A process for removing impurities from royal jelly

Abstract

This invention discloses a process for removing impurities from royal jelly, comprising the following steps: (1) taking a lightweight three-dimensional mesh material, immersing it in a beeswax-ethanol solution, and evaporating the ethanol after immersion to obtain the impurity-removing adsorbent material; (2) spreading the impurity-removing adsorbent material on the surface of fresh royal jelly, introducing nitrogen gas for microbubble flotation, removing the impurity-removing adsorbent material after flotation to obtain the flotated royal jelly; (3) centrifuging the flotated royal jelly to obtain centrifuged slurry and precipitate, washing the precipitate with water, allowing it to stand and separate into layers, discarding the bottom impurities, and mixing the obtained crystalline particles evenly with the centrifuged slurry. This invention uses a special adsorbent material combined with microbubble flotation to remove most of the impurities in royal jelly, and then centrifuging to remove dust and other impurities. This comprehensive approach effectively improves the impurity removal effect without affecting the effective components of royal jelly, and also promotes the stable existence of 10-HDA in royal jelly, thus improving the storage effect.

Description

Technical Field

[0001] The present invention belongs to the technical field of food processing, and particularly relates to a process for removing impurities from royal jelly. Background Art

[0002] Royal jelly is a milky white or light yellow paste secreted by the mandibles of worker bees for the exclusive consumption of queen bees and bee larvae. Fresh royal jelly is a viscous paste, semi-fluid, with a delicate texture, slightly sticky, having a strong pungent taste, a slightly sweet aftertaste, and is partially soluble in water. 10-Hydroxy-2-decenoic acid (10-HDA), also known as royal jelly acid, is an important unsaturated fatty acid in royal jelly, accounting for about 50% of the total fatty acids in royal jelly, and its content in royal jelly is 1.4% - 2.0%. The content of 10-HDA in royal jelly specified by Standard GB9697 is defined as qualified if it is above 1.4%. 10-HDA is a white crystal at normal temperature, a relatively stable substance, easily soluble in methanol, ethanol, chloroform, ether, slightly soluble in acetone, and hardly soluble in water, with a melting point of 64°C. 10-HDA has various physiological activities, 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 injury and injuries caused by chemical substances, etc.

[0003] During the production process, fresh royal jelly often contains impurities such as broken wax pieces and larvae, which affect the purity and sensory state of royal jelly. To solve this problem, manufacturers generally filter and remove impurities from royal jelly. However, during the filtration and impurity removal process, part of the 10-HDA is easily filtered out together with the impurities, resulting in the loss of 10-HDA in the royal jelly after filtration and impurity removal, and the quality does not meet the standard.

[0004] In addition, although fresh royal jelly generally does not easily precipitate 10-HDA, it is very easy to precipitate 10-HDA crystals under the influence of temperature, especially when the temperature is below 2 - 4°C, it is extremely easy to crystallize. China stipulates that royal jelly should be stored at a low temperature of -18°C, resulting in different degrees of crystals in the frozen royal jelly, which affects the appearance and taste.

[0005] The invention patent CN86107034B discloses a processing and production method for fresh royal jelly products. The filter residue after filtering royal jelly is further extracted to obtain 10-HDA crystals, which can be added to royal jelly as needed to adjust the quality of royal jelly and solve the problem of unqualified 10-HDA.

[0006] The above technologies have the following problems: 1. In the process of extracting 10-HDA from the filter residue after royal jelly filtration, 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 10-HDA extracted from the filter residue is added back to royal jelly, both 10-HDA and royal jelly need to be freeze-dried. Otherwise, adding 10-HDA directly to liquid royal jelly will still result in instability, causing the royal jelly to have a severe grainy texture and unstable storage.

[0008] Based on the above issues, filtered royal jelly is prone to quality defects, while the impurity problem of unfiltered royal jelly is difficult to solve.

