Process for removing impurities from royal jelly

Abstract

The invention discloses a royal jelly impurity removal process which comprises the following steps: (1) taking a light three-dimensional mesh material, soaking in a beewax-ethanol solution, and volatilizing ethanol after soaking to obtain an impurity removal adsorption material; (2) spreading the impurity-removing adsorption material on the surface of the fresh royal jelly, introducing nitrogen to carry out micro-bubble flotation, and taking out the impurity-removing adsorption material after flotation to obtain the royal jelly after flotation; and (3) centrifugally separating the floated royal jelly to obtain centrifugal slurry and precipitate, adding water into the precipitate for washing, standing for layering, removing impurities at the bottom layer, and uniformly mixing the obtained crystal particles with the centrifugal slurry to obtain the royal jelly. According to the method, most of impurities in the royal jelly can be removed by combining a special adsorption impurity removal material with microbubble flotation, then impurities such as dust are removed through centrifugal separation, the impurity removal effect can be comprehensively and effectively improved, effective components of the royal jelly cannot be affected, stable existence of 10-HDA in the royal jelly is promoted, and the storage effect is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of food processing, and in particular relates to a royal jelly impurity removal process. Background Art

[0002] Royal jelly is a milky white or light yellow pulpy substance secreted by the upper jaw of worker bees for the queen bee and bee larvae to eat. Fresh royal jelly is a viscous pulpy substance, semi-fluid, delicate to the touch, slightly sticky, with a strong spicy taste, a slightly sweet aftertaste, and partially soluble in water. 10-Hydroxy-2-De cenoic acid (10-Hydroxy-2-De cenoic acid) is referred to as 10-HDA, also known as royal jelly acid, is an important unsaturated fatty acid in royal jelly, accounting for about 50% of the total amount of royal jelly fatty acids, and the content in royal jelly is 1.4%-2.0%. The content of 10-HDA in royal jelly specified in standard GB9697 is qualified when it is above 1.4%. 10-HDA is a white crystal at room temperature. It is a relatively stable substance. It is easily soluble in methanol, ethanol, chloroform, and ether, slightly soluble in acetone, and difficult to dissolve in water. The melting point is 64°C. 10-HDA has multiple physiological activities. It can strengthen the body and strongly inhibit various cancer cells such as lymphoma and breast cancer, enhance the body's immune function, and treat acute radiation damage and damage caused by chemicals.

[0003] During the production process, fresh royal jelly often contains impurities such as wax flakes and larvae, which affect the purity and sensory state of the royal jelly. To solve this problem, manufacturers generally filter and remove impurities from the royal jelly. However, during the filtering and removing process, some 10-HDA is easily filtered out along with the impurities, resulting in the loss of 10-HDA in the royal jelly after filtering and removing impurities, and the quality does not meet the standards.

[0004] In addition, although fresh royal jelly is generally not easy to precipitate 10-HDA, it is easy to precipitate 10-HDA crystals under the influence of temperature, especially when it is below 2-4°C. my country stipulates that royal jelly should be stored at -18°C, which makes it easy for different degrees of crystals to appear in royal jelly after freezing, affecting the appearance and taste.

[0005] Invention patent CN86107034B discloses a method for processing and producing fresh royal jelly products, which further extracts the filter residue after filtering the royal jelly to obtain 10-HDA crystals, which can be added to the royal jelly as needed to adjust the quality of the royal jelly and solve the problem of 10-HDA not meeting the standard.

[0006] The above technologies have the following problems: 1. In the process of extracting 10-HDA from the residue after filtering royal jelly, impurities such as broken wax flakes (beeswax) and larvae are not removed first, which affects the separation of 10-HDA; some also use a variety of chemical substances, which affect the safety and purity of royal jelly, and the operation is cumbersome.

[0007] 2. When the 10-HDA extracted from the filter residue is added back to the royal jelly, both 10-HDA and the royal jelly need to be freeze-dried. Otherwise, adding 10-HDA directly to the liquid royal jelly will still make it unstable, causing the royal jelly to have a serious granular feel and unstable storage.

[0008] Based on the above problems, the royal jelly that is currently filtered and processed is prone to the risk of substandard quality, but the impurity problem of royal jelly that is not filtered and processed is difficult to solve.

[0009] In summary, how to provide a royal jelly impurity removal process that not only removes impurities in royal jelly through a simple and environmentally friendly method, but also does not cause 10-HDA loss and can ensure the stability of royal jelly is an urgent problem to be solved. Summary of the invention

[0010] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a royal jelly impurity removal process. Most of the hydrophobic impurities in the royal jelly can be removed by special adsorption impurity removal materials combined with microbubble flotation, and then impurities such as sand and dust are removed by centrifugal separation. The impurity removal effect can be effectively improved comprehensively without affecting the effective ingredients of the royal jelly. In addition, the present invention also promotes the stable existence of 10-HDA in the royal jelly and improves the storage effect.

