Green deodorization method suitable for ultramicro sea cucumber powder

Abstract

The invention discloses a green deodorization method suitable for ultramicro sea cucumber powder, and belongs to the field of food processing. The method comprises the following steps: S1, putting sea cucumber coarse powder into an extraction kettle of a supercritical extraction instrument, and deodorizing the sea cucumber powder; s2, crushing the sea cucumber powder subjected to fishy smell removal in the step S1 by using an ultrafine crusher to obtain sea cucumber powder, and controlling the bulk density of the powder to be 0.65-0.7 g / mL and the tap density to be 0.70-0.80 g / mL; and S3, putting the sea cucumber powder subjected to superfine grinding in the step S2 into an extraction kettle of a supercritical extraction instrument for deodorization. According to the invention, the second hole disc is additionally arranged on the gas distributor in the supercritical extraction instrument, so that carbon dioxide fluid flows back during extraction, the pressure of the carbon dioxide fluid discharged from the material basket is reduced, and the material is prevented from being taken out, thereby solving the problem of pipeline blockage of ultra-micro powder and improving the extraction efficiency and the production efficiency.

Description

Technical Field

[0001] The invention relates to a green deodorization method suitable for ultrafine sea cucumber powder, and belongs to the field of food processing. Background Art

[0002] Sea cucumbers belong to the phylum Echinodermata, class Holothuroidea. They are high in protein, low in fat, and low in cholesterol. They are also rich in a variety of trace elements and active substances such as polyunsaturated fatty acids, and have extremely high nutritional value. However, sea cucumbers have the phenomenon of "autolysis", which significantly increases the difficulty of transporting and preserving fresh sea cucumbers. Therefore, in order to prevent the occurrence of sea cucumber autolysis, most sea cucumbers need to undergo specific processing after harvesting. Among them, powder products have the advantages of fast absorption, convenient consumption, and easy storage, so sea cucumbers are often processed into powder products. Among sea cucumber powder products, ultra-fine sea cucumber powder has greatly improved its powder fineness, making it more conducive to the human body to absorb the active ingredients and nutrients in the sea cucumber powder after consumption, so it has better market prospects and research and development value.

[0003] However, due to the influence of the living environment of sea cucumbers, the body wall of sea cucumbers has a fishy smell. The crushing process during the processing of sea cucumber powder will increase the specific surface area of ​​the powder, making the sea cucumber powder have a heavier fishy smell, affecting the flavor and quality of the finished sea cucumber powder. Moreover, this situation will be further aggravated when preparing ultrafine sea cucumber powder, because the specific surface area of ​​the powder increases more, which will eventually affect the market prospects of ultrafine sea cucumber powder.

[0004] At present, the traditional methods for removing the fishy smell from sea cucumber powder are flavor masking and molecular embedding deodorization technology. The flavor masking method is to cover up the fishy smell of sea cucumber products by adding seasonings, and the molecular embedding deodorization technology is to use wall materials to embed the sea cucumber powder to cover up the fishy smell. However, these two methods increase the use of auxiliary materials and reduce the nutritional value of sea cucumber powder products; secondly, they are more suitable for removing the fishy smell of conventional sea cucumber powder (10-20 meshes), and the deodorization effect on ultra-fine sea cucumber powder (above 100 meshes) is poor.

[0005] There are other methods for removing the fishy smell from sea cucumber powder in the prior art. For example, Chinese patent CN 115918770 A (a method for preparing a marine biological health-care peptide preparation) uses a biological enzymatic hydrolysis method, through the metabolism of microorganisms, small molecular fishy substances participate in anabolism and are transformed into fishy-free macromolecular substances to achieve fishy removal, but this method is still relatively complicated, and the metabolism is not easy to control, and it is difficult to ensure the quality of industrial production.