[0009] In conclusion, the urgent problem to be solved is how to provide a royal jelly impurity removal process that not only removes impurities from royal jelly in a simple and environmentally friendly way, but also avoids 10-HDA loss and ensures the stability of royal jelly. Summary of the Invention

[0010] The purpose of this invention is to overcome the shortcomings of the prior art and provide a royal jelly impurity removal process. By combining special adsorption and impurity removal materials with microbubble flotation, most of the hydrophobic impurities in royal jelly can be removed. Then, centrifugation is used to remove impurities such as sand and dust. The overall process can effectively improve the impurity removal effect without affecting the effective components of royal jelly. Furthermore, this invention also promotes the stable existence of 10-HDA in royal jelly and improves the storage effect.

[0011] To achieve the above objectives, the present invention adopts the following technical solution: A process for removing impurities from royal jelly includes the following steps: (1) Take a clean, lightweight three-dimensional mesh material and immerse it in a beeswax-ethanol solution. After immersion, evaporate the ethanol and then cool and sterilize it at 0-10 ℃ to obtain the impurity removal adsorption material. (2) Spread the impurity removal adsorption material obtained in step (1) on the surface of fresh royal jelly, and then place it in a microbubble flotation device. Nitrogen gas is introduced for microbubble flotation. Surface impurities (fragmented wax pieces, larvae, etc.) are adsorbed on the surface of the bubbles due to hydrophobicity and thus accumulate on the surface of the jelly, thereby removing these impurities. After the flotation is completed, the impurity removal adsorption material is taken out to obtain the flotated royal jelly. (3) After flotation, the royal jelly is centrifuged to obtain centrifuged slurry and precipitate. The precipitate is washed with (10-50 times) water, allowed to stand and separate into layers, and the bottom layer (sand, dust, etc.) impurities are discarded to obtain crystalline particles. The crystalline particles are mixed evenly with the centrifuged 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 thickness of the lightweight three-dimensional mesh material is 1-5 cm, with a porosity ≥90%.

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

[0014] Preferably, in step (1), the concentration of the beeswax-ethanol solution (i.e., the mass percentage of beeswax) is 5-20%, the impregnation time is 30-50 min, and the impregnation temperature is 30-50 ℃.

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

[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 central beeswax (beeswax secreted by Chinese honeybees).

[0017] Preferably, in step (2), the diameter of the microbubbles is 50-100 μm, the nitrogen gas introduction rate is 0.3-0.6 L / min, the flotation temperature is 5-10℃ (the 10-HDA crystal particles formed in this temperature range are fewer, and the temperature will not be too high to affect the activity of 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 royal jelly.

[0018] Preferably, in step (3), the centrifugation speed is 2000-3000 r / min, the temperature is 3-6 ℃, and the time is 3-6 min. The centrifugation speed and temperature need to be properly controlled. If the centrifugation speed is too slow, the separation will not be complete, and if the centrifugation speed is too fast, the effective components of royal jelly will be easily damaged. If the centrifugation temperature is too low, the fluidity of the jelly will not be strong and the separation will not be complete. If the centrifugation temperature is too high, the crystalline particles (10-HDA crystals) cannot be separated.

[0019] Preferably, before centrifuging the royal jelly after flotation in step (3), it is necessary to perform cold storage treatment. The cold storage temperature is 1-3 ℃ and the cold storage time is 10-30h (the purpose of cold storage is to fully analyze the unstable 10-HDA crystals, prepare for the subsequent crystallization particle processing, and obtain more stable 10-HDA).

[0020] Preferably, step (3) further includes treating the crystalline particles as follows: S1. Take the lower layer of the centrifuged slurry, freeze it at -10-20℃, grind it into particles 1, take the crystalline particles and mix them with (3-5 times the amount) of ethanol, then spray them onto the surface of particles 1, and evaporate the ethanol under reduced pressure after spraying 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)℃ and keep it for 1-3 hours.