[0011] In order to achieve the above object, the present invention adopts the following technical solutions: A royal jelly impurity removal process comprises the following steps: (1) Take a clean lightweight three-dimensional mesh material and immerse it in a beeswax-ethanol solution. After the immersion is completed, the ethanol is evaporated, and then cooled and sterilized at 0-10°C to obtain an impurity removal adsorption material; (2) spreading the impurity removal adsorption material obtained in step (1) on the surface of fresh royal jelly, and then placing it in a microbubble flotation device, introducing nitrogen gas for microbubble flotation, and surface impurities (wax flakes, larvae, etc.) are adsorbed on the surface of bubbles due to hydrophobicity and thus enriched on the surface of the slurry, thereby removing these impurities. After the flotation is completed, the impurity removal adsorption material is taken out to obtain the royal jelly after flotation; (3) The royal jelly after flotation is centrifuged to obtain centrifugal slurry and precipitate. The precipitate is washed with (10-50 times) water, allowed to stand for stratification, and impurities on the bottom layer (sand, dust, etc.) are discarded to obtain crystalline particles. The crystalline particles are evenly mixed with the centrifugal slurry to complete the royal jelly impurity removal process and obtain pure royal jelly.

[0012] Preferably, in step (1), the lightweight three-dimensional mesh material is a natural plant material with a three-dimensional mesh structure or an artificially synthesized plastic three-dimensional mesh material, and the lightweight three-dimensional mesh material has a thickness of 1-5 cm and a porosity of ≥90%.

[0013] More preferably, the lightweight three-dimensional mesh material is loofah sponge, which has strong adsorption and large capacity and can absorb a large amount of surface impurities.

[0014] Preferably, in step (1), the concentration of the beeswax-ethanol solution (ie, the mass percentage of beeswax) is 5-20%, the immersion time is 30-50 min, and the immersion temperature is 30-50°C.

[0015] Preferably, in step (1), the immersion process includes: first immersing in a beeswax-ethanol solution with a concentration of 5-10% for 10-20 min at a immersion temperature of 30-40°C, then evaporating the ethanol, and then immersing in a beeswax-ethanol solution with a concentration of 15-20% for 20-30 min at a immersion temperature of 40-50°C.

[0016] Preferably, in step (1), when the acidity of fresh royal jelly is 30-40 mL / 100g, the beeswax used is western beeswax (beeswax secreted by western bees); when the acidity of fresh royal jelly is 41-53 mL / 100g, the beeswax used is Chinese beeswax (beeswax secreted by Chinese honey bees).

[0017] Preferably, in step (2), the diameter of the microbubbles is 50-100 μm, the nitrogen introduction rate is 0.3-0.6 L / min, the flotation temperature is 5-10°C (fewer 10-HDA crystal particles are formed in this temperature range, and the temperature will not be too high to affect the activity of the royal jelly), the flotation time is 6-15 min, and the amount of impurity removal adsorption material added is 4-10% of the volume of the royal jelly.

[0018] Preferably, in step (3), the centrifugal speed is 2000-3000 r / min, the temperature is 3-6 °C, and the time is 3-6 min. The centrifugal speed and temperature need to be controlled appropriately. If the centrifugal speed is too slow, the separation is not thorough. If the centrifugal speed is too fast, the effective ingredients of royal jelly are easily damaged. If the centrifugal temperature is too low, the slurry fluidity is not strong and the separation is not thorough. If the centrifugal temperature is too high, the crystalline particles (10-HDA crystals) cannot be separated.

[0019] Preferably, in step (3), the royal jelly after flotation is refrigerated before centrifugation, and the refrigeration temperature is 1-3°C and the refrigeration time is 10-30h (the purpose of refrigeration is to fully precipitate unstable 10-HDA crystals, prepare for the subsequent treatment of crystal particles, and obtain more stable 10-HDA).

[0020] Preferably, step (3) further comprises treating the crystallized particles as follows: S1, taking the lower layer of the centrifuged slurry, freezing it at -(10-20)°C, grinding it into particles 1, taking the crystal particles, adding (3-5 times the amount) of ethanol to mix, and then spraying it on the surface of particles 1, and after spraying, decompressing and volatilizing the ethanol to obtain particles 2; S2. Take the upper layer of the centrifuged slurry and spray it onto the surface of particle 2. After spraying, cool it to - (10-20) ° C and keep it for 1-3 hours.

[0021] Preferably, the mass ratio of the lower slurry, the upper slurry and the crystal particles is (5-10): (0.5-3): 1, and the particle size of the particles 1 is 10-60 μm.

[0022] Technical effects of the present invention: 1. The present invention uses nitrogen to perform microbubble flotation on fresh royal jelly. By controlling the nitrogen introduction rate and the flotation temperature, hydrophobic impurities such as broken wax flakes and larvae in the royal jelly are gathered on the surface. At the same time, an impurity removal adsorption material with a three-dimensional network structure is spread on the surface of the royal jelly to adsorb and remove these hydrophobic impurities. Then, impurities such as sand and dust are removed by centrifugal separation, which can effectively remove most of the impurities in the royal jelly without affecting the effective ingredients 10-HDA, protein, sugar, etc. in the royal jelly.

[0023] 2. When preparing the impurity removal adsorption material of the present invention, the lightweight three-dimensional mesh material is impregnated with beeswax to improve its affinity with impurities such as broken wax flakes and larvae, while reducing its affinity with 10-HDA, thereby preventing the impurity removal adsorption material from adsorbing 10-HDA. During the impregnation, a low-concentration beeswax-ethanol solution is first used for impregnation to form a basic beeswax layer, and then a higher concentration beeswax-ethanol solution is used for impregnation to increase the thickness and density of the beeswax layer and improve the stability of the beeswax layer.