[0006] For example, Chinese patent CN 116491632 A (a method for preparing low-smell and low-salt sea cucumber powder) uses endogenous enzyme moderate regulation and treatment, supercritical carbon dioxide extraction and separation, and other means to prepare a low-smell and low-salt sea cucumber powder. This solution has many steps and is complex to operate. In addition, this method is still aimed at removing the smell of ordinary sea cucumber powder. A conventional supercritical extractor is used, and its gas diffuser has not been improved. This will cause pipeline blockage during the subsequent processing of ultrafine sea cucumber powder, affecting production and manufacturing. Similar problems of fine powder blocking pipelines are also mentioned in the last paragraph of the left column on page 49 of "Supercritical Extraction of Sea Cucumber Cerebrosides and HPLC Detection and Analysis", which specifically states that "excessively fine materials can also cause blockage of sintering plates and pipelines in the extraction kettle under high pressure, which will be detrimental to the extraction process,..."

[0007] It can be seen that both traditional methods and existing technologies have defects in removing the fishy smell from ultrafine sea cucumber powder, so it is necessary to explore how to achieve simple and effective fishy removal of ultrafine sea cucumber powder without adding auxiliary materials. Summary of the invention

[0008] Technical issues

[0009] The product of sea cucumber will produce a fishy smell after being crushed. The fishy smell problem of ultrafine sea cucumber powder is particularly serious, which affects its flavor and quality, and also hinders the market application of ultrafine sea cucumber powder. The traditional method of removing the fishy smell will use auxiliary materials to reduce the nutritional value of sea cucumber powder products; the use of enzymatic hydrolysis is more complicated and the process is not easy to control; the use of conventional supercritical extraction instruments to remove the fishy smell will cause pipeline blockage. Therefore, it is necessary to provide a simple and effective method for removing the fishy smell of ultrafine sea cucumber powder without adding auxiliary materials.

[0010] Technical content

[0011] The purpose of the present invention is to solve the problem that the fishy smell of the product increases after the sea cucumber powder is crushed, and to provide a method for removing the fishy smell of ultrafine sea cucumber powder. The present invention improves the gas diffuser in the supercritical extraction instrument and combines the physical ultrafine physical crushing technology to develop a high-quality ultrafine sea cucumber powder product.

[0012] In order to achieve the above object, the present invention provides a method for removing fishy smell from ultrafine sea cucumber powder, comprising the following steps:

[0013] S1, placing the sea cucumber powder in an extraction kettle of a supercritical extraction instrument, and performing supercritical carbon dioxide extraction to remove the fishy smell of the sea cucumber powder;

[0014] S2, using an ultrafine grinder to grind the sea cucumber powder removed from step S1 to obtain sea cucumber powder, wherein the bulk density of the sea cucumber powder is controlled to be 0.65-0.7 g / mL, and the tap density is 0.70-0.80 g / mL;

[0015] S3, placing the sea cucumber powder after ultrafine grinding in step S2 in an extraction kettle of a supercritical extractor for supercritical carbon dioxide extraction, and finally completing the deodorization of the ultrafine sea cucumber powder.

[0016] Furthermore, the sea cucumber powder in step S1 is 5-20 mesh sea cucumber powder.

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

[0018] Place fresh sea cucumbers in warm water at 50-60℃ for 4-8 hours, open the abdomen of the temporarily cultured sea cucumber, remove the contents in the body cavity, and wash the body wall with water. Then, pass the sea cucumbers through a vacuum freeze dryer for 20-24 hours to remove moisture, and finally grind the dried sea cucumbers into 5-20 mesh sea cucumber coarse powder in a grinder.

[0019] Furthermore, the parameters of the extraction kettle of the supercritical extractor in step S1 are set to 30-40° C., extraction pressure to 25-30 MPa, CO2 flow rate to 25-30 L / h, and extraction time to 2-2.5 h.

[0020] Furthermore, in step S2, precooling is performed before pulverizing using an ultrafine pulverizer; the precooling is performed using dry ice, liquid nitrogen, or by placing the pulverizer in a freezing environment; the precooling temperature is below -20 degrees Celsius.

[0021] Furthermore, the pulverization using the ultrafine pulverizer in step S2 is performed at a rotation speed of 8000 to 12000 rpm using a 0.3 to 0.6 mm pore size mesh screen.

