A drying method for deer blood freeze-dried powder
By employing a multi-stage, precisely controlled drying method, the problem of excessively high residual moisture in freeze-dried deer blood was solved, thereby improving the quality of freeze-dried products and ensuring product consistency.
Patent Information
- Application Number
- CN202510751034.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-06
- Publication Date
- 2026-01-06
- Estimated Expiration
- 2045-06-06
AI Technical Summary
Existing technologies lack methods for detecting the residual moisture and porosity of freeze-dried deer blood, resulting in excessively high residual moisture, which affects the quality of freeze-dried deer blood.
A complete quality control closed loop is formed through a multi-stage, precisely controlled drying method, including pretreatment, low-temperature freezing, detection of ice crystal size and uniformity, detection of moisture residue and porosity, and feedback adjustment of rehydration performance.
This has resulted in a comprehensive improvement in freeze-dried product quality, increased red blood cell recovery rate, reduced freezing energy consumption, and ensured consistent product quality and high standards.
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Figure CN120549874B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of deer blood freeze-drying technology, and more particularly to a drying method for deer blood freeze-dried powder. Background Technology
[0002] Deer blood is widely known in folk medicine and is considered a top-grade herb. As early as the Song Dynasty, there were records of people drinking deer blood after pricking their skin, resulting in plump and healthy skin. Li Shizhen of the Ming Dynasty conducted a more detailed study on the medicinal effects of deer blood, recording in his *Compendium of Materia Medica* that it greatly replenishes deficiencies, nourishes essence and blood, and detoxifies smallpox and other poisons. He also suggested that for effective consumption, it is best to pricking the blood between the antlers of a deer and drinking it with wine. The Qing imperial family further embraced this practice. According to Xu Ke's *Qing Dynasty Anecdotes*, Emperor Wenzong suffered from many illnesses and a sallow complexion. Doctors advised him to drink deer blood, so he raised over a hundred deer and ordered daily blood collection. When the Anglo-French allied forces entered Beijing, Emperor Xianfeng suffered a severe attack of cough and ordered deer blood for his supply. However, it was unavailable in time, and he subsequently died. In modern times, animal experiments and clinical studies have proven that deer blood does indeed possess multiple therapeutic and health-promoting effects, including beautifying the complexion, treating anemia, regulating immunity, delaying aging, improving memory, combating fatigue, and improving sexual function.
[0003] Chinese Patent Publication No. CN116440167A discloses a method for producing freeze-dried deer blood powder, comprising the following steps: preparing a blood anticoagulant solution, and then placing 0.2%-0.8% of the blood mass of the blood anticoagulant solution in a mixing tank for later use; collecting fresh deer blood using blood collection equipment, and then testing and analyzing the collected fresh deer blood to determine whether the fresh deer blood meets the requirements for use; adding the tested and qualified fresh deer blood to the mixing tank containing the blood anticoagulant solution, and then adding high-proof pure grain liquor to the mixing tank, followed by using a mixer to homogenize and stir the blood anticoagulant solution, fresh deer blood, and high-proof pure grain liquor. In this invention, pure water is added to the fresh deer blood, and emulsification technology is used to emulsify the mixture of fresh deer blood and pure water. Cell wall breaking and concentration are performed on the mixture of fresh deer blood and pure water using a cell wall breaking machine, which ultimately increases the content of effective components in the freeze-dried deer blood powder product to a certain extent.
[0004] It is evident that the existing technology has the following problems: due to the lack of means to detect the residual moisture and porosity of freeze-dried deer blood, the residual moisture is too high, which affects the quality of freeze-dried deer blood. Summary of the Invention
[0005] Therefore, the present invention provides a drying method for freeze-dried deer blood powder to overcome the problem in the prior art that the lack of means to detect the residual moisture and porosity of freeze-dried deer blood leads to excessively high residual moisture, which affects the quality of freeze-dried deer blood.
[0006] To achieve the above objectives, the present invention provides a drying method for freeze-dried deer blood powder, comprising the following steps:
[0007] Deer blood is pretreated to obtain clarified blood, and the clarified blood is then subjected to low-temperature freezing to obtain frozen deer blood. The actual ice crystal size of the frozen deer blood is detected, and the freezing rate is adjusted based on the actual ice crystal size.
[0008] If the ice crystal size meets the drying requirements, the ice crystal uniformity of the frozen deer blood is tested to obtain the actual ice crystal uniformity. The actual ice crystal uniformity is compared with the standard ice crystal uniformity range to determine whether the frozen deer blood should be initially sublimated.
[0009] The freeze-dried deer blood after the first sublimation was tested for residual moisture and porosity. The determination of whether to perform a second sublimation was based on the residual moisture and porosity.
[0010] The rehydration properties of freeze-dried deer blood after the second sublimation were tested to obtain the rehydration time and rehydration rate. Based on the rehydration time and rehydration rate, it was determined whether to adjust the heating rate of the first sublimation.
[0011] The actual ice crystal uniformity includes ice crystal size uniformity and ice crystal spatial uniformity.
[0012] Furthermore, the process of cryogenically freezing the clarified blood to obtain frozen deer blood includes,
[0013] Clarified blood is placed in a pre-specified deer blood freezing tray, and the clarified blood is frozen based on the initial freezing thickness to obtain frozen deer blood;
[0014] The initial frozen thickness is determined based on the heat conduction efficiency of the clarified blood.
[0015] Furthermore, the process of determining whether to adjust the freezing rate based on the actual ice crystal size includes,
[0016] By comparing the actual ice crystal size with the standard ice crystal size range, an ice crystal comparison result is obtained, and the freezing rate is determined based on the ice crystal comparison result.
[0017] The standard ice crystal size range is determined based on the average diameter of clear blood cells.