[0021] Preferably, the mass ratio of the lower slurry, the upper slurry, and the crystallized 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. This invention uses nitrogen gas for microbubble flotation of fresh royal jelly. By controlling the nitrogen gas introduction rate and flotation temperature, hydrophobic impurities such as broken wax flakes and larvae in the royal jelly are made to accumulate on the surface. At the same time, a three-dimensional mesh-structured impurity-removing adsorption material is spread on the surface of the royal jelly to adsorb and remove these hydrophobic impurities. Then, centrifugation is used to remove impurities such as sand and dust, which can effectively remove most of the impurities in the royal jelly without affecting the effective components such as 10-HDA, protein, and sugar in the royal jelly.

[0023] 2. In preparing the impurity-removing adsorbent material according to this invention, the lightweight three-dimensional mesh material is impregnated with beeswax to increase its affinity for impurities such as broken wax fragments and larvae, while reducing its affinity for 10-HDA, thus preventing the adsorbent material from adsorbing 10-HDA. During impregnation, a low-concentration beeswax-ethanol solution is first used to form a basic beeswax layer, followed by impregnation with a higher-concentration beeswax-ethanol solution to increase the thickness and density of the beeswax layer and improve its stability.

[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 content of 10-HDA and free acid is generally low, and the polarity is low. When impregnating lightweight three-dimensional mesh materials, western beeswax should be used, which can significantly reduce the affinity between royal jelly and the impurity removal adsorption material, promoting the flotation effect while reducing royal jelly loss. When the acidity of royal jelly is high, the content of 10-HDA and free acid is generally also high, and the polarity is high. When impregnating lightweight three-dimensional mesh materials, medium beeswax should be used to reduce the affinity between royal jelly and the impurity removal adsorption material. Therefore, the properties of the beeswax used in the impregnation of lightweight three-dimensional mesh materials in this invention directly affect the flotation effect of royal jelly and need to be selected appropriately.

[0025] 4. The present invention further processes the crystalline particles (mainly containing 10-HDA crystals) obtained by centrifugation in step (3), dispersing the effective substance 10-HDA of the crystalline particles in the sandwich layer formed by the lower layer of the centrifuged slurry (with higher density) and the upper layer of the slurry (with lower density and higher lipid content), and then adding it to the centrifuged slurry to obtain the finished product after impurity removal. This can improve the dispersion stability and fusion of 10-HDA in royal jelly, reduce the graininess, and has strong stability, which is beneficial for subsequent storage.

[0026] Before centrifuging the royal jelly after flotation in step (3), the present invention also refrigerates it for a certain period of time, which can fully extract 10-HDA crystals, making it easier to process the crystal particles and improve storage stability.

[0027] 5. Although the 10-HDA content in royal jelly is relatively stable under different storage conditions, its significant 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. This invention can regulate the position of 10-HDA in royal jelly through a sandwich layer structure with different densities on both sides, reducing the contact between 10-HDA and air, thereby reducing the possibility of oxidative deterioration of 10-HDA and ensuring the stability of 10-HDA content during the storage of royal jelly. Detailed Implementation

[0028] The above-mentioned solution will be further described below with reference to 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 used 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 / 100g, and the beeswax used is medium beeswax (acid value 5-8).

[0031] This embodiment provides a process for removing impurities from royal jelly, including the following steps: (1) Take a clean loofah sponge (thickness 3 cm, porosity ≥90%) and immerse it in a beeswax-ethanol solution with a concentration (i.e., the mass percentage of beeswax) of 12% for 40 min. The immersion temperature is 40 ℃. After immersion, evaporate the ethanol and then cool it at 3 ℃ and sterilize it with ultraviolet light to obtain the impurity removal adsorption material. (2) Spread the impurity removal adsorption material obtained in step (1) on the surface of fresh royal jelly, and then place it in a microbubble flotation device. Nitrogen gas is introduced at a rate of 0.45 L / min for microbubble flotation. The diameter of the microbubble is 50-100 μm, the flotation temperature is 8 ℃, and the flotation time is 10 min. After the flotation is completed, the impurity removal adsorption material is taken out to obtain the flotated royal jelly. The amount of impurity removal adsorption material added is 7% of the volume of royal jelly.