[0024] 3. The acidity of royal jelly is correlated with its 10-HDA and free acid content. When the acidity of royal jelly is low, the 10-HDA and free acid content is generally low, and the polarity is low. The beeswax used for impregnation of lightweight three-dimensional mesh materials should be western beeswax, which can significantly reduce the affinity of royal jelly with impurity removal adsorption materials, promote flotation effect, and reduce royal jelly loss; when the acidity of royal jelly is high, the 10-HDA and free acid content is generally high, and the polarity is high. The beeswax used for impregnation of lightweight three-dimensional mesh materials should be Chinese beeswax to reduce the affinity of royal jelly with impurity removal adsorption materials. Therefore, the properties of the beeswax used in the impregnation of lightweight three-dimensional mesh materials in the present invention directly affect the flotation effect of royal jelly, and it is necessary to select a suitable one.

[0025] 4. The present invention further processes the crystal particles (mainly containing 10-HDA crystals) obtained by centrifugal separation in step (3), disperses the effective substance 10-HDA in the crystal particles in a sandwich layer formed by the lower slurry (with higher density) and the upper slurry (with lower density and containing more lipid components) of the centrifuged slurry, and then adds the 10-HDA to the centrifuged slurry to obtain a finished product after impurities are removed. This can improve the dispersion stability and fusion of 10-HDA in royal jelly, reduce the granularity, and has strong stability, which is conducive to subsequent storage.

[0026] In the present invention, the royal jelly after flotation is subjected to refrigeration treatment for a certain period of time before centrifugal separation in step (3), so that 10-HDA crystals can be fully separated out, which facilitates the subsequent treatment of the crystal particles to improve storage stability.

[0027] 5. Although the 10-HDA content in royal jelly is relatively stable under different storage conditions, its obvious content loss generally occurs in the early stage of storage, which may be related to oxidation due to contact with air in the early stage of storage. The present invention can adjust the position of 10-HDA in royal jelly through the sandwich layer structure with different densities on both sides, thereby reducing the contact of 10-HDA with air, thereby reducing the possibility of oxidation and deterioration of 10-HDA, and ensuring the stability of the 10-HDA content during the storage of royal jelly. DETAILED DESCRIPTION

[0028] The above scheme is further described below in conjunction with specific embodiments; it should be understood that these embodiments are used to illustrate the basic principles, main features and advantages of the present invention, and the present invention is not limited to the scope of the following embodiments; the implementation conditions adopted in the embodiments can be further adjusted according to specific requirements, and the implementation conditions not specified are usually the conditions in conventional experiments.

[0029] Unless otherwise specified in the following examples, all raw materials are commercially available or prepared by conventional methods in the art. Example 1

[0030] In this embodiment, the acidity of the fresh royal jelly raw material is 50 mL / 100 g, and the beeswax used is Chinese beeswax (acid value 5-8).

[0031] This embodiment provides a royal jelly impurity removal process, comprising the following steps: (1) Take clean loofah pulp (3 cm thick, porosity ≥ 90%), immerse it in a beeswax-ethanol solution with a concentration (i.e., the mass percentage of beeswax) of 12% for 40 min at a temperature of 40°C. After immersion, evaporate the ethanol, cool it at 3°C, and sterilize it with ultraviolet light to obtain the impurity removal adsorption material. (2) Spreading the impurity-removing adsorbent material obtained in step (1) on the surface of fresh royal jelly, and then placing it in a microbubble flotation apparatus, introducing nitrogen at a rate of 0.45 L / min for microbubble flotation, the diameter of the microbubbles is 50-100 μm, the flotation temperature is 8°C, the flotation time is 10 min, and after the flotation is completed, the impurity-removing adsorbent material is taken out to obtain the royal jelly after flotation; the amount of impurity-removing adsorbent material added is 7% of the volume of the royal jelly.

[0032] (3) The royal jelly after flotation is centrifuged at a speed of 2500 r / min, a temperature of 4°C, and a time of 5 min to obtain a centrifugal slurry and a precipitate. The precipitate is washed with 20 times the amount of water and allowed to stand for stratification. The impurities on the bottom layer (sand) are discarded to obtain crystalline particles (mainly containing 10-HDA particles). The crystalline particles are evenly mixed with the centrifugal slurry to complete the royal jelly impurity removal process and obtain pure royal jelly. Example 2

[0033] In this embodiment, the acidity of the fresh royal jelly raw material is 35 mL / 100 g, and the beeswax used is western beeswax (acid value 18-20).

[0034] This embodiment provides a royal jelly impurity removal process, and the specific steps are the same as those in Embodiment 1. Example 3

[0035] In this embodiment, the acidity of the fresh royal jelly raw material is 35 mL / 100 g, and the beeswax used is Chinese beeswax (acid value 5-8).

[0036] This embodiment provides a royal jelly impurity removal process, and the specific steps are the same as those in Embodiment 1. Example 4

[0037] In this embodiment, the acidity of the fresh royal jelly raw material is 50 mL / 100 g, and the beeswax used is western beeswax (acid value 18-20).