[0018] Furthermore, the process of obtaining the actual ice crystal uniformity by detecting the ice crystal uniformity of frozen deer blood includes,
[0019] Take out the flat deer blood plate, divide the flat deer blood plate evenly to obtain several deer blood plates to be tested, select several deer blood plates to be tested from each test area, and test the ice crystal uniformity of the deer blood plates to be tested to obtain the actual ice crystal uniformity.
[0020] The flat deer blood plate is the frozen deer blood in the freezing tray after freezing. The area to be tested includes the central area of the flat deer blood plate and other areas surrounding the central area.
[0021] Furthermore, the process of obtaining the actual ice crystal uniformity by detecting the ice crystal uniformity of the deer blood plate to be tested includes,
[0022] The deer blood plate to be tested is subjected to low-temperature slicing to obtain deer blood plate slices. The shape and length of the ice crystals in the deer blood plate slices are analyzed, and the uniformity of ice crystal size is determined based on the ice crystal area and ice crystal length.
[0023] The ice crystal shape includes dispersed ice crystals and rounded ice crystals, and the ice crystal length is the longest possible length of a single ice crystal.
[0024] Furthermore, the process of obtaining the actual ice crystal uniformity by detecting the ice crystal uniformity of the deer blood plate to be tested includes,
[0025] Select and test deer blood plate slices in different test areas to obtain several ice crystal size uniformity values. Compare the ice crystal size uniformity values to obtain the actual ice crystal uniformity difference value. Based on the comparison between the actual ice crystal uniformity difference value and the standard ice crystal uniformity difference value, determine whether to perform initial sublimation on the frozen deer blood.
[0026] The ice crystal uniformity difference value is determined based on the average cell diameter.
[0027] Furthermore, the process of testing the residual moisture and porosity of the freeze-dried deer blood after the initial sublimation includes,
[0028] The moisture content of the middle and edge regions of freeze-dried deer blood is detected by infrared spectroscopy, and the average value is taken to obtain the actual moisture content. Freeze-dried deer blood in the test area after the first sublimation is selected and sliced to obtain freeze-dried deer blood slices. The channel area of the freeze-dried deer blood slices is detected, and the need for secondary sublimation is determined based on the channel area ratio and the actual moisture content.
[0029] The channel area ratio is the ratio of the channel area to the surface area of the freeze-dried slice.
[0030] Furthermore, the process of testing the rehydration properties of freeze-dried deer blood after the second sublimation to obtain the rehydration time and rehydration rate includes the following steps:
[0031] Place the freeze-dried deer blood blocks into purified water at a preset temperature, calculate the rehydration time by measuring the time required for the freeze-dried deer blood blocks to completely dissolve in the purified water, place freeze-dried deer blood blocks of the same batch into purified water, remove the freeze-dried deer blood blocks according to the preset rehydration absorption time, and determine the rehydration rate by the ratio of the weight of the dry freeze-dried deer blood blocks before being placed into purified water to the weight of the rehydrated freeze-dried blocks after being placed into purified water.
[0032] Furthermore, the process of determining whether to adjust the heating rate of the initial sublimation based on the rehydration time and the rehydration rate includes:
[0033] An actual heating rate evaluation value is generated based on the rehydration time and rehydration rate. The heating rate evaluation value is compared with the standard heating rate evaluation value range to obtain a heating rate evaluation value comparison result. Based on the heating rate evaluation value comparison result, it is determined whether to adjust the heating rate of the initial sublimation.
[0034] The standard heating rate evaluation range is determined based on historical data of deer blood freeze-drying.
[0035] Furthermore, the process of determining whether to adjust the initial sublimation heating rate based on the comparison results of the heating rate evaluation values includes:
[0036] If the heating rate evaluation value is less than the minimum value of the standard heating rate evaluation value range, the heating rate is increased according to the difference between the minimum value of the standard heating rate evaluation value range and the heating rate evaluation value.
[0037] If the heating rate evaluation value is within the standard heating rate evaluation value range, maintain the original heating rate.
[0038] If the heating rate evaluation value is greater than the maximum value of the standard heating rate evaluation value range, the heating rate is reduced based on the difference between the heating rate evaluation value and the maximum value of the standard heating rate evaluation value range.
[0039] Compared with existing technologies, the advantages of this invention lie in its comprehensive improvement of freeze-dried quality through multi-stage precise control. In the pretreatment stage, a gradient centrifugation combined with low-temperature settling clarification process is employed to improve red blood cell recovery rate. Simultaneously, heat conduction is optimized using 316 stainless steel freezing trays. A four-fold detection mechanism is introduced: dynamic control of ice crystal size, dual-index evaluation of uniformity, coordinated determination of moisture and porosity, and feedback adjustment of rehydration performance, forming a complete quality control closed loop. Furthermore, the initial freezing thickness, determined based on heat conduction efficiency, increases production capacity while reducing freezing energy consumption.
[0040] Furthermore, the process of determining the initial freezing thickness through heat conduction efficiency can maximize the initial freezing thickness when freezing deer blood, thereby improving freezing efficiency and increasing the utilization rate of the deer blood holding freezing tray.
[0041] Furthermore, determining the standard ice crystal size range by clarifying the average diameter of blood cells can prevent ice crystals that are too large from piercing the cell wall. At the same time, it can also prevent the formation of intracellular ice crystals due to insufficient water exudation caused by excessively small intracellular ice crystals during freezing.
[0042] Furthermore, uniformly dividing the flat deer blood plate into different test areas enables the detection of ice crystal size uniformity in different test areas, avoiding misjudgment of the actual ice crystal uniformity of the flat deer blood plate, and increasing drying efficiency. By making a preliminary judgment on the ice crystal shape of the deer blood plate slices to be tested, areas where the ice crystal size uniformity does not meet the standard can be quickly identified, thereby improving drying efficiency. By observing and calculating the ice crystal area and ice crystal length of 10 fields of view of the deer blood plate slices to be tested, the corresponding ice crystal size uniformity can be obtained, further refining the detection of ice crystal size uniformity in the test area and improving the effect of freeze-drying deer blood.