[0032] (3) The royal jelly after flotation is centrifuged at a speed of 2500 r / min, a temperature of 4 ℃, and a time of 5 min to obtain centrifuged slurry and precipitate. The precipitate is washed with 20 times the amount of water, allowed to stand and separate into layers, and the bottom layer (sand particles) impurities are discarded to obtain crystalline particles (mainly containing 10-HDA crystals). The crystalline particles are mixed evenly with the centrifuged 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 / 100g, and the beeswax used is Western beeswax (acid value 18-20).

[0034] This embodiment provides a process for removing impurities from royal jelly, and the specific steps are the same as in Embodiment 1. Example 3

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

[0036] This embodiment provides a process for removing impurities from royal jelly, and the specific steps are the same as in Embodiment 1. Example 4

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

[0038] This embodiment provides a process for removing impurities from royal jelly, and the specific steps are the same as in Embodiment 1. Example 5

[0039] This embodiment provides a process for removing impurities from royal jelly. The difference between this process and that in embodiment 1 is that the soaking process of the loofah sponge in step (1) is divided into two soakings. In this case, step (1) is specifically as follows: Take a clean loofah sponge (3 cm thick, porosity ≥90%), first soak it in an 8% beeswax-ethanol solution for 15 min at a soaking temperature of 35 ℃, then evaporate the ethanol, and then soak it in an 18% beeswax-ethanol solution for 25 min at a soaking temperature of 45 ℃. After soaking, evaporate the ethanol, then cool it at 3 ℃ and sterilize it with ultraviolet light to obtain the impurity removal adsorption material.

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

[0041] This embodiment provides a royal jelly impurity removal process, which differs from Embodiment 5 in that the crystalline particles obtained in step (3) are treated to improve the dispersion stability and integrability of 10-HDA in royal jelly. Step (3) specifically involves: The flotation-processed royal jelly was centrifuged at 2500 r / min, 4 ℃, and for 5 min to obtain a centrifuged slurry and precipitate. The precipitate was washed with 20 times its volume of water, allowed to stand to separate into layers, and the bottom layer (sand, dust, etc.) was discarded to obtain crystalline particles (mainly containing 10-HDA crystals). The crystalline particles were then processed as follows: S1. Take the lower layer of the centrifuged slurry, freeze it at -15 ℃, grind it into particles 1 with a particle size of 30 μm, take the crystalline particles and mix them with (4 times the amount) ethanol, then spray them onto the surface of particles 1, and evaporate the ethanol under reduced pressure after spraying 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 -15 ℃ and keep it for 2 hours to obtain the treated crystalline particles. The mass ratio of the lower layer slurry, the upper layer slurry and the crystalline particles is 7:1:1.

[0042] The treated crystallized particles are mixed evenly with the remaining centrifuged slurry to complete the royal jelly impurity removal process and obtain pure royal jelly.

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

[0044] This embodiment provides a process for removing impurities from royal jelly. The difference between this process and Embodiment 6 is that step (3) requires cold storage before centrifugation of the flotated royal jelly. The purpose of this cold storage is to allow sufficient precipitation of 10-HDA crystals, preparing for subsequent crystallization. Specifically, step (3) is as follows: The royal jelly after flotation was refrigerated at 2 ℃ for 20 h. After refrigeration, it was centrifuged at 2500 r / min at 4 ℃ for 5 min to obtain a centrifuged slurry and precipitate. The precipitate was washed with 20 times its volume of water, allowed to stand to separate into layers, and the bottom layer (sand, dust, etc.) was discarded to obtain crystalline particles (mainly containing 10-HDA crystals). The crystalline particles were then processed as follows: S1. Take the lower layer of the centrifuged slurry, freeze it at -15 ℃, grind it into particles 1 with a particle size of 30 μm, take the crystalline particles and mix them with (4 times the amount) ethanol, then spray them onto the surface of particles 1, and evaporate the ethanol under reduced pressure after spraying 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 -15 ℃ and keep it for 2 hours to obtain the treated crystalline particles. The mass ratio of the lower layer slurry, the upper layer slurry and the crystalline particles is 7:1:1.

