided with a gas disperser; the gas disperser in the supercritical extraction instrument is an improved gas disperser; the improved gas disperser is placed in the extraction tank; The improved gas disperser comprises a mounting pipe (1), a connecting flange (2), a first hole disc (3), a filter screen (4), a support column (5), a baffle (6), a telescopic rod (7), a spring (70), a pressing plate (8), and a second hole disc (9); The mounting pipe (1) is made of transparent material, facilitating observation of the internal condition; the upper and lower outer sides of the mounting pipe (1) are connected with the connecting flanges (2), facilitating external connection of pipelines; the inner sides of the middle and lower parts of the mounting pipe (1) are connected with the first hole discs (3); the lower sides of the first hole discs (3) are connected with the filter screens (4); the first hole discs (3) are connected with four support columns (5); the upper sides of the support columns (5) are connected with the baffles (6); the baffles (6) are in contact with the mounting pipe (1); the telescopic rods (7) are connected with the springs (70) between the fixed ends and the telescopic ends; the telescopic ends of the telescopic rods (7) are rotatably connected with the pressing plates (8); the second hole disc (9) is placed between the baffles (6); the pressing plates (8) are in contact with the second hole disc (9); the first hole disc (3) and the second hole disc (9) have the same shape; twelve conical parts are arranged on the upper side of the second hole disc (9), facilitating backflow.

2. The method of claim 1, wherein, The sea cucumber coarse powder in step S1 is sea cucumber coarse powder with a mesh size of 5-20.

3. The method according to claim 1 or 2, characterized in that, The sea cucumber coarse powder is prepared by the following method: Fresh sea cucumbers are placed in warm water at 50-60 °C for temporary cultivation for 4-8 h; the temporarily cultivated sea cucumbers are opened at the abdomen, the contents in the body cavity of the sea cucumbers are removed, and the body wall of the sea cucumbers is washed with water; then the sea cucumbers are subjected to vacuum freeze-drying for 20-24 h to remove water; finally, the dried sea cucumbers are crushed into sea cucumber coarse powder with a mesh size of 5-20 by using a grinder.

4. The method as claimed in claim 1, wherein, The crushing by using a supermicro grinder in step S2 is performed under a rotational speed of 8000-12000 rpm and by using a screen with a mesh size of 0.3-0.6 mm.

Citation Information

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