[0043] Furthermore, rigorous testing of ice crystal size uniformity and regional identification ensures that the quality of the freeze-dried deer blood powder meets high standards. Defective deer blood plate slices are promptly identified and disposed of to prevent them from entering subsequent production processes. Clearly defined acceptance / disapproval criteria for different regions help optimize the production process, improve production efficiency, and enhance product quality consistency.
[0044] Furthermore, this technical solution demonstrates significant advantages in quality control of deer blood freeze-drying by establishing a dual-index detection system for moisture residue and porosity. Fourier transform infrared spectroscopy is used to detect moisture in the central and edge regions of the freeze-dried product. The actual moisture residue (6.25%) is calculated by the difference between a preset light intensity (0.4) and the measured absorption peak intensity (0.38), and a compensation parameter calibrated from historical data (As=1.25) is introduced to ensure measurement accuracy. Simultaneously, microscopic image analysis technology is used to quantify the channel area ratio (0.9) of the freeze-dried skeleton. By setting threshold standards for the highest moisture residue (8%) and the lowest channel area ratio (0.85), accurate secondary sublimation determination is achieved. Dual-parameter collaborative detection can comprehensively evaluate freeze-drying quality; the dynamic compensation mechanism controls moisture calculation errors.
[0045] Furthermore, this technical solution achieves precise control of the deer blood freeze-drying process by establishing a quantitative correlation model between rehydration performance and freeze-drying process parameters. Rehydration time and rehydration rate are used as core evaluation indicators and converted into heating rate evaluation values. When the heating rate evaluation value is less than the minimum value of the standard heating rate evaluation value range, the heating rate is increased based on the difference between the minimum value and the heating rate evaluation value. This avoids insufficient heating rate leading to incomplete sublimation of ice crystals, causing water to recondense inside the freeze-dried deer blood, forming localized liquid water. Slow heating prolongs ice crystal growth time, resulting in excessively large ice crystals that puncture deer blood cells and affect product quality. Conversely, when the heating rate evaluation value is greater than the maximum value of the standard heating rate evaluation value range, the heating rate is decreased based on the difference between the two values. This avoids rapid heating causing the surface of the freeze-dried deer blood to dry and form a hard shell, hindering the escape of water vapor from the sublimation of internal ice crystals. Attached Figure Description
[0046] Figure 1 This is a flowchart of the drying method for freeze-dried deer blood powder in this embodiment;
[0047] Figure 2 This is a flowchart of the deer blood pretreatment method for the drying method of deer blood freeze-dried powder in this embodiment;
[0048] Figure 3 This is a flowchart illustrating the process for determining the quality of the flattened deer blood plate used in the drying method for deer blood freeze-dried powder in this embodiment.
[0049] Figure 4 This is a flowchart illustrating the process of adjusting the heating rate in the drying method for deer blood freeze-dried powder in this embodiment. Detailed Implementation
[0050] To make the objectives and advantages of the present invention clearer, the present invention will be further described below with reference to embodiments; it should be understood that the specific embodiments described herein are merely for explaining the present invention and are not intended to limit the present invention.
[0051] Preferred embodiments of the present invention will now be described with reference to the accompanying drawings. Those skilled in the art should understand that these embodiments are merely illustrative of the technical principles of the present invention and are not intended to limit the scope of protection of the present invention.
[0052] It should be noted that in the description of this invention, the terms "upper", "lower", "left", "right", "inner", "outer", etc., which indicate the direction or positional relationship, are based on the direction or positional relationship shown in the drawings. This is only for the convenience of description and is not intended to indicate or imply that the device or element must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, it should not be construed as a limitation of this invention.
[0053] Furthermore, it should be noted that, in the description of this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.
[0054] Please see Figures 1-4 As shown, Figure 1 This is a flowchart of the drying method for freeze-dried deer blood powder in this embodiment; Figure 2 This is a flowchart of the deer blood pretreatment method for the drying method of deer blood freeze-dried powder in this embodiment; Figure 3 This is a flowchart illustrating the process for determining the quality of the flattened deer blood plate used in the drying method for deer blood freeze-dried powder in this embodiment. Figure 4 This is a flowchart illustrating the process of adjusting the heating rate in the drying method for deer blood freeze-dried powder in this embodiment.
[0055] This embodiment provides a drying method for freeze-dried deer blood powder, including the following steps:
[0056] Step S1: Pre-treat the deer blood to obtain clarified blood, freeze the clarified blood at low temperature to obtain frozen deer blood, detect the actual ice crystal size of the frozen deer blood, and determine whether to adjust the freezing rate based on the actual ice crystal size.
[0057] Step S2: If the ice crystal size meets the drying requirements, the ice crystal uniformity of the frozen deer blood is detected to obtain the actual ice crystal uniformity. The actual ice crystal uniformity is compared with the standard ice crystal uniformity range to determine whether the frozen deer blood should be initially sublimated.
[0058] Step S3: The freeze-dried deer blood after the first sublimation is subjected to moisture residue test and porosity test. Based on the moisture residue and porosity, it is determined whether to perform a second sublimation.
[0059] Step S4: Perform a rehydration test on the freeze-dried deer blood after the second sublimation to obtain the rehydration time and rehydration rate. Determine whether to adjust the heating rate of the first sublimation based on the rehydration time and the rehydration rate.
[0060] The actual ice crystal uniformity includes ice crystal size uniformity and ice crystal spatial uniformity.
[0061] This embodiment also provides a method for pretreating deer blood, including the following steps:
[0062] Step S11: Collect fresh deer blood using vacuum blood collection tubes or sterile containers, add an anticoagulant (such as 3.8% sodium citrate, in a ratio of 1:9), cool the fresh deer blood to 4°C and let it stand for 2 hours.
