Ultramicro-grade antler powder and preparation method thereof
By sonicating and freezing the red deer antler powder and ethanol solution, the uneven quality of the red deer antler powder was solved, and ultrafine powders containing rich amino acids and phospholipids were prepared, which improved the efficacy and safety of the medicine. A systematic quality evaluation system has been established.
Patent Information
- Application Number
- CN202411570255.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-06
- Publication Date
- 2024-12-17
AI Technical Summary
The existing red deer antler powder has uneven quality, poor efficacy, and the preparation process and animal sources affect the efficacy of the drug. The lack of a systematic quality evaluation system leads to safety and effectiveness issues.
The red deer antlers were sliced and dried and ground into coarse powder, mixed with ethanol solution for ultrasonic treatment and lyophilization to prepare ultramicro-grade red deer antler powder. By adjusting the ethanol solution ratio, ultrasonic frequency and lyophilization temperature, the particle size and composition of the powder were controlled. , ensure the stability and efficacy of the product.
The prepared ultra-micro-grade red antler powder is powdery, has a low moisture content, an appropriate pH value, and a uniform particle size. It contains a large amount of amino acids, proteins and phospholipids, with good quality, which improves the efficacy and bioavailability.
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Figure CN119139352A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of deer product processing, and in particular relates to ultra-fine red deer antler powder and a preparation method thereof. Background Art
[0002] Since Chinese medicine powder can be used to prepare other preparations, or can be taken directly with boiled water or medicinal soup or decocted with other medicines, it is widely used for its characteristics of improving effective utilization, saving medicinal resources, and flexible compatibility. Red deer antler powder is also included in it. However, most of the red deer antler products on the market are roughly processed and the product quality is uneven. The time when the antlers are collected is also unclear. Its processing technology, quality and animal source will have a serious impact on its efficacy. Therefore, it is urgent to develop a more efficient red deer antler powder preparation process and establish a systematic quality evaluation system to ensure the safety and effectiveness of red deer antler powder as a health product. Summary of the invention
[0003] In view of this, the object of the present invention is to provide an ultra-fine red deer antler powder and a preparation method thereof, so as to solve the technical problems of uneven quality and poor efficacy of existing red deer antler powder.
[0004] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:
[0005] The present invention provides a method for preparing ultrafine red deer antler powder, comprising the following steps:
[0006] The antler slices of red deer are dried and ground to obtain coarse powder; the coarse powder is mixed with an ethanol solution, filtered after ultrasonication, and the filtrate obtained by lyophilization is obtained to obtain ultrafine red deer antler powder;
[0007] The volume fraction of the ethanol solution is 90-98%;
[0008] The mass volume ratio of the coarse powder and the ethanol solution is 1g:8-12mL.
[0009] Preferably, the mesh size of the coarse powder is 250-350 meshes.
[0010] Preferably, the frequency of the ultrasound is 70 to 90 KHZ, and the time of the ultrasound is 10 to 20 minutes.
[0011] Preferably, the freeze-drying temperature is -45°C to -35°C, and the freeze-drying time is 1 to 3 days.
[0012] The invention also provides ultra-fine red deer antler powder prepared by the preparation method.
[0013] Compared with the prior art, the present invention has the following beneficial effects:
[0014] The red deer antler powder obtained by the invention through grinding, ultrasonic treatment, freeze drying and the like is in powder form, light yellow in color, and has a water content of 0.9274%. The pH value of the ultrafine red deer antler powder is 7.66, the average volume is 475.3nm, the PDI is 0.159, the main element contained in the ultrafine red deer antler powder is carbon (C), some inorganic elements such as Na, Cl and K, etc., and a large amount of amino acids, protein substances and phospholipid components are also contained, the quality is good, and the drug effect is fully exerted. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] Figure 1 This is a visual picture of 300 mesh red deer antler powder;
[0016] Figure 2 This is the element analysis chart of ultra-fine red deer antler powder;
[0017] Figure 3 This is the X-ray diffraction result of ultra-fine red deer antler powder;
[0018] Figure 4 This is the Fourier transform infrared spectrum of ultra-fine red deer antler powder. DETAILED DESCRIPTION
[0019] The present invention provides a method for preparing ultrafine red deer antler powder, comprising the following steps:
[0020] The antlers of red deer are sliced, dried, and ground to obtain coarse powder; the coarse powder is mixed with an ethanol solution, filtered after ultrasonication, and the filtrate obtained by lyophilization to obtain ultrafine red deer antler powder.