[0038] This embodiment provides a royal jelly impurity removal process, and the specific steps are the same as those in Embodiment 1. Example 5

[0039] This embodiment provides a royal jelly impurity removal process, which is different from the embodiment 1 in that the soaking process of the sponge gourd in step (1) is divided into two soakings, and the specific step (1) is as follows: Take clean loofah pulp (thickness 3 cm, porosity ≥ 90%), first immerse it in an 8% beeswax-ethanol solution for 15 minutes at a temperature of 35°C, then evaporate the ethanol, and then immerse it in an 18% beeswax-ethanol solution for 25 minutes at a temperature of 45°C. After immersion, evaporate the ethanol, then cool it at 3°C ​​and sterilize it with ultraviolet light to obtain the impurity removal adsorption material.

[0040] The rest is the same as Example 1. Example 6

[0041] This embodiment provides a royal jelly impurity removal process, which differs from Embodiment 5 in that the crystal particles obtained in step (3) are treated to improve the dispersion stability and fusion of 10-HDA in royal jelly. In this case, step (3) is specifically as follows: The royal jelly after flotation was centrifuged at a speed of 2500 r / min, a temperature of 4 ℃, and a time of 5 minutes to obtain centrifugal slurry and sediment. The sediment was washed with 20 times of water, allowed to stand for stratification, and the bottom layer (sand, dust, etc.) impurities were discarded to obtain crystal particles (mainly containing 10-HDA crystals). The crystal particles were treated as follows: S1, take the lower layer of the centrifuged slurry, freeze it at -15 °C, grind it into particles 1 with a particle size of 30 μm, take the crystal particles and add (4 times the amount) of ethanol to mix, and then spray it on the surface of particles 1, and after spraying, reduce the pressure to evaporate the ethanol to obtain particles 2; S2. Take the upper slurry of the centrifuged slurry and spray it onto the surface of particle 2. After spraying, cool it to -15 °C and keep it for 2 hours to obtain the treated crystal particles. The mass ratio of the lower slurry, the upper slurry and the crystal particles is 7:1:1.

[0042] The treated crystal particles are evenly mixed with the remaining centrifuged slurry, thus completing the royal jelly impurity removal process and obtaining pure royal jelly.

[0043] The rest is the same as Example 5. Example 7

[0044] This embodiment provides a royal jelly impurity removal process, which is different from the embodiment 6 in that in step (3), the royal jelly after flotation needs to be refrigerated before centrifugal separation, in order to fully separate the 10-HDA crystals and prepare for the subsequent treatment of the crystal particles. In this case, step (3) is specifically as follows: The royal jelly after flotation was refrigerated at 2 °C for 20 hours. After refrigeration, it was centrifuged at 2500 r / min, 4 °C for 5 minutes to obtain centrifuged slurry and sediment. The sediment was washed with 20 times water, allowed to stand and stratify, and the bottom impurities (sand, dust, etc.) were discarded to obtain crystal particles (mainly containing 10-HDA crystal particles). The crystal particles were treated as follows: S1, take the lower layer of the centrifuged slurry, freeze it at -15 °C, grind it into particles 1 with a particle size of 30 μm, take the crystal particles and add (4 times the amount) of ethanol to mix, and then spray it on the surface of particles 1, and after spraying, reduce the pressure to evaporate the ethanol to obtain particles 2; S2. Take the upper slurry of the centrifuged slurry and spray it onto the surface of particle 2. After spraying, cool it to -15 °C and keep it for 2 hours to obtain the treated crystal particles. The mass ratio of the lower slurry, the upper slurry and the crystal particles is 7:1:1.

[0045] The treated crystal particles are evenly mixed with the remaining centrifuged slurry, thus completing the royal jelly impurity removal process and obtaining pure royal jelly.

[0046] The rest is the same as Example 6. Example 8

[0047] In this embodiment, the acidity of the fresh royal jelly raw material is 50 mL / 100 g, and the beeswax used is Chinese beeswax (acid value 5-8).

[0048] This embodiment provides a royal jelly impurity removal process, comprising the following steps: (1) Take clean loofah pulp (thickness 1 cm, porosity ≥ 90%), immerse it in a 5% beeswax-ethanol solution for 10 min at 40 °C, evaporate the ethanol, and immerse it in a 15% beeswax-ethanol solution for 20 min at 50 °C. After immersion, evaporate the ethanol, cool it at 0 °C, and sterilize it with ultraviolet light to obtain the impurity removal adsorption material.

[0049] (2) Spreading the impurity-removing adsorbent material obtained in step (1) on the surface of fresh royal jelly, and then placing it in a microbubble flotation apparatus, introducing nitrogen at a rate of 0.3 L / min for microbubble flotation, the diameter of the microbubble is 50-100 μm, the flotation temperature is 5°C, the flotation time is 15 min, and after the flotation is completed, the impurity-removing adsorbent material is taken out to obtain the royal jelly after flotation; the amount of impurity-removing adsorbent material added is 4% of the volume of the royal jelly.

[0050] (3) The royal jelly after flotation was refrigerated at 1°C for 10 hours. After refrigeration, it was centrifuged at 2000 r / min, 6°C for 3 minutes to obtain centrifuged slurry and precipitate. The precipitate was washed with 10 times the amount of water, allowed to stand for stratification, and the bottom layer (sand) impurities were discarded to obtain crystal particles (mainly containing 10-HDA crystal particles). The crystal particles were treated as follows: S1, take the lower layer of the centrifuged slurry, freeze it at -10 °C, grind it into particles 1 with a particle size of 10 μm, take the crystal particles and add (3 times the amount) of ethanol to mix, and then spray it on the surface of particles 1, and after spraying, reduce the pressure to evaporate the ethanol to obtain particles 2; S2. Take the upper slurry of the centrifuged slurry and spray it onto the surface of particle 2. After spraying, cool it to -10 °C and keep it for 3 hours to obtain the treated crystal particles. The mass ratio of the lower slurry, the upper slurry and the crystal particles is 5:0.5:1.