[0063] Step S12: Remove large particles such as hair and tissue fragments by passing them through a 100-200 mesh sieve, and let stand for 10 minutes to eliminate air bubbles and avoid uneven structure during freeze-drying;
[0064] Step S13: The fresh deer blood is centrifuged at a speed of 3000-4000 rpm for 15-20 minutes. The centrifuge produces three layers. The lower layer of the solution is taken to obtain clear blood, which contains red blood cells.
[0065] Specifically, the process of obtaining frozen deer blood by cryogenic freezing of the clarified blood includes,
[0066] Clarified blood is placed in a pre-specified deer blood freezing tray, and the clarified blood is frozen based on the initial freezing thickness to obtain frozen deer blood;
[0067] The initial frozen thickness is determined based on the heat conduction efficiency of the clarified blood.
[0068] In this embodiment, a deer blood holding freezing tray with dimensions of 30×30×1cm (length×width×height), a capacity of 3L, a thickness of 5mm, and made of medical-grade stainless steel (e.g., 316L stainless steel) is used to hold clarified blood. The deer blood holding freezing tray is polished to facilitate the removal of frozen deer blood.
[0069] The initial freezing thickness is determined based on the heat transfer efficiency of the clarified blood. The process involves testing the heat transfer efficiency of the clarified blood in the deer blood holding freezing tray. The clarified blood is poured into the deer blood holding freezing tray, and the thickness of the clarified blood is tested sequentially from thin to thick, with 0.1 cm as a test interval. The clarified blood is then cooled down, and the final thickness at which the clarified blood reaches the preset temperature of 4°C within a preset time, such as 5 minutes, is set as the initial freezing thickness. The final thickness of the initial freezing thickness is 0.5 cm after continuous testing.
[0070] The process of determining the initial freezing thickness by measuring heat transfer efficiency can maximize the initial freezing thickness when freezing deer blood, thereby improving freezing efficiency and increasing the utilization rate of the deer blood holding freezing tray.
[0071] Specifically, the process of determining whether to adjust the freezing rate based on the actual ice crystal size includes,
[0072] By comparing the actual ice crystal size with the standard ice crystal size range, an ice crystal comparison result is obtained, and the freezing rate is determined based on the ice crystal comparison result.
[0073] The standard ice crystal size range is determined based on the average diameter of clear blood cells.
[0074] Multi-stage precise control achieved a comprehensive improvement in freeze-dried quality. In the pretreatment stage, a gradient centrifugation combined with low-temperature settling clarification process was employed to improve red blood cell recovery rate. Simultaneously, heat transfer was optimized using 316 stainless steel freezing trays. A four-fold detection mechanism was introduced: dynamic control of ice crystal size, dual-index evaluation of uniformity, coordinated determination of moisture and porosity, and feedback adjustment of rehydration performance, forming a complete quality control closed loop. Among these, the initial freezing thickness, determined based on heat transfer efficiency, increased production capacity while reducing freezing energy consumption.
[0075] Specifically, the process of obtaining the actual ice crystal uniformity by detecting the ice crystal uniformity of frozen deer blood includes the following steps:
[0076] Take out the flat deer blood plate, divide the flat deer blood plate evenly to obtain several deer blood plates to be tested, select several deer blood plates to be tested from each test area, and test the ice crystal uniformity of the deer blood plates to be tested to obtain the actual ice crystal uniformity.
[0077] The flat deer blood plate is the frozen deer blood in the freezing tray after freezing. The area to be tested includes the central area of the flat deer blood plate and other areas surrounding the central area.
[0078] Specifically, the process of obtaining the actual ice crystal uniformity by detecting the ice crystal uniformity of the deer blood plate to be tested includes,
[0079] The deer blood plate to be tested is subjected to low-temperature slicing to obtain deer blood plate slices. The shape and length of the ice crystals in the deer blood plate slices are analyzed, and the uniformity of ice crystal size is determined based on the ice crystal area and ice crystal length.
[0080] The ice crystal shape includes dispersed ice crystals and rounded ice crystals, and the ice crystal length is the longest possible length of a single ice crystal.
[0081] The standard ice crystal size range is determined based on the average diameter of clear blood cells. The cell diameter of healthy clear blood cells is detected to be in the range of 7-9 μm. Since ice crystals that are too large may puncture healthy clear blood cells, and ice crystals that are too small may cause insufficient water to seep out of the cells due to excessive freezing rate, thus forming intracellular ice crystals, the standard ice crystal size range is set to be 5-15 μm.
[0082] Determining the standard ice crystal size range by clarifying the average diameter of blood cells can prevent ice crystals that are too large from piercing the cell wall. At the same time, it can also prevent ice crystals that are too small during freezing from forming intracellular ice crystals because the freezing rate is too fast and the intracellular water has not fully seeped out.
[0083] The flat deer blood plate measures 30×30×1cm. The plate is removed and placed in a -20°C environment for segmentation, resulting in several test areas, each measuring 10×10cm. The flat deer blood plate is now evenly divided into nine 10×10cm test areas. Each test area is further segmented to obtain test plates measuring 2×2cm. The central 10×10cm area of the flat deer blood plate is selected as the middle area of the flat deer blood plate. Each test area contains 25 test plates.
[0084] Five deer blood plates were randomly selected from each testing area. Each plate was sliced using a cryostat, with a slice thickness controlled at 20 μm. Ten fields of view were randomly selected from each slice under a microscope for observation. The shape and length of ice crystals in any field of view were recorded. The slices were then projected onto the ground, and the projected area was calculated using image analysis software. The calculation process is existing technology and will not be described in detail here. The area of each field of view was set to 0.04 mm² (200 × 200 μm).
[0085] After observing 10 fields of view of any deer blood plate slice to be tested, if there are more than or equal to the number of rounded ice crystals exceeding the standard in the 10 fields of view, it is determined that the uniformity of ice crystal size of the corresponding deer blood plate slice to be tested does not meet the standard.