[0022] Furthermore, the parameters of the extraction kettle of the supercritical extractor in step S3 are set to 30-40° C., extraction pressure to 25-30 MPa, CO2 flow rate to 25-30 L / h, and extraction time to 2-2.5 h.

[0023] Furthermore, the supercritical extractor in step S1 and step S3 is a supercritical extractor equipped with a gas diffuser.

[0024] Furthermore, the gas diffuser in the supercritical extraction apparatus is an improved gas diffuser.

[0025] Furthermore, the improved gas diffuser comprises a mounting pipe (1), a connecting flange (2), a first perforated plate (3), a filter screen (4), a support column (5), a baffle (6), a telescopic rod (7), a spring (70), a pressure plate (8) and a second perforated plate (9);

[0026] The mounting tube (1) is made of a transparent material, which is convenient for observing the internal situation. The outer sides of the upper and lower parts of the mounting tube (1) are connected with connecting flanges (2) to facilitate external pipe connection. The inner side of the middle part and the inner side of the lower part of the mounting tube (1) are connected with a first hole plate (3). The lower side of the first hole plate (3) is connected with a filter screen (4). Four support columns (5) are connected between the first hole plates (3). The upper sides of the support columns (5) are connected with baffles (6). The baffles (6) are connected to the mounting tube (1). ), the baffle plates (6) are connected with telescopic rods (7), a spring (70) is connected between the fixed end and the telescopic end of the telescopic rod (7), a pressure plate (8) is rotatably connected to the telescopic end of the telescopic rod (7), a second hole plate (9) is placed between the baffle plates (6), the pressure plate (8) is in contact with the second hole plate (9), the first hole plate (3) and the second hole plate (9) have the same shape, and twelve conical parts are provided on the upper side of the second hole plate (9) to facilitate backflow.

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

[0028] 1. The gas diffuser of the conventional supercritical extractor lacks the design of a second hole plate. When extracting some relatively fine materials, the materials will be taken out of the material basket and blown into the carbon dioxide pipeline, causing the carbon dioxide pipeline to be blocked and the extraction cannot be completed normally. Therefore, the present invention adds a second hole plate to the gas diffuser to allow the carbon dioxide fluid to reflux, reduce the pressure of the carbon dioxide fluid when it is discharged from the material basket, and prevent the material from being carried out, thereby solving the pipeline blockage problem for ultrafine powders; at the same time, the reflux of the carbon dioxide fluid can also be used for secondary extraction, thereby improving the extraction efficiency and production efficiency.

[0029] 2. The present invention uses a supercritical extractor equipped with an improved gas diffuser to extract the ultrafine sea cucumber powder, thereby removing the fishy smell of the ultrafine sea cucumber powder. The overall process is simple and easy to operate, and does not involve complex processes such as enzymatic hydrolysis. It is particularly suitable for process production. Moreover, the fishy smell of the prepared ultrafine sea cucumber powder is greatly reduced, the edible quality is high, and the market value is large. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 The three-dimensional structure diagram of the improved gas diffuser; wherein, 1, mounting pipe, 2, connecting flange, 5, supporting column, 7, telescopic rod, 8, pressing plate, 9, second hole plate;

[0031] Figure 2 It is a partially cutaway three-dimensional structural schematic diagram of an improved gas diffuser; wherein, 1, a mounting pipe, 2, a connecting flange, 3, a first hole plate, 4, a filter screen, 5, a support column, 6, a baffle, 7, a telescopic rod, 8, a pressure plate, 9, a second hole plate;

[0032] Figure 3The enlarged three-dimensional structural diagram of the improved gas diffuser at A; wherein, 1, mounting tube, 5, support column, 6, baffle, 7, telescopic rod, 70, spring, 8, pressure plate, 9, second hole plate;

[0033] Figure 4 This is a supercritical extraction device with a gas diffuser installed, where the red arrow indicates the installation location of the gas diffuser;

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

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

[0036] Figure 7 It is a comparative example 2GC-IMS two-dimensional difference topography;