[0021] In the present invention, the antler slices of red deer are dried and then ground to obtain coarse powder; the thickness of the slices is preferably 1-2 mm, more preferably 1.5 mm; the drying method is air-drying at room temperature, and the air-drying time is preferably 2-3 days, more preferably 2.5 days; the grinding method is machine (high-speed crusher) grinding; the mesh size of the coarse powder is preferably 250-350 meshes, more preferably 280-320 meshes;
[0022] After obtaining the coarse powder, the present invention mixes the coarse powder with an ethanol solution. The volume fraction of the ethanol solution is preferably 90 to 98%, and more preferably 92 to 96%. The mass volume ratio of the coarse powder to the ethanol solution is preferably 1 g: 8 to 12 mL, and more preferably 1 g: 9 to 11 mL.
[0023] In the present invention, the frequency of the ultrasound is preferably 70-90KHZ, more preferably 75-85KHZ; the time of the ultrasound is preferably 10-20min, more preferably 12-18min; the ultrasound can dissolve the drug in the solution to form a stable solution, improve the bioavailability and efficacy of the drug, and reduce the dosage and side effects. In addition, ultrasound can also prepare more stable and uniform drug particles, thereby achieving better therapeutic effects; the filtering method is to use polytetrafluoroethylene (PTFE) microporous membrane filtration; the freeze-drying temperature is preferably -45℃~-35℃, more preferably -42℃~-38℃; the freeze-drying time is preferably 1-3d, more preferably 2 days.
[0024] The invention also provides ultra-fine red deer antler powder prepared by the preparation method.
[0025] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.
[0026] Example 1
[0027] The antlers of red deer are collected, and after removing impurities, sliced, the slices are sliced to a thickness of 1.5 mm, aired at room temperature for 2.5 days until dry, and ground by a high-speed grinder to obtain 300-mesh red deer antler powder. The 300-mesh red deer antler powder is dissolved in a 95% ethanol solution, the mass volume ratio of the antler powder to the ethanol solution is 1 g: 10 mL, and after ultrasonic (80KHZ) treatment for 15 minutes, the antler powder is filtered with a polytetrafluoroethylene (PTFE) microporous filter membrane, and the filtrate obtained by filtration is placed in a freeze dryer at a temperature of -40°C and freeze-dried for 2 days to obtain ultra-fine red deer antler powder.
[0028] Example 2
[0029] The antlers of red deer are collected, and after removing impurities, sliced, the slices are sliced to a thickness of 1 mm, dried in the sun at room temperature for 2 days, and ground by a high-speed grinder to obtain 250-mesh antler powder. The 250-mesh antler powder is dissolved in a 90% ethanol solution, the mass volume ratio of the antler powder to the ethanol solution is 1 g: 8 mL, and after being treated with ultrasound (70KHZ) for 10 minutes, the antler powder is filtered with a polytetrafluoroethylene (PTFE) microporous filter membrane, and the filtrate obtained by filtration is placed in a freeze dryer at a temperature of -35°C and freeze-dried for 1 day to obtain ultra-fine red deer antler powder.
[0030] Example 3
[0031] The antlers of red deer are collected, and after removing impurities, sliced, the slices are sliced to a thickness of 2 mm, aired at room temperature for 3 days until dry, and ground by a high-speed grinder to obtain 350-mesh antler powder. The 350-mesh antler powder is dissolved in a 98% ethanol solution, the mass volume ratio of the antler powder to the ethanol solution is 1 g: 12 mL, and after being treated with ultrasound (90KHZ) for 20 minutes, the antler powder is filtered with a polytetrafluoroethylene (PTFE) microporous filter membrane, and the filtrate obtained by filtration is placed in a freeze dryer at a temperature of -45°C and freeze-dried for 3 days to obtain ultra-fine red deer antler powder.
[0032] Experimental Example 1
[0033] The quality of the ultrafine red antler powder was evaluated by detecting the morphology, moisture content, pH value, particle size and size distribution, elemental analysis, X-ray diffraction and Fourier transform infrared (FT-IR) spectroscopy of the ultrafine red antler powder prepared in Example 1.
[0034] 1. Red deer antler powder form
[0035] like Figure 1 As shown, 300 mesh red deer antler powder is powdery and light yellow.
[0036] 2. Water content of red deer antler powder
[0037] The red deer antler powder is heated by the drying method to evaporate the water in the sample, and then the water content of the red deer antler powder is calculated by weighing the mass difference of the sample.