[0086] After observing 10 fields of view of any deer blood plate slice to be tested, if there are fewer than the number of rounded ice crystals in the 10 fields of view, it is determined that the ice crystal size uniformity of the corresponding deer blood plate slice to be tested meets the standard.
[0087] After observing 10 fields of view of any deer blood plate slice to be tested, if there are 0 cases of excessive round ice crystals in the 10 fields of view, the uniformity of ice crystal size is determined according to the ice crystal area and ice crystal length.
[0088] After observing 10 fields of view of any deer blood platelet slice to be tested, if rounded ice crystals appear in 3 or more of the 10 fields of view, then the ice crystal size uniformity of the corresponding deer blood platelet slice to be tested is determined to be non-compliant with the standard.
[0089] After observing 10 fields of view of any deer blood plate slice to be tested, if there are fewer than 3 fields of view with rounded ice crystals, then the uniformity of ice crystal size of the corresponding deer blood plate slice to be tested is determined to meet the standard.
[0090] After observing 10 fields of view of any deer blood plate slice to be tested, if there are 0 cases of excessive round ice crystals in the 10 fields of view, the uniformity of ice crystal size is determined according to the ice crystal area and ice crystal length.
[0091] Suppose that the following ice crystal data were detected in 10 fields of view of a deer blood plate slice. The fields of view are numbered and the ice crystals are all scattered ice crystals.
[0092] The area of the ice crystal corresponding to field of view 1 is 80 μm. ² The ice crystals are 8 μm long;
[0093] The area of the ice crystal corresponding to field of view 2 is 85 μm. ² The ice crystals are 9 μm long;
[0094] The area of the ice crystal corresponding to field of view 3 is 78 μm. ² The ice crystals are 7 μm long;
[0095] The area of the ice crystal corresponding to field of view 4 is 82 μm. ² The ice crystals are 8 μm long;
[0096] The area of the ice crystal corresponding to field of view 5 is 88 μm. ² The ice crystals are 10 μm long;
[0097] The area of the ice crystal corresponding to field of view 6 is 90 μm. ² The ice crystals are 10 μm long;
[0098] The area of the ice crystal corresponding to field of view 7 is 84 μm. ² The ice crystals are 9 μm long;
[0099] The area of the ice crystal corresponding to field of view 8 is 76 μm. ² The ice crystals are 7 μm long;
[0100] The area of the ice crystal corresponding to field of view 9 is 92 μm. ² The ice crystals are 11 μm long;
[0101] The area of the ice crystal corresponding to field of view 10 is 86 μm. ² The ice crystals are 9 μm long;
[0102] The ice crystal size uniformity of any deer blood plate slice to be tested is the average of the ice crystal size uniformity of 10 fields of view.
[0103] The uniformity of ice crystal size in the field of view is (A / A+|Aa-Ab|)×Wa+(B / B+|Ba-Bb|)×Wb;
[0104] Where A is the area compensation parameter for ice crystal area relative to actual ice crystal uniformity, set to 5 μm; Aa is the ice crystal area in the current field of view; Ab is the average ice crystal area across 10 fields of view; Wa is the ice crystal area weight of 0.6; and B is the area compensation parameter for ice crystal length relative to actual ice crystal uniformity, set to 10 μm. ² Ba represents the current ice crystal length in the field of view; Bb represents the average ice crystal length across 10 fields of view; Wb represents the ice crystal length with a weight of 0.4.
[0105] The uniformity of ice crystal size in field of view 1 is (10 / 10 + |80 - 84.1|) × 0.6 + (5 / 5 + |8 - 8.8|) × 0.4 ≈ 0.770;
[0106] The uniformity of ice crystal size in field of view 2 is (10 / 10 + |85 - 84.1|) × 0.6 + (5 / 5 + |9 - 8.8|) × 0.4 ≈ 0.935;
[0107] The uniformity of ice crystal size in field of view 3 is (10 / 10 + |78 - 84.1|) × 0.6 + (5 / 5 + |7 - 8.8|) × 0.4 ≈ 0.915;
[0108] The uniformity of ice crystal size in field of view 4 is (10 / 10 + |82 - 84.1|) × 0.6 + (5 / 5 + |8 - 8.8|) × 0.4 ≈ 0.841;
[0109] The uniformity of ice crystal size in field of view 5 is (10 / 10 + |88 - 84.1|) × 0.6 + (5 / 5 + |10 - 8.8|) × 0.4 ≈ 0.754;
[0110] The uniformity of ice crystal size in field of view 6 is (10 / 10 + |90 - 84.1|) × 0.6 + (5 / 5 + |10 - 8.8|) × 0.4 ≈ 0.699;
[0111] The uniformity of ice crystal size in field of view 7 is (10 / 10 + |84 - 84.1|) × 0.6 + (5 / 5 + |9 - 8.8|) × 0.4 ≈ 0.979;
[0112] The uniformity of ice crystal size in field of view 8 is (10 / 10 + |76 - 84.1|) × 0.6 + (5 / 5 + |7 - 8.8|) × 0.4 ≈ 0.625;
[0113] The uniformity of ice crystal size in field of view 9 is (10 / 10 + |92 - 84.1|) × 0.6 + (5 / 5 + |11 - 8.8|) × 0.4 ≈ 0.613;
[0114] The uniformity of ice crystal size in field of view 10 is (10 / 10 + |86 - 84.1|) × 0.6 + (5 / 5 + |9 - 8.8|) × 0.4 ≈ 0.889;
[0115] The uniformity of ice crystal size in the deer blood plate slice to be tested is (0.770+0.935+0.915+0.841+0.754+0.699+0.979+0.625+0.613+0.889) / 10=0.803;
[0116] Dividing the flat deer blood plate into different test areas allows for the detection of ice crystal size uniformity in different areas, avoiding misjudgment of the actual ice crystal uniformity of the flat deer blood plate and increasing drying efficiency. By making a preliminary judgment on the ice crystal shape of the deer blood plate slices to be tested, areas where the ice crystal size uniformity does not meet the standard can be quickly identified, thereby improving drying efficiency. By observing and calculating the ice crystal area and ice crystal length of 10 fields of view of the deer blood plate slices to be tested, the corresponding ice crystal size uniformity can be obtained, further refining the detection of ice crystal size uniformity in the test area and improving the effect of freeze-drying deer blood.