[0045] The treated crystallized particles are mixed evenly with the remaining centrifuged slurry to complete the royal jelly impurity removal process and obtain pure royal jelly.

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

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

[0048] This embodiment provides a process for removing impurities from royal jelly, including the following steps: (1) Take a clean loofah sponge (thickness 1 cm, porosity ≥90%), first soak it in a 5% beeswax-ethanol solution for 10 min at a soaking temperature of 40 ℃, then evaporate the ethanol, then soak it in a 15% beeswax-ethanol solution for 20 min at a soaking temperature of 50 ℃, evaporate the ethanol after soaking, then cool it at 0 ℃ and sterilize it with ultraviolet light to obtain the impurity removal adsorption material.

[0049] (2) Spread the impurity removal adsorption material obtained in step (1) on the surface of fresh royal jelly, and then place it in a microbubble flotation device. Nitrogen gas is introduced 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 ℃, and the flotation time is 15 min. After the flotation is completed, the impurity removal adsorption material is taken out to obtain the flotated royal jelly. The amount of impurity removal adsorption material added is 4% of the volume of royal jelly.

[0050] (3) The royal jelly after flotation was refrigerated at 1 ℃ for 10 h. After refrigeration, it was centrifuged at 2000 r / min at 6 ℃ for 3 min to obtain centrifuged slurry and precipitate. The precipitate was washed with 10 times its volume of water, allowed to stand and separate into layers, and the bottom layer (sand particles) was discarded to obtain crystalline particles (mainly containing 10-HDA crystals). The crystalline particles were then processed as follows: S1. Take the lower layer of the centrifuged slurry, freeze it at -10 ℃, grind it into particles 1 with a particle size of 10 μm, take the crystalline particles and mix them with (3 times the amount) ethanol, then spray them onto the surface of particles 1, and evaporate the ethanol under reduced pressure after spraying 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 ℃ and maintain it for 3 hours to obtain the treated crystalline particles. The mass ratio of the lower layer slurry, the upper layer slurry and the crystalline particles is 5:0.5:1.

[0051] The treated crystallized particles are mixed evenly with the remaining centrifuged slurry to complete the royal jelly impurity removal process and obtain pure royal jelly. Example 9

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

[0053] This embodiment provides a process for removing impurities from royal jelly, including the following steps: (1) Take a clean loofah sponge (thickness 5 cm, porosity ≥90%), first soak it in a 10% beeswax-ethanol solution for 20 min at a soaking temperature of 30 ℃, then evaporate the ethanol, then soak it in a 20% beeswax-ethanol solution for 30 min at a soaking temperature of 40 ℃, after soaking, evaporate the ethanol, then cool it at 10 ℃ and sterilize it with ultraviolet light to obtain the impurity removal adsorption material.

[0054] (2) Spread the impurity removal adsorption material obtained in step (1) on the surface of fresh royal jelly, and then place it in a microbubble flotation device. Nitrogen gas is introduced at a rate of 0.6 L / min for microbubble flotation. The diameter of the microbubble is 50-100 μm, the flotation temperature is 10℃, and the flotation time is 6 min. After the flotation is completed, the impurity removal adsorption material is taken out to obtain the flotated royal jelly. The amount of impurity removal adsorption material added is 10% of the volume of royal jelly.