[0051] The treated crystal particles are evenly mixed with the remaining centrifuged slurry, thus completing the royal jelly impurity removal process and obtaining pure royal jelly. Example 9

[0052] In this embodiment, the acidity of the fresh royal jelly raw material is 50 mL / 100 g, and the beeswax used is Chinese beeswax (acid value 5-8).

[0053] This embodiment provides a royal jelly impurity removal process, comprising the following steps: (1) Take clean loofah pulp (5 cm thick, porosity ≥ 90%), immerse it in a 10% beeswax-ethanol solution for 20 min at 30 °C, evaporate the ethanol, and immerse it in a 20% beeswax-ethanol solution for 30 min at 40 °C. After immersion, evaporate the ethanol, cool it at 10 °C, and sterilize it with ultraviolet light to obtain the impurity removal adsorption material.

[0054] (2) Spreading the impurity-removing adsorbent material obtained in step (1) on the surface of fresh royal jelly, and then placing it in a microbubble flotation apparatus, introducing nitrogen at a rate of 0.6 L / min for microbubble flotation, the diameter of the microbubbles is 50-100 μm, the flotation temperature is 10° C., the flotation time is 6 min, and after the flotation is completed, the impurity-removing adsorbent material is taken out to obtain the royal jelly after flotation; the amount of impurity-removing adsorbent material added is 10% of the volume of the royal jelly.

[0055] (3) The royal jelly after flotation was refrigerated at 3°C ​​for 30 hours; after refrigeration, it was centrifuged at 3000 r / min, 3°C for 6 minutes to obtain centrifuged slurry and precipitate. The precipitate was washed with 50 times water, allowed to stand for stratification, and the bottom layer (sand, dust, etc.) impurities were discarded to obtain crystal particles (mainly containing 10-HDA crystal particles). The crystal particles were treated as follows: S1, take the lower layer of the centrifuged slurry, freeze it at -20 °C, grind it into particles 1 with a particle size of 60 μm, take the crystal particles and add (5 times the amount) of ethanol to mix, and then spray it on the surface of particles 1, and after spraying, reduce the pressure to evaporate the ethanol to obtain particles 2; S2. Take the upper slurry of the centrifuged slurry and spray it onto the surface of particle 2. After spraying, cool it to -20 °C and keep it for 1 hour to obtain the treated crystal particles. The mass ratio of the lower slurry, the upper slurry and the crystal particles is 10:3:1.

[0056] The treated crystal particles are evenly mixed with the remaining centrifuged slurry, thus completing the royal jelly impurity removal process and obtaining pure royal jelly.

[0057] Comparative Example 1 The difference between this comparative example and Example 1 is that no impurity removal adsorption material is used in the royal jelly impurity removal process. In this case, the impurity removal process does not include step (1). Step (2) is: placing fresh royal jelly in a microbubble flotation device, introducing nitrogen at a rate of 0.45 L / min for microbubble flotation, the diameter of the microbubbles is 50-100 μm, the flotation temperature is 8°C, the flotation time is 10 min, and after the flotation is completed, the surface impurities are scraped off to obtain the floated royal jelly.

[0058] Comparative Example 2 The difference between this comparative example and Example 1 is that the royal jelly impurity removal process does not use microbubble flotation, and only uses adsorption impurity removal materials for adsorption. At this time, the impurity removal process includes the following steps: (1) Take clean loofah pulp (3 cm thick, porosity ≥ 90%), immerse it in a beeswax-ethanol solution with a concentration (i.e., the mass percentage of beeswax) of 12% for 40 min at a temperature of 40°C. After immersion, evaporate the ethanol, cool it at 3°C, and sterilize it with ultraviolet light to obtain the impurity removal adsorption material. (2) The impurity removal adsorption material prepared in step (1) is mixed evenly with fresh royal jelly to adsorb impurities at an adsorption temperature of 8°C and an adsorption time of 10 min. After the adsorption is completed, the impurity removal adsorption material is removed to obtain royal jelly after flotation. The amount of impurity removal adsorption material added is 3% of the volume of the royal jelly.

[0059] (3) The royal jelly after flotation is centrifuged at a speed of 2500 r / min, a temperature of 4°C, and a time of 5 min to obtain a centrifugal slurry and a precipitate. The precipitate is washed with 20 times the amount of water, allowed to stand for stratification, and the bottom impurities are discarded to obtain crystalline particles (mainly containing 10-HDA crystals). The crystalline particles are evenly mixed with the centrifugal slurry to complete the royal jelly impurity removal process and obtain pure royal jelly.

[0060] Comparative Example 3 The difference between this comparative example and Example 1 is that the sponge gourd in the royal jelly impurity removal process step (1) is replaced with activated carbon.

[0061] Comparative Example 4 The difference between this comparative example and Example 1 is that the sponge gourd in the royal jelly impurity removal process step (1) is replaced with silica gel.