[0117] If the uniformity of ice crystal size in the deer blood plate slices to be tested does not meet the standard, other slices of the same deer blood plate to be tested are tested for rounded ice crystals. If, after testing, the actual ratio of the number of slices with more or less rounded ice crystals exceeding the standard to the total number of slices of the same deer blood plate to be tested is greater than the standard judgment ratio, it is determined whether the corresponding test area is the middle area or other areas. If the corresponding test area is the middle area, the flat deer blood plates are judged to be unqualified and need to be re-frozen. In this embodiment, since there are high quality requirements for deer blood freeze-dried powder, the flat deer blood plates are judged to be unqualified if the corresponding test area is the middle area.
[0118] The standard judgment ratio is determined based on the corresponding historical data;
[0119] If the corresponding area to be tested is another area, the deer blood plate in the corresponding area is deemed unqualified, and the middle area and other edge areas are retained.
[0120] For example, if the standard judgment ratio is set to 5%, and the actual ratio is greater than the standard judgment ratio, the actual ratio indicates that the middle area of the flat deer blood plate is unqualified, that is, the entire flat deer blood plate is unqualified, and the uniformity of ice crystal size does not meet the requirements.
[0121] If the actual ratio indicates that other areas of the flat deer blood plate are not up to standard, then the actual ice crystal uniformity is determined to meet the standard based on the comparison between the actual ice crystal uniformity difference value of other areas and the standard ice crystal uniformity difference value.
[0122] For example, the actual ice crystal uniformity of other regions 1 is 0.853; the actual ice crystal uniformity of other regions 2 is 0.953; and the actual ice crystal uniformity of other regions 3 is 0.754. The average of the actual ice crystal uniformity of the three other regions is 0.853. The standard judgment ratio is 20%, so the standard judgment ratio range is [0.853×(1-5%), 0.853×(1+5%)], that is, [0.810, 0.896]. Other regions within this range are regions whose actual ice crystal uniformity meets the standard, and other regions outside this range are regions whose actual ice crystal uniformity does not meet the standard.
[0123] Dispersed ice crystals include irregular ice crystals and needle-shaped ice crystals; rounded ice crystals include hexagonal ice crystals.
[0124] Strict ice crystal size uniformity testing and regional identification ensure that the quality of freeze-dried deer blood powder meets high standards. Defective deer blood plate slices are promptly identified and disposed of to prevent substandard products from entering subsequent production processes. Clearly defined acceptance / disapproval criteria for different regions help optimize production processes, improve production efficiency, and ensure product quality consistency.
[0125] Specifically, the process of obtaining the actual ice crystal uniformity by detecting the ice crystal uniformity of the deer blood plate to be tested includes,
[0126] Select and test deer blood plate slices in different test areas to obtain several ice crystal size uniformity values. Compare the ice crystal size uniformity values to obtain the actual ice crystal uniformity difference value. Based on the comparison between the actual ice crystal uniformity difference value and the standard ice crystal uniformity difference value, determine whether to perform initial sublimation on the frozen deer blood.
[0127] The ice crystal uniformity difference value is determined based on the average cell diameter.
[0128] Specifically, the process of testing the residual moisture and porosity of freeze-dried deer blood after the initial sublimation includes the following steps:
[0129] The moisture content of the middle and edge regions of freeze-dried deer blood is detected by infrared spectroscopy, and the average value is taken to obtain the actual moisture content. Freeze-dried deer blood in the test area after the first sublimation is selected and sliced to obtain freeze-dried deer blood slices. The channel area of the freeze-dried deer blood slices is detected, and the need for secondary sublimation is determined based on the channel area ratio and the actual moisture content.
[0130] The channel area ratio is the ratio of the channel area to the surface area of the freeze-dried slice.
[0131] Infrared spectroscopy was performed on the freeze-dried deer blood in the middle and edge regions. Infrared light of a specific wavelength in the infrared spectrum of a preset intensity was irradiated onto the freeze-dried deer blood. The intensity of the absorption peak of the specific wavelength in the infrared spectrum of the remaining freeze-dried deer blood after passing through the freeze-dried deer blood was detected. The actual moisture content was determined by multiplying the difference between the specific wavelength in the infrared spectrum of the preset intensity and the intensity of the absorption peak of the specific wavelength in the infrared spectrum of the remaining freeze-dried deer blood after passing through the freeze-dried deer blood and the product of the difference and the compensation parameter for the influence of the difference on the actual moisture content.
[0132] The freeze-dried deer blood slices were irradiated with compensating light. The irradiation standard was to be able to observe the channels in the freeze-dried deer blood slices. The channels are porous structures left after the ice crystals sublimate during the initial sublimation. The observation equipment with a computer was used to observe them and calculate their channel area ratio. The observation equipment can be a microscope or other instruments that can meet the requirements for observing microstructures.
[0133] For example, using a Fourier transform infrared spectrometer, a specific wave intensity is preset to 0.4.
[0134] If the intensity of the absorption peak at a specific wavelength in the infrared spectrum of the remaining freeze-dried deer blood after passing through the freeze-drying process is 0.38, then the actual moisture content is (0.4-0.38) / 0.4×As, where As is a compensation parameter for the effect of the difference on the actual moisture content.
[0135] As is set as the compensation parameter for the impact of the difference on the actual moisture residue, which is 1.25 and is determined based on historical data of the compensation parameter for the impact of the difference on the actual moisture residue.