[0055] (3) The royal jelly after flotation was refrigerated at 3 ℃ for 30 h. After refrigeration, it was centrifuged at 3000 r / min at 3 ℃ for 6 min to obtain centrifuged slurry and precipitate. The precipitate was washed with 50 times the amount of water, allowed to stand and separate into layers, and the bottom layer (sand, dust, etc.) was discarded to obtain crystalline particles (mainly containing 10-HDA crystals). The crystalline particles were then processed as follows: S1. Take the lower layer of the centrifuged slurry, freeze it at -20 ℃, grind it into particles 1 with a particle size of 60 μm, take the crystalline particles and mix them with (5 times the amount) ethanol, then spray them onto the surface of particles 1, and evaporate the ethanol under reduced pressure after spraying 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 -20 ℃ and keep it for 1 hour to obtain the treated crystalline particles. The mass ratio of the lower layer slurry, the upper layer slurry and the crystalline particles is 10:3:1.

[0056] The treated crystallized particles are mixed evenly with the remaining centrifuged slurry to complete the royal jelly impurity removal process and obtain 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. At this time, the impurity removal process does not include step (1). Step (2) is: placing fresh royal jelly in a microbubble flotation device, passing nitrogen gas 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 ℃, the flotation time is 10 min, and after the flotation is completed, the surface impurities are scraped off to obtain the flotated royal jelly.

[0058] Comparative Example 2 The difference between this comparative example and Example 1 is that microbubble flotation is not used in the royal jelly impurity removal process; only adsorption materials are used for adsorption. In this case, the impurity removal process includes the following steps: (1) Take a clean loofah sponge (thickness 3 cm, porosity ≥90%) and immerse it in a beeswax-ethanol solution with a concentration (i.e., the mass percentage of beeswax) of 12% for 40 min. The immersion temperature is 40 ℃. After immersion, evaporate the ethanol and then cool it at 3 ℃ and sterilize it with ultraviolet light to obtain the impurity removal adsorption material. (2) The impurity removal adsorption material obtained in step (1) is stirred evenly with fresh royal jelly for impurity adsorption. The adsorption temperature is 8 ℃ and the adsorption time is 10 min. After the adsorption is completed, the impurity removal adsorption material is taken out to obtain the royal jelly after flotation. The amount of impurity removal adsorption material added is 3% of the volume of royal jelly.

[0059] (3) The royal jelly after flotation is centrifuged at a speed of 2500 r / min, a temperature of 4 ℃, and a time of 5 min to obtain centrifuged slurry and precipitate. The precipitate is washed with 20 times the amount of water, allowed to stand and separate into layers, and the bottom impurities are discarded to obtain crystalline particles (mainly containing 10-HDA crystals). The crystalline particles are mixed evenly with the centrifuged 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 loofah sponge in step (1) of the royal jelly impurity removal process is replaced with activated carbon.

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

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

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

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

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

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

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

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

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

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

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

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

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

[0074] Comparative Example 17 The difference between this comparative example and Example 7 is that when treating the crystal particles in step (3) of the royal jelly impurity removal process, step S1 is not included. That is, the crystal particles are treated as follows: take the upper layer of the centrifuged slurry, spray it onto the surface of the crystal particles, cool it to -15 ℃ and keep it for 2 hours after spraying, and the treated crystal particles are obtained.

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

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

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

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

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

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

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

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

[0083] I. Quality Inspection of Royal Jelly Obtained by the Impurity Removal Process of the Present Invention In accordance with the requirements of GB9697 "Royal Jelly", the quality of the fresh royal jelly used in this invention and the royal jelly obtained by the impurity removal process in Examples 1-9 were tested, and the results are shown in Table 1 below. The fresh royal jelly used in Examples 1 and 4-9 was the same, designated as ①, and the fresh royal jelly used in Examples 2-3 was the same, designated as ②.