[0062] Comparative Example 5 The difference between this comparative example and Example 1 is that the sponge gourd sponge is not soaked in the royal jelly impurity removal process step (1). In this case, step (1) is: taking clean sponge gourd sponge, sterilizing it with ultraviolet light, and obtaining the impurity removal adsorption material.

[0063] Comparative Example 6 The difference between this comparative example and Example 1 is that in the royal jelly impurity removal process step (2), the nitrogen introduction rate is 0.1 L / min.

[0064] Comparative Example 7 The difference between this comparative example and Example 1 is that in the royal jelly impurity removal process step (2), the nitrogen introduction rate is 0.8 L / min.

[0065] Comparative Example 8 The difference between this comparative example and Example 1 is that in the royal jelly impurity removal process step (2), the flotation temperature is 3°C.

[0066] Comparative Example 9 The difference between this comparative example and Example 1 is that in the royal jelly impurity removal process step (2), the flotation temperature is 12°C.

[0067] Comparative Example 10 The difference between this comparative example and Example 1 is that in the royal jelly impurity removal process step (2), the flotation time is 4 minutes.

[0068] Comparative Example 11 The difference between this comparative example and Example 1 is that in the royal jelly impurity removal process step (2), the flotation time is 18 minutes.

[0069] Comparative Example 12 The difference between this comparative example and Example 1 is that in the royal jelly impurity removal process step (3), the centrifugal speed is 1000 r / min.

[0070] Comparative Example 13 The difference between this comparative example and Example 1 is that in the royal jelly impurity removal process step (3), the centrifugal speed is 4000 r / min.

[0071] Comparative Example 14 The difference between this comparative example and Example 1 is that in the royal jelly impurity removal process step (3), the temperature of the centrifugal treatment is 1°C.

[0072] Comparative Example 15 The difference between this comparative example and Example 1 is that in the royal jelly impurity removal process step (3), the temperature of the centrifugal treatment is 8°C.

[0073] Comparative Example 16 The difference between this comparative example and Example 7 is that when the crystal particles are treated in the royal jelly impurity removal process step (3), step S2 is not included, that is, the crystal particles are subjected to the following treatment: S1. Take the lower layer of the centrifuged slurry, freeze it at -15 °C, grind it into particles 1 with a particle size of 50 μm, take the crystal particles and add (4 times the amount) of ethanol to mix, and then spray it on the surface of particles 1. After spraying, reduce the pressure to evaporate the ethanol to obtain particles 2, which are the treated crystal particles.

[0074] Comparative Example 17 The difference between this comparative example and Example 7 is that when the crystal particles are treated in the royal jelly impurity removal process step (3), step S1 is not included, that is, the crystal particles are subjected to the following treatment: taking the upper slurry of the centrifuged slurry, spraying it onto the surface of the crystal particles, cooling it to -15°C after spraying and keeping it for 2 hours, and obtaining the treated crystal particles.

[0075] Comparative Example 18 The difference between this comparative example and Example 7 is that when the crystal particles are treated in the royal jelly impurity removal process step (3), the lower slurry in step S1 is exchanged with the upper slurry in step S2.

[0076] Comparative Example 19 The difference between this comparative example and Example 7 is that in the royal jelly impurity removal process step (3), the crystal particles are treated as follows: the upper slurry, the lower slurry and the crystal particles of the centrifuged slurry are mixed evenly, and then cooled to -15°C and maintained for 2 hours to obtain the treated crystal particles.

[0077] Comparative Example 20 The difference between this comparative example and Example 7 is that when the crystal particles are treated in the royal jelly impurity removal process step (3), the particle size of the particles 1 is 5 μm.

[0078] Comparative Example 21 The difference between this comparative example and Example 7 is that when the crystal particles are treated in the royal jelly impurity removal process step (3), the particle size of the particles 1 is 100 μm.

[0079] Comparative Example 22 The difference between this comparative example and Example 7 is that when the crystal particles are treated in the royal jelly impurity removal process step (3), the mass ratio of the lower layer slurry to the crystal particles is 3:1.

[0080] Comparative Example 23 The difference between this comparative example and Example 7 is that when the crystal particles are treated in the royal jelly impurity removal process step (3), the mass ratio of the lower layer slurry to the crystal particles is 15:1.

[0081] Comparative Example 24 The difference between this comparative example and Example 7 is that when the crystal particles are treated in the royal jelly impurity removal process step (3), the mass ratio of the upper slurry to the crystal particles is 0.2:1.

[0082] Comparative Example 25 The difference between this comparative example and Example 7 is that when the crystal particles are treated in the royal jelly impurity removal process step (3), the mass ratio of the upper slurry to the crystal particles is 4:1.

[0083] 1. Quality inspection of royal jelly obtained by the impurity removal process of the present invention Referring to the requirements of GB9697 "Royal Jelly", the quality of the fresh royal jelly used in the present invention and the royal jelly obtained by the impurity removal process of Examples 1-9 was tested, and the results are shown in Table 1 below. Among them, the fresh royal jelly used in Examples 1 and 4-9 is the same, numbered ①, and the fresh royal jelly used in Examples 2-3 is the same, numbered ②.