[0037] Figure 8 The contents of different types of volatile substances in Example 1, Comparative Example 1 and Comparative Example 2 (different letters indicate significance);

[0038] Fig. 9 The contents of key volatile substances in Example 1, Comparative Example 1 and Comparative Example 2 (different letters indicate significance). DETAILED DESCRIPTION

[0039] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0040] In the present invention, unless otherwise clearly specified and limited, the terms "connected", "connected", and "fixed" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0041] In the present invention, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may include that the first and second features are in direct contact, or may include that the first and second features are not in direct contact but are in contact through another feature between them. Moreover, a first feature being "above", "above" and "above" a second feature includes that the first feature is directly above and obliquely above the second feature, or simply indicates that the first feature is higher in level than the second feature. A first feature being "below", "below" and "below" a second feature includes that the first feature is directly below and obliquely below the second feature, or simply indicates that the first feature is lower in level than the second feature.

[0042] Experimental instruments

[0043] The supercritical extractor equipped with an improved gas diffuser used in the embodiments and comparative examples is manufactured by Jiangsu Gaoke Pharmaceutical Equipment Co., Ltd. and has a model number of GKSCFE220-40-30L. The gas diffuser of the supercritical extractor has been improved. Figures 1 to 3 .

[0044] The improved gas diffuser comprises a mounting pipe 1, a connecting flange 2, a first perforated plate 3, a filter screen 4, a supporting column 5, a baffle 6, a telescopic rod 7, a spring 70, a pressing plate 8 and a second perforated plate 9.

[0045] The mounting tube 1 is made of transparent material, which is convenient for observing the internal situation. The outer sides of the upper and lower parts of the mounting tube 1 are connected with connecting flanges 2 for external connection to pipelines. The inner side of the middle part and the inner side of the lower part of the mounting tube 1 are connected with a first hole plate 3, and the lower side of the first hole plate 3 is connected with a filter screen 4. Four support columns 5 are connected between the first hole plates 3, and the upper sides of the support columns 5 are connected with baffles 6, and the baffles 6 are in contact with the mounting tube 1. The baffles 6 are connected with telescopic rods 7, and springs 70 are connected between the fixed end and the telescopic end of the telescopic rod 7. The telescopic ends of the telescopic rods 7 are rotatably connected with pressure plates 8. A second hole plate 9 is placed between the baffles 6, and the pressure plates 8 are in contact with the second hole plate 9. The first hole plate 3 and the second hole plate 9 have the same shape, and twelve conical parts are provided on the upper side of the second hole plate 9 for reflux.

[0046] When supercritical extraction of carbon dioxide is performed, an improved gas diffuser is used to drive the device to the place where the components need to be extracted, so that the connecting flange 2 at the bottom of the mounting tube 1 is connected to the feed pipe. The mounting tube 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 extended, and the spring 70 is stretched. Then, the second orifice plate 9 is brought into contact with the baffle 6, and then the pressing plate 8 is reversely rotated to reset, and then the pressing plate 8 is released, the spring 70 rebounds, and the telescopic rod 7 shrinks and recovers, so that the pressing plate 8 is brought into contact with the second orifice plate 9, so that the second orifice plate 9 can be fixed to prevent the second orifice plate 9 from falling when the carbon dioxide fluid flows. Then, it is connected to the feed port of the extraction tank through the upper connecting flange 2. By adding carbon dioxide fluid into the feed pipeline, the carbon dioxide fluid enters the installation pipe 1, flows through the first hole plate 3, the filter screen 4 and the second hole plate 9, and then flows into the extraction tank to extract the material. The first hole plate 3 and the second hole plate 9 have the same shape, so that the carbon dioxide fluid can be fed evenly, the extraction efficiency and the production efficiency can be improved. At the same time, the device can be placed in the extraction tank, and the carbon dioxide can achieve a reflux effect under the action of the cone, so that the carbon dioxide fluid refluxes under the action of the cone on the second hole plate 9 for secondary extraction, which is convenient for secondary extraction of the material, reduces the pressure of the carbon dioxide fluid when it is discharged from the material basket, prevents the material from being brought out, and improves the extraction effect.