[0136] Therefore, the actual residual moisture content is (0.4-0.38) / 0.4×1.25=6.25%;
[0137] After testing, the surface area of the observation surface corresponding to the freeze-dried deer blood slices was found to be 2 × 0.5 cm = 1 cm². 2 The detection channel area is Bs. If the detection channel area is 0.9 cm², ... 2 Therefore, the channel area ratio is 0.9 / 1 = 0.9;
[0138] The maximum residual moisture content was set at 8%, and the minimum channel area ratio was set at 0.85.
[0139] If the actual residual moisture content is greater than the maximum residual moisture content or the channel area ratio is less than the minimum channel area ratio, it is determined that the secondary sublimation requirement is not met and the primary sublimation needs to be performed again.
[0140] If the actual residual moisture content is less than or equal to the maximum residual moisture content, or if the channel area ratio is greater than or equal to the minimum channel area ratio, then a second sublimation is determined.
[0141] This technical solution demonstrates significant advantages in quality control of deer blood freeze-drying by establishing a dual-index detection system for moisture residue and porosity. Fourier transform infrared spectroscopy is used to detect moisture in the central and edge regions of the freeze-dried product. The actual moisture residue (6.25%) is calculated by the difference between a preset light intensity (0.4) and the measured absorption peak intensity (0.38), and a compensation parameter calibrated from historical data (As=1.25) is introduced to ensure measurement accuracy. Simultaneously, microscopic image analysis technology is used to quantify the channel area ratio (0.9) of the freeze-dried skeleton. By setting threshold standards for the highest moisture residue (8%) and the lowest channel area ratio (0.85), accurate secondary sublimation determination is achieved. Dual-parameter collaborative detection can comprehensively evaluate freeze-drying quality; the dynamic compensation mechanism controls moisture calculation errors.
[0142] Specifically, the process of testing the rehydration properties of freeze-dried deer blood after secondary sublimation to obtain the rehydration time and rehydration rate includes the following steps:
[0143] Place the freeze-dried deer blood blocks into purified water at a preset temperature, calculate the rehydration time by measuring the time required for the freeze-dried deer blood blocks to completely dissolve in the purified water, place freeze-dried deer blood blocks of the same batch into purified water, remove the freeze-dried deer blood blocks according to the preset rehydration absorption time, and determine the rehydration rate by the ratio of the weight of the dry freeze-dried deer blood blocks before being placed into purified water to the weight of the rehydrated freeze-dried blocks after being placed into purified water.
[0144] The initial weight of the drying block was measured using an electronic balance with an accuracy of 0.01g. The preset water temperature was 20℃.
[0145] The freeze-dried deer blood blocks were completely immersed in 200ml of purified water, and the time for complete dissolution was recorded with a stopwatch. The rehydration time was found to be 45 seconds.
[0146] The rehydration absorption time was set to 20 seconds. After immersing the freeze-dried deer blood blocks from the same batch in clean water for 20 seconds, they were removed, their surface moisture was blotted dry with filter paper, and their weight was 3.75g. The rehydration rate was (3.75-2.5) / 2.5×100%=50%.
[0147] The rehydration absorption time is determined based on historical data on rehydration absorption time.
[0148] Specifically, the process of determining whether to adjust the heating rate of the initial sublimation based on the rehydration time and the rehydration rate includes the following:
[0149] An actual heating rate evaluation value is generated based on the rehydration time and rehydration rate. The heating rate evaluation value is compared with the standard heating rate evaluation value range to obtain a heating rate evaluation value comparison result. Based on the heating rate evaluation value comparison result, it is determined whether to adjust the heating rate of the initial sublimation.
[0150] The standard heating rate evaluation value range is determined based on historical data of deer blood freeze-dried products. The historical data is the average of multiple batches of deer blood freeze-dried products that meet the production requirements regarding the standard heating rate evaluation value.
[0151] Specifically, the process of determining whether to adjust the heating rate of the initial sublimation based on the comparison results of the heating rate evaluation values includes,
[0152] If the heating rate evaluation value is less than the minimum value of the standard heating rate evaluation value range, the heating rate is increased according to the difference between the minimum value of the standard heating rate evaluation value range and the heating rate evaluation value.
[0153] If the heating rate evaluation value is within the standard heating rate evaluation value range, maintain the original heating rate.
[0154] If the heating rate evaluation value is greater than the maximum value of the standard heating rate evaluation value range, the heating rate is reduced based on the difference between the heating rate evaluation value and the maximum value of the standard heating rate evaluation value range.
[0155] In this embodiment, the standard heating rate evaluation value range is set to [40, 60] based on historical data.
[0156] The actual heating rate evaluation value is the product of the ratio of the historical average rehydration time to the current measured rehydration time and the current rehydration rate.
[0157] Based on the historical average rehydration time of 35 seconds, the actual heating rate is evaluated as (35 / 45)×50=38.9.
[0158] If the heating rate evaluation value is less than the minimum value of the standard heating rate evaluation value range, the heating rate is increased according to the difference between the minimum value of the standard heating rate evaluation value range and the heating rate evaluation value.
[0159] When the heating rate is insufficient, the rehydration time is 70 seconds, the rehydration rate is 35%, and the heating rate evaluation value is (35 / 70)×35=17.5.
[0160] The initial heating rate was set to 2.8℃ / min, and the compensation parameter for the effect of the difference between the minimum value of the standard heating rate evaluation range and the heating rate evaluation value on the initial heating rate was set to 0.2.
[0161] The increased heating rate is 2.8 + (40 - 17.5) × 0.2 = 7.3℃ / min;
[0162] If the heating rate evaluation value is within the standard heating rate evaluation value range, maintain the original heating rate.
[0163] If the heating rate evaluation value is greater than the maximum value of the standard heating rate evaluation value range, the heating rate is reduced according to the difference between the heating rate evaluation value and the maximum value of the standard heating rate evaluation value range.