[0038] Experimental results: The water content of red deer antler powder is 0.9274%.
[0039] 3. pH value of ultra-fine red deer antler powder
[0040] The ultrafine deer antler powder aqueous solution was prepared by mixing deer antler powder and distilled water in a mass volume ratio of 1:10, and the pH value of the ultrafine deer antler powder was detected by an acidity meter.
[0041] Experimental results: The pH value of ultra-fine red deer antler powder is 7.66.
[0042] 4. Ultrafine red deer antler powder particle size and size distribution
[0043] The particle size of ultra-fine red antler powder is tested by Malvern, and the average volume of ultra-fine red antler powder should be <1μm.
[0044] Experimental results: as shown in Table 1.
[0045] Table 1 Particle size and size distribution of ultrafine red deer antler powder
[0046]
[0047] As shown in Table 1, the average volume of ultra-fine red deer antler powder is 475.3nm and the PDI is 0.159.
[0048] 5. Elemental analysis of ultra-fine red deer antler powder
[0049] The main elements contained in ultra-fine red deer antler powder were detected by EDS energy spectrum analyzer.
[0050] Experimental results: Figure 2 As shown in the figure, the main element contained in the ultra-fine red deer antler powder is carbon (C), as well as some inorganic elements such as Na, Cl and K.
[0051] 6. X-ray diffraction of ultra-fine red deer antler powder
[0052] The overall identification method of X-ray diffraction was used to intuitively observe the geometric topological patterns of the XRD patterns of red deer antler powder.
[0053] Experimental results: Figure 3 As shown, using the overall identification method of X-ray diffraction, the XRD pattern of red deer antler powder is intuitively observed to be 2 θ There are several peaks between 22° and 68°. θ The diffraction peaks of red deer antler powder were found at =25.82°, 31.90°, 39.78°, 46.70°, 49.45°, 53.12° and 64.06°.
[0054] 7. Fourier transform infrared spectrum of ultra-fine red deer antler powder
[0055] The main absorption peaks of ultra-fine red deer antler powder were analyzed by Fourier transform infrared spectroscopy.
[0056] Experimental results: Figure 4 As shown in Figure 2, the main absorption peaks of ultra-fine red deer antler powder include: wave number 3300cm -1 Strong broad peaks in the vicinity; wave number 2930cm -1 、2850cm -1 Nearby methylene absorption peak; wave number 1650cm -1 、1540cm -1 Strong absorption peaks of amide I band and amide II band nearby; wave number 1242cm -1 、1030cm -1 There are two obvious sugar vibration peaks nearby. 1650cm -1 、1540cm -1 The skeleton vibration peak is attached to the corresponding 3300cm -1The strong and broad -NH2 antisymmetric stretching vibration peak at 560cm indicates that they contain a large amount of amino acids and protein substances. The characteristic peak intensity of red deer antler powder at this position is relatively strong, indicating that its amino acid content is high. -1 There is a strong and sharp absorption peak at 600 cm -1 The shoulder peak appears at 870cm -1 The weak absorption peak that appears at 4° indicates that red deer antler powder also contains a large amount of phospholipids.
[0057] It can be seen from the above embodiments and experimental examples that the red deer antler powder prepared by the present invention contains the main element carbon (C), as well as some inorganic elements such as Na, Cl and K, and also contains a large amount of amino acids, protein substances and phospholipid components, and has good quality, which is conducive to the full play of the medicinal effect.
[0058] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.
Claims
1. A method for preparing ultrafine red deer antler powder, characterized in that: The following steps are involved: The antler slices of red deer are dried and ground to obtain coarse powder; the coarse powder is mixed with an ethanol solution, filtered after ultrasonication, and the filtrate obtained by lyophilization is obtained to obtain ultrafine red deer antler powder; The volume fraction of the ethanol solution is 90-98%; The mass volume ratio of the coarse powder and the ethanol solution is 1g:8-12mL.
2. The preparation method according to claim 1, characterized in that: The mesh number of the coarse powder is 250 to 350 meshes.
3. The preparation method according to claim 1, characterized in that: The frequency of the ultrasound is 70 to 90 KHZ, and the time of the ultrasound is 10 to 20 minutes.
4. The preparation method according to claim 1, characterized in that: The freeze-drying temperature is -45°C to -35°C, and the freeze-drying time is 1 to 3 days.
5. The ultrafine red deer antler powder prepared by the preparation method according to any one of claims 1 to 4.