[0084] Table 1

[0085] As shown in Table 1, the royal jelly obtained by the impurity removal process of Examples 1-9 of the present invention meets the quality requirements of GB9697, indicating the feasibility of the process of the present invention. Compared with fresh royal jelly, the ash content in Examples 1-2 and 5-9 is significantly reduced, and the content of effective ingredients 10-hydroxy-2-decenoic acid, protein, total sugar, etc. does not change significantly, indicating that the process of the present invention has a significant impurity removal effect on royal jelly, and the loss of effective ingredients (especially 10-hydroxy-2-decenoic acid) is less.

[0086] Compared with Examples 1 and 2, Example 3 (the acidity of fresh royal jelly is 35 mL / 100g, and the beeswax used is Chinese beeswax) and Example 4 (the acidity of fresh royal jelly is 50 mL / 100g, and the beeswax used is Western beeswax) did not select the type of beeswax according to the different acidities of fresh royal jelly according to the present invention, and the impurity removal effect of impurities such as broken wax flakes and larvae was reduced, which affected the subsequent removal effect of impurities such as dust, increased ash content, and increased 10-hydroxy-2-decenoic acid loss.

[0087] 2. Comparison of the effects of the impurity removal process of the present invention 1. Effect of removing impurities such as wax flakes and larvae According to the process of Examples 1-9 and Comparative Examples 1-11 of the present invention, fresh royal jelly was removed from impurities. The royal jelly obtained in different steps was observed under a microscope to see whether there were impurities such as broken wax flakes and larvae. The results are shown in Table 2.

[0088] Among them, the evaluation is based on the area ratio of impurities: no obvious impurities: level 0; impurity area accounts for 1-5%: level 1; impurity area accounts for 6-10%: level 2; impurity area accounts for 11-15%: level 3; impurity area accounts for 16-20%: level 4; impurity area accounts for 21-30%: level 5; impurity area accounts for 31-40%: level 6; impurity area accounts for 41-50%: level 7; impurity area accounts for 51-60%: level 8; impurity area accounts for 61-80%: level 9; impurity area accounts for 81-100%: level 10.

[0089] Table 2

[0090] It can be seen from Table 2 that compared with fresh royal jelly, the royal jelly removal process of Examples 1-9 of the present invention has a more obvious effect on removing impurities such as broken wax flakes and larvae, especially the royal jelly obtained by the impurity removal process of Examples 6-9, which did not have obvious impurities such as broken wax flakes and larvae.

[0091] Compared with Examples 1 and 2, Example 3 (the acidity of fresh royal jelly is 35 mL / 100g, and the beeswax used is Chinese beeswax) and Example 4 (the acidity of fresh royal jelly is 50 mL / 100g, and the beeswax used is Western beeswax) did not select the type of beeswax according to the different acidities of fresh royal jelly according to the method of the present invention, and the impurity removal effect was reduced.

[0092] On the basis of Example 1, Examples 5-9 used two beeswax impregnations of different concentrations when impregnating the sponge gourd with beeswax solution, so that the impurity removal effect was improved.

[0093] Compared with Example 1, the impurity removal process steps in Comparative Examples 1-11 were changed, resulting in reduced impurity removal effects.

[0094] 2. Dust and other impurities removal effect With reference to the requirements of GB9697 "Royal Jelly", the ash content of the royal jelly obtained by the impurity removal process of Example 1 and Comparative Examples 12-15 was tested. The results are shown in Table 3.

[0095] Table 3

[0096] It can be seen from the results in Table 3 that, compared with Example 1, Comparative Examples 12-15 changed the conditions of centrifugal separation, so that the removal of impurities such as sand and dust was affected, and the ash content in the royal jelly was increased.

[0097] 3. Changes in 10-hydroxy-2-decenoic acid (10-HDA) content before and after microbubble flotation According to the process of Examples 1-9 and Comparative Examples 1-5 of the present invention, fresh royal jelly was subjected to microbubble flotation, and the change of 10-HDA content was measured and compared with the fresh royal jelly raw material. The results are shown in Table 4.

[0098] Table 4

[0099] As shown in Table 4, the loss of 10-HDA is small in the microbubble flotation process of Examples 1-2 and 5-9 of the present invention. Compared with Examples 1 and 2, Examples 3 and 4 do not select the type of beeswax according to the different acidity of fresh royal jelly according to the present invention, and the loss of 10-HDA also increases.

[0100] Compared with Example 1, Comparative Examples 1-5 changed the impurity removal process steps, resulting in an increase in 10-HDA loss.

[0101] III. Changes of royal jelly obtained by the impurity removal process of the present invention at different storage times In order to improve the dispersion stability and fusion of 10-HDA in royal jelly, the present invention further processes the obtained crystal particles (mainly containing 10-HDA crystals) after centrifugal separation and dust removal. Comparing the 10-HDA content in the royal jelly after the impurity removal process in Table 1 above with the 10-HDA content in the royal jelly after the microbubble flotation process in Table 4, it can be seen that the processing steps of the present invention on the crystal particles (mainly containing 10-HDA crystals) have a low impact on the 10-HDA content and will not cause obvious 10-HDA loss.

[0102] 1. Changes in 10-HDA content of royal jelly at different storage times The royal jelly obtained by the impurity removal process of Examples 6-9 of the present invention and Comparative Examples 16-25 was tested for changes in 10-HDA content at the same storage temperature of -18°C and different storage times (0, 3, 7, 14, 21, 28 days) and compared with fresh royal jelly raw materials. The results are shown in Table 5 below.