[0047] Example 1

[0048] S1. Physical crushing of sea cucumber powder: fresh sea cucumbers are placed in warm water at 60°C for 6 hours, the abdomen of the temporarily cultivated sea cucumbers is opened, the contents in the body cavity of the sea cucumbers are removed, and the body wall of the sea cucumbers is cleaned with water, and then the sea cucumbers are passed through a vacuum freeze dryer for 24 hours to remove moisture, and finally the dried sea cucumbers are crushed into 20-mesh sea cucumber coarse powder in a grinder.

[0049] S2, supercritical treatment: Use a supercritical extractor equipped with an improved gas diffuser to remove the fishy smell of the sea cucumber powder. Place the sea cucumber powder obtained in step S1 in the extraction kettle of the supercritical extractor. The temperature of the extraction kettle 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, collect the sea cucumber powder in the extraction kettle.

[0050] S3, ultrafine grinding combined with supercritical: the sea cucumber powder obtained in step S2 is precooled in liquid nitrogen for 1 hour, and then crushed by an ultrafine grinder, the ultrafine grinder speed is 10000rpm, the mesh aperture is 0.6mm, and the powder is crushed to obtain a powder, the bulk density of the powder is controlled to be 0.65g / mL, and the tap density is 0.73g / mL; the sea cucumber powder is then deodorized by a supercritical extractor equipped with an improved gas diffuser, and the powder crushed by the ultrafine grinder is placed in an extraction kettle of the supercritical extractor, 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 to obtain ultrafine sea cucumber powder.

[0051] Comparative Example 1

[0052] S1. Physical crushing of sea cucumber powder: fresh sea cucumbers are placed in warm water at 60°C for 6 hours, the abdomen of the temporarily cultivated sea cucumbers is opened, the contents in the body cavity of the sea cucumbers are removed, and the body wall of the sea cucumbers is cleaned with water, and then the sea cucumbers are passed through a vacuum freeze dryer for 24 hours to remove moisture, and finally the dried sea cucumbers are crushed into 20-mesh sea cucumber coarse powder in a grinder.

[0053] S2, supercritical treatment: Use a supercritical extractor equipped with an improved gas diffuser to remove the fishy smell of the sea cucumber powder. Place the sea cucumber powder obtained in step S1 in the extraction kettle of the supercritical extractor. The temperature of the extraction kettle 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, collect the sea cucumber powder in the extraction kettle.

[0054] Comparative Example 2

[0055] S1. Physical crushing of sea cucumber powder: fresh sea cucumbers are placed in warm water at 60°C for 6 hours, the abdomen of the temporarily cultivated sea cucumbers is opened, the contents in the body cavity of the sea cucumbers are removed, and the body wall of the sea cucumbers is cleaned with water, and then the sea cucumbers are passed through a vacuum freeze dryer for 24 hours to remove moisture, and finally the dried sea cucumbers are crushed into 20-mesh sea cucumber coarse powder in a grinder.

[0056] S2, supercritical treatment: Use a supercritical extractor equipped with an improved gas diffuser to remove the fishy smell of the sea cucumber powder. Place the sea cucumber powder obtained in step S1 in the extraction kettle of the supercritical extractor. The temperature of the extraction kettle 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, collect the sea cucumber powder in the extraction kettle.

[0057] S3, ultrafine physical pulverization: The sea cucumber powder obtained in step S2 is pulverized using an ultrafine pulverizer at a speed of 10000 rpm and a mesh aperture of 0.6 mm to obtain the sea cucumber powder, and 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 cucumbers are placed in warm water at 60°C for 6 hours, the abdomen of the temporarily cultivated sea cucumbers is opened, the contents in the body cavity of the sea cucumbers are removed, and the body wall of the sea cucumbers is cleaned with water, and then the sea cucumbers are passed through a vacuum freeze dryer for 24 hours to remove moisture, and finally the dried sea cucumbers are crushed into 20-mesh sea cucumber coarse powder in a grinder.