[0084] Table 1

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

[0086] Compared with Examples 1 and 2, Examples 3 (fresh royal jelly with an acidity of 35 mL / 100g, and the beeswax used was medium-grade beeswax) and 4 (fresh royal jelly with an acidity of 50 mL / 100g, and the beeswax used was western-grade beeswax) did not select the type of beeswax according to the different acidities of fresh royal jelly in accordance with the present invention. As a result, the removal effect of impurities such as broken wax pieces and larvae was reduced, which affected the subsequent removal effect of impurities such as dust, resulting in an increase in ash content and an increase in the loss of 10-hydroxy-2-decenoic acid.

[0087] II. Comparison of the effects of the impurity removal process of the present invention 1. Effectiveness in removing impurities such as broken wax fragments and larvae. Fresh royal jelly was purified according to the processes of Examples 1-9 and Comparative Examples 1-11 of this invention. The royal jelly obtained in different steps was observed under a microscope to see if there were any impurities such as broken wax fragments and larvae. The results are shown in Table 2.

[0088] The evaluation is based on the area percentage of impurities: No obvious impurities: Level 0; Impurities area percentage 1-5%: Level 1; Impurities area percentage 6-10%: Level 2; Impurities area percentage 11-15%: Level 3; Impurities area percentage 16-20%: Level 4; Impurities area percentage 21-30%: Level 5; Impurities area percentage 31-40%: Level 6; Impurities area percentage 41-50%: Level 7; Impurities area percentage 51-60%: Level 8; Impurities area percentage 61-80%: Level 9; Impurities area percentage 81-100%: Level 10.

[0089] Table 2

[0090] As shown in Table 2, compared with fresh royal jelly, the royal jelly impurity 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. In particular, the royal jelly obtained by the impurity removal process of Examples 6-9 did not show obvious impurities such as broken wax flakes and larvae.

[0091] Compared with Examples 1 and 2, Examples 3 (fresh royal jelly with an acidity of 35 mL / 100g, and the beeswax used was medium-grade beeswax) and 4 (fresh royal jelly with an acidity of 50 mL / 100g, and the beeswax used was western-grade 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 their impurity removal effect was reduced.

[0092] Based on Example 1, Examples 5-9 used beeswax with different concentrations twice when impregnating the loofah sponge with beeswax solution, which improved the impurity removal effect.

[0093] Compared with Example 1, Comparative Examples 1-11 changed the impurity removal process steps, resulting in a decrease in impurity removal effect.

[0094] 2. Effectiveness in removing dust and other impurities In accordance with the requirements of GB9697 "Royal Jelly", the ash content of the royal jelly obtained by the impurity removal process in Example 1 and Comparative Examples 12-15 was tested, and the results are shown in Table 3.

[0095] Table 3

[0096] As shown in Table 3, compared with Example 1, Comparative Examples 12-15 changed the centrifugal separation conditions, which affected the removal of impurities such as sand and dust, and increased the ash content in royal jelly.

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

[0098] Table 4

[0099] As shown in Table 4, the 10-HDA loss is relatively small in the microbubble flotation processes of Examples 1-2 and 5-9 of this invention. Compared with Examples 1 and 2, Examples 3 and 4 did not select the beeswax type according to the different acidities of fresh royal jelly as per this invention, and the 10-HDA loss also increased.

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

[0101] III. Changes in royal jelly obtained by the impurity removal process of this invention at different storage times To improve the dispersion stability and incorporation of 10-HDA in royal jelly, this invention further treats the resulting crystalline particles (mainly containing 10-HDA crystals) after centrifugal separation to remove dust. Comparing the 10-HDA content in royal jelly after the impurity removal process in Table 1 with the 10-HDA content in royal jelly after the microbubble flotation process in Table 4, it can be seen that the treatment step of this invention on the crystalline particles (mainly containing 10-HDA crystals) has a low impact on the 10-HDA content and does not result in significant 10-HDA loss.