[0103] Table 5

[0104] As shown in Table 5, compared with the 27.88% 10-HDA loss rate of fresh royal jelly in 28 days, after treating the crystal particles (mainly containing 10-HDA crystals) in Examples 6-9 of the present invention, the storage stability of the 10-HDA content in the royal jelly was improved, and the 10-HDA loss rate under the storage condition of -18°C and 28 days was significantly reduced to the range of 3.92-13.79%. It shows that the royal jelly impurity removal process of the present invention can also improve the storage stability of royal jelly products.

[0105] Compared with Example 7, Comparative Examples 16-25 changed the processing steps of the crystal particles. As a result, the 10-HDA content in the royal jelly gradually decreased with the extension of storage time, indicating that the storage stability decreased.

[0106] 2. Changes in the granularity of royal jelly at different storage times The royal jelly obtained according to the impurity removal process of Examples 6-9 of the present invention and Comparative Examples 16-25 was stored at the same storage temperature of -18°C and different storage times (0, 7, 14, and 28 days) and the granularity of the royal jelly was observed. The results are shown in Table 6.

[0107] Among them, the evaluation is based on the number of crystals appearing in the royal jelly: no obvious crystallization: level 0; slight crystallization: level 1; medium amount of crystallization: level 2; and a large number of crystals: level 3.

[0108] Table 6

[0109] As shown in Table 6, compared with fresh royal jelly, the storage stability of royal jelly was improved after the crystal particles (mainly containing 10-HDA crystal particles) were treated in Examples 6-9 of the present invention, and the number of crystals visually observed under the storage conditions of 2°C and 28 days was significantly reduced, and the granularity was reduced. In particular, Examples 7-9 had better effects.

[0110] Compared with Example 7, Comparative Examples 16-25 changed the processing steps of the crystal particles. As a result, the number of crystals visually observed in the royal jelly gradually increased with the extension of storage time, and the granular feel increased, indicating that the storage stability decreased.

[0111] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A royal jelly impurity removal process, characterized in that: The following steps are involved: (1) Take a lightweight three-dimensional mesh material and immerse it in a beeswax-ethanol solution. After the immersion is completed, the ethanol is evaporated, and then cooled and sterilized to obtain an impurity removal adsorption material; (2) spreading the impurity removal adsorption material obtained in step (1) on the surface of fresh royal jelly, and then introducing nitrogen gas to perform microbubble flotation. After the flotation is completed, the impurity removal adsorption material is taken out to obtain the royal jelly after flotation; (3) The royal jelly after flotation is centrifuged to obtain centrifugal slurry and precipitate, the precipitate is washed with water, allowed to stand for stratification, and the bottom impurities are discarded to obtain crystal particles, and the crystal particles are evenly mixed with the centrifugal slurry.

2. The process according to claim 1, characterized in that: In step (1), the lightweight three-dimensional mesh material is a natural plant material with a three-dimensional mesh structure or an artificially synthesized plastic three-dimensional mesh material. The thickness of the lightweight three-dimensional mesh material is 1-5 cm, and the porosity is ≥90%.

3. The process according to claim 1, characterized in that: In step (1), the concentration of the beeswax-ethanol solution is 5-20%, the immersion time is 30-50 min, and the immersion temperature is 30-50 °C.

4. The process according to claim 1, characterized in that: In step (1), when the acidity of fresh royal jelly is 30-40 mL / 100 g, the beeswax used is western beeswax; when the acidity of fresh royal jelly is 41-53 mL / 100 g, the beeswax used is Chinese beeswax.

5. The process according to claim 1, characterized in that: In step (2), the nitrogen introduction rate is 0.3-0.6 L / min, the flotation temperature is 5-10°C, the flotation time is 6-15 min, and the amount of impurity removal adsorption material added is 4-10% of the volume of the royal jelly.

6. The process according to claim 1, characterized in that: In step (3), the centrifugal speed is 2000-3000 r / min, the temperature is 3-6 °C, and the time is 3-6 min.

7. The process according to claim 1, characterized in that: In step (3), the royal jelly after flotation needs to be refrigerated before centrifugal separation. The refrigeration temperature is 1-3°C and the refrigeration time is 10-30h.

8. The process according to any one of claims 1 to 7, characterized in that: Step (3) further includes treating the crystallized particles as follows: S1, taking the lower layer of the centrifuged slurry, freezing and grinding it into particles 1, taking the crystal particles and adding ethanol to mix, and then spraying it on the surface of particles 1, and after spraying, decompressing and volatilizing the ethanol to obtain particles 2; S2. Take the upper layer of the centrifuged slurry and spray it onto the surface of particle 2. After spraying, cool it to - (10-20) ° C and keep it for 1-3 hours.

9. The process according to claim 2, characterized in that: In step (1), the immersion process includes: first immersing in a beeswax-ethanol solution with a concentration of 5-10% for 10-20 minutes at a immersion temperature of 30-40°C, then evaporating the ethanol, and then immersing in a beeswax-ethanol solution with a concentration of 15-20% for 20-30 minutes at a immersion temperature of 40-50°C.

10. The process according to claim 8, characterized in that: The mass ratio of the lower slurry, the upper slurry and the crystal particles is (5-10): (0.5-3): 1, and the particle size of the particles 1 is 10-60 μm.

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