[0060] S2, supercritical treatment: Use a conventional supercritical extractor (the gas diffuser is not improved and the design of the second hole plate is lacking) to remove the fishy smell of the sea cucumber powder. The sea cucumber powder obtained in step S1 is placed in the extraction kettle of the supercritical extractor. The temperature of the extraction kettle 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.

[0061] S3, ultrafine grinding combined with supercritical: the sea cucumber powder obtained in step S2 is precooled in liquid nitrogen for 1 hour, and then crushed in an ultrafine grinder, the ultrafine grinder speed is 10000rpm, and the mesh aperture is 0.6mm to obtain powder, the bulk density of the powder is controlled to be 0.65g / mL, and the tap density is 0.73g / mL; then the sea cucumber powder is deodorized using a conventional supercritical extractor (the gas diffuser is not improved, and the design of the second hole plate is lacking), and the powder crushed by the ultrafine grinder is placed in the extraction kettle of the supercritical extractor, and 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.

[0062] The pipeline is blocked during the extraction process and the extraction cannot be completed normally. This is because the ultra-fine sea cucumber powder is too small and can be easily carried out of the material basket by the carbon dioxide fluid and enter the carbon dioxide pipeline, causing the carbon dioxide pipeline to be blocked. The unextracted sea cucumber powder still has a strong fishy smell.

[0063] Referring to Xu Jialin's experimental method (Xu Jialin, Peng Jian, Xu Yujuan, et al. Study on the physical and chemical properties of mango ultrafine powder with different amounts of peel added [J]. Food and Fermentation Industry, 2024, 1-13.), take an EP tube with a volume of 2mL, fill the EP tube with sea cucumber powder, and record the mass M of the sea cucumber powder in the container. The calculation of the bulk density is 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 of birch inonotus powder and polysaccharide extraction effect [J]. Chinese Food Additives, 2021, 32(11): 1-8.), take a 2mL EP tube, fill the EP tube with sea cucumber powder, vibrate the EP tube continuously, and continue to add samples until the powder weight reaches a stable state. Record the mass M1 of the sea cucumber powder in the container. The calculation of the tap density is shown in the formula: tap density (g / mL) = M1 / 2. The larger the tap density, the smaller the particle gap, 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 influence 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.), 0.1g of sea cucumber powder was added with 1mL of deionized water and placed in a 20mL headspace injection bottle. After incubation at 60℃ for 30min, the sample was automatically injected, the injection needle temperature was 85℃, the injection volume was 500μL, and the splitless mode was adopted.

[0066] Chromatographic conditions: WAX capillary column, column temperature 60°C, operation time 30 min, carrier gas purity N2 ≥ 99.999%, N2 purity ≥ 99.999%. Analysis conditions: 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) was set to 150 mL / min. Each spectrum was scanned 12 times on average. All analyses were performed in triplicate. The retention index (RI) of VC was calculated using N-ketone C4-C9 (Beijing Sinopharm Chemical Reagent Co., Ltd.) as an external reference. Qualitative analysis was performed by comparing the RI with the drift time of the standard in the GC-IMS library.

[0068] The ultrafine sea cucumber powder prepared in Example 1 and the sea cucumber powder prepared in Comparative Example 1 and Comparative Example 2 were tested, and the testing process was referred to the above method. Among them, the GC-IMS two-dimensional difference topography is as follows Figures 5 to 7 As shown, the darker the color, the greater the concentration of the characteristic flavor of the sample. It can be seen from the figure that the green deodorization technology provided by the present invention effectively removes the fishy substances in the sample, and the overall flavor of the sample after deodorization is not much different. The results of Comparative Examples 1 and 2 show that the ultrafine grinding process will increase the concentration of volatile substances in the sample, so it is necessary to further deodorize after ultrafine grinding, and the use of conventional supercritical extraction instruments cannot complete the deodorization of ultrafine sea cucumber powder.