[0102] 1. Changes in 10-HDA content in royal jelly under different storage times The royal jelly obtained according to the impurity removal process of Examples 6-9 and Comparative Examples 16-25 of this invention was tested for the changes in 10-HDA content under the same storage temperature of -18℃ 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 after 28 days, the treatment of crystalline particles (mainly containing 10-HDA crystals) in Examples 6-9 of this invention improved the storage stability of 10-HDA content in royal jelly. The 10-HDA loss rate under storage conditions of -18℃ for 28 days was significantly reduced, ranging from 3.92% to 13.79%. This indicates that the royal jelly impurity removal process of this 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 royal jelly gradually decreased with the extension of storage time, indicating a decrease in storage stability.

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

[0107] The evaluation is based on the amount of crystals appearing in royal jelly: no obvious crystals: grade 0; slight crystals: grade 1; moderate amount of crystals: grade 2; more crystals: grade 3.

[0108] Table 6

[0109] As shown in Table 6, compared with fresh royal jelly, the treatment of crystalline particles (mainly containing 10-HDA crystals) in Examples 6-9 of this invention improved the storage stability of royal jelly. The number of visible crystals was significantly reduced under storage conditions of 2 °C and 28 days, and the grainy texture was reduced. In particular, Examples 7-9 showed better results.

[0110] Compared with Example 7, Comparative Examples 16-25 changed the processing steps for the crystallized particles. As a result, the number of visible crystals in the royal jelly gradually increased with the extension of storage time, the particle texture increased, and the storage stability decreased.

[0111] Finally, it should be noted that the above description is merely 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 foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A process for the removal of impurities from royal jelly, characterized in that: Includes the following steps: (1) Take a lightweight three-dimensional mesh material, immerse it in a beeswax-ethanol solution, evaporate the ethanol after immersion, then cool and sterilize to obtain the impurity removal adsorption material. (2) Spread the impurity removal adsorption material obtained in step (1) on the surface of fresh royal jelly, and then pass nitrogen gas through it for microbubble flotation. After the flotation is completed, remove the impurity removal adsorption material to obtain the royal jelly after flotation. (3) Centrifuge the royal jelly after flotation to obtain centrifuged slurry and precipitate. Wash the precipitate with water, let it stand to separate into layers, discard the bottom impurities to obtain crystalline particles, mix the crystalline particles with the centrifuged slurry evenly, and it is ready. In step (1), when the acidity of fresh royal jelly is 30-40 mL / 100g, the beeswax used is Western beeswax; when the acidity of fresh royal jelly is 41-53 mL / 100g, the beeswax used is Chinese beeswax.

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 a synthetic 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 of claim 1, characterized in that: In step (1), the concentration of the beeswax-ethanol solution is 5-20%, the impregnation time is 30-50 min, and the impregnation temperature is 30-50 ℃.

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

5. The process of claim 1, characterized in that: In step (3), the centrifugation speed is 2000-3000 r / min, the temperature is 3-6 ℃, and the time is 3-6 min.

6. The process of claim 1, characterized in that: Before centrifuging the royal jelly after flotation in step (3), it is necessary to perform cold storage treatment. The cold storage temperature is 1-3 ℃ and the cold storage time is 10-30h.

7. The process according to any one of claims 1 to 6, characterized in that: Step (3) also includes the following treatment of the crystalline particles: S1. Take the lower layer of the centrifuged slurry, freeze and grind it into particles 1, take the crystalline particles and mix them with ethanol, then spray them onto the surface of particles 1. After spraying, evaporate the ethanol under reduced pressure 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)℃ and keep it for 1-3 hours.

8. The process of claim 2, wherein: In step (1), the impregnation process includes: first, impregnating in a 5-10% beeswax-ethanol solution for 10-20 min at an impregnation temperature of 30-40 ℃, then evaporating the ethanol, and then impregnating in a 15-20% beeswax-ethanol solution for 20-30 min at an impregnation temperature of 40-50 ℃.

9. The process of claim 7, characterized in that: The mass ratio of the lower slurry, the upper slurry, and the crystallized particles is (5-10):(0.5-3):1, and the particle size of the particles 1 is 10-60 μm.

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