[0069] Combining the HNONO 3H IMS2020 database with the NIST gas phase database, seven categories of volatile substances, namely aldehydes, alcohols, ketones, acids, esters, furans and others, were identified from the topographic map. Among them, aldehydes are the main volatile organic compounds. 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 as follows Figures 8-9 As shown. Valeraldehyde, butyraldehyde, hexanal, heptaldehyde, octanal and benzaldehyde are aldehydes with relatively high content. Among them, it is observed that the key fishy smell substances in Example 1 are significantly reduced compared with Comparative Examples 1 and 2 (p<0.05).

[0070] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for removing fishy smell from ultrafine sea cucumber powder, characterized in that: The following steps are involved: S1, placing the sea cucumber powder in an extraction kettle of a supercritical extraction instrument, and performing supercritical carbon dioxide extraction to remove the fishy smell of the sea cucumber powder; S2, using an ultrafine grinder to grind the sea cucumber powder removed from step S1 to obtain sea cucumber powder, wherein the bulk density of the sea cucumber powder is controlled to be 0.65-0.7 g / mL, and the tap density is 0.70-0.80 g / mL; S3, placing the sea cucumber powder after ultrafine grinding in step S2 in an extraction kettle of a supercritical extractor for supercritical carbon dioxide extraction, and finally completing the deodorization of the ultrafine sea cucumber powder; The supercritical extractor in step S1 and step S3 is a supercritical extractor equipped with a gas diffuser; the gas diffuser in the supercritical extractor is an improved gas diffuser; The improved gas diffuser comprises a mounting pipe (1), a connecting flange (2), a first perforated plate (3), a filter screen (4), a supporting column (5), a baffle (6), a telescopic rod (7), a spring (70), a pressure plate (8) and a second perforated plate (9); The mounting tube (1) is made of a transparent material, which is convenient for observing the internal situation. The outer sides of the upper and lower parts of the mounting tube (1) are connected with connecting flanges (2) to facilitate external pipe connection. The inner side of the middle part and the inner side of the lower part of the mounting tube (1) are connected with a first hole plate (3). The lower side of the first hole plate (3) is connected with a filter screen (4). Four support columns (5) are connected between the first hole plates (3). The upper sides of the support columns (5) are connected with baffles (6). The baffles (6) are connected to the mounting tube (1). ), the baffle plates (6) are connected with telescopic rods (7), a spring (70) is connected between the fixed end and the telescopic end of the telescopic rod (7), a pressure plate (8) is rotatably connected to the telescopic end of the telescopic rod (7), a second hole plate (9) is placed between the baffle plates (6), the pressure plate (8) is in contact with the second hole plate (9), the first hole plate (3) and the second hole plate (9) have the same shape, and twelve conical parts are provided on the upper side of the second hole plate (9) to facilitate backflow.

2. The method according to claim 1, characterized in that The sea cucumber coarse powder in step S1 is 5-20 mesh sea cucumber coarse powder.

3. The method according to claim 1 or 2, characterized in that Sea cucumber powder is prepared by the following method: Place fresh sea cucumbers in warm water at 50-60℃ for 4-8 hours, open the abdomen of the temporarily cultured sea cucumber, remove the contents in the body cavity, and wash the body wall with water. Then, pass the sea cucumbers through a vacuum freeze dryer for 20-24 hours to remove moisture, and finally grind the dried sea cucumbers into 5-20 mesh sea cucumber coarse powder in a grinder.

4. The method according to claim 1, characterized in that In step S1, the parameters of the extraction kettle of the supercritical extractor are set to 30-40° C., extraction pressure to 25-30 MPa, CO2 flow rate to 25-30 L / h, and extraction time to 2-2.5 h.

5. The method according to claim 1, characterized in that The pulverization using the ultrafine pulverizer in step S2 is performed at a rotation speed of 8000 to 12000 rpm using a 0.3 to 0.6 mm aperture mesh screen.

6. The method according to claim 1, characterized in that In step S3, the parameters of the extraction kettle of the supercritical extractor are set to 30-40° C., extraction pressure to 25-30 MPa, CO2 flow rate to 25-30 L / h, and extraction time to 2-2.5 h.

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