[0164] When the heating rate is too high, the rehydration time is 18s, the rehydration rate is 25%, and the heating rate evaluation value is (35 / 18)×25=48.6;
[0165] The reduced heating rate is 2.8 - (48.6 - 40) × 0.2 = 1.08℃ / min.
[0166] This technical solution achieves precise control of the deer blood freeze-drying process by establishing a quantitative correlation model between rehydration performance and freeze-drying process parameters. Rehydration time and rehydration rate are used as core evaluation indicators and converted into heating rate evaluation values. When the heating rate evaluation value is less than the minimum value of the standard heating rate evaluation value range, the heating rate is increased based on the difference between the minimum value and the heating rate evaluation value. This avoids insufficient heating rate leading to incomplete sublimation of ice crystals, causing water to recondense inside the freeze-dried deer blood, forming localized liquid water. Slow heating prolongs ice crystal growth time, resulting in excessively large ice crystals that puncture deer blood cells and affect product quality. Conversely, when the heating rate evaluation value is greater than the maximum value of the standard heating rate evaluation value range, the heating rate is decreased based on the difference between the two values. This avoids rapid heating causing the surface of the freeze-dried deer blood to dry and form a hard shell, hindering the escape of water vapor from the sublimation of internal ice crystals.
[0167] The technical solution of the present invention has been described above with reference to the preferred embodiments shown in the accompanying drawings. However, it will be readily understood by those skilled in the art that the scope of protection of the present invention is obviously not limited to these specific embodiments. Without departing from the principles of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will all fall within the scope of protection of the present invention.
[0168] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.
Claims
1. A drying method for deer blood freeze-dried powder, characterized in that, The method comprises the following steps, The method comprises the following steps, For the case that the ice crystal size meets the drying requirement, the ice crystal uniformity of the frozen deer blood is detected to obtain an actual ice crystal uniformity, and different to-be-detected deer blood plate slices in different to-be-detected regions are selected and detected to obtain a plurality of ice crystal size uniformities. A comparison is made between the ice crystal size uniformities to obtain an actual ice crystal uniformity difference value. Whether the frozen deer blood is subjected to primary sublimation is determined according to a comparison result of the actual ice crystal uniformity difference value and a standard ice crystal uniformity difference value. The ice crystal uniformity difference value is determined according to the average diameter of cells. Whether the frozen deer blood is subjected to primary sublimation is determined by comparing the actual ice crystal uniformity and a standard ice crystal uniformity interval. The water residue degree of the freeze-dried deer blood after primary sublimation is detected, and the porosity of the freeze-dried deer blood is detected. The water residue degree of the freeze-dried deer blood in a middle region and an edge region is detected by infrared spectroscopy, and an average value is obtained to obtain an actual water residue degree. The freeze-dried deer blood in the to-be-detected region after primary sublimation is sliced to obtain a freeze-dried deer blood slice. Whether secondary sublimation is performed is determined according to a channel area ratio and the actual water residue degree. The channel area ratio is a ratio of a channel area to a surface area of the freeze-dried slice. Whether secondary sublimation is performed is determined according to the water residue degree and the porosity. The rehydration detection of the freeze-dried deer blood after secondary sublimation is performed to obtain a rehydration time length and a rehydration rate. Whether the heating rate of primary sublimation is adjusted is determined according to the rehydration time length and the rehydration rate. An actual heating rate evaluation value is generated according to the rehydration time length and the rehydration rate. A heating rate evaluation value comparison result is obtained by comparing the actual heating rate evaluation value with a standard heating rate evaluation value interval. Whether the heating rate of primary sublimation is adjusted is determined according to the heating rate evaluation value comparison result. The standard heating rate evaluation value interval is determined according to historical data of the freeze-dried deer blood. The actual ice crystal uniformity includes an ice crystal size uniformity and an ice crystal space uniformity.
2. The drying method for the deer blood freeze-dried powder according to claim 1, characterized in that, The process of obtaining the frozen deer blood by low-temperature freezing of the clarified blood comprises, The clarified blood is carried by a deer blood carrier with a preset specification to carry a freezing disc, and the clarified blood is frozen based on an initial freezing thickness to obtain the frozen deer blood. The initial freezing thickness is determined according to the heat conduction efficiency of the clarified blood.
3. The drying method for the deer blood freeze-dried powder according to claim 2, characterized in that, The process of determining whether to adjust the freezing rate according to the actual ice crystal size comprises, A comparison is made between the actual ice crystal size and a standard ice crystal size range to obtain an ice crystal comparison result. Whether to adjust the freezing rate is determined according to the ice crystal comparison result. The standard ice crystal size range is determined according to the average diameter of cells in the clarified blood.
4. The drying method for the deer blood freeze-dried powder according to claim 3, characterized in that, The process of detecting the ice crystal uniformity of the frozen deer blood to obtain an actual ice crystal uniformity comprises, The flat deer blood plate is taken out, and the flat deer blood plate is uniformly divided to obtain a plurality of to-be-detected deer blood plates. A plurality of to-be-detected deer blood plates in different to-be-detected regions are selected, and the ice crystal uniformity of the to-be-detected deer blood plates is detected to obtain an actual ice crystal uniformity. The flat deer blood plate is the frozen deer blood in the frozen plate after the freezing is completed, and the to-be-detected area includes a middle area of the flat deer blood plate and other areas surrounding the middle area.
5. The drying method for the deer blood freeze-dried powder according to claim 4, characterized in that, The process of detecting the ice crystal uniformity of the to-be-detected deer blood plate to obtain the actual ice crystal uniformity includes, The to-be-detected deer blood plate is cryosectioned to obtain a to-be-detected deer blood plate section, the ice crystal shape and the ice crystal length of the to-be-detected deer blood plate section are analyzed, and the ice crystal size uniformity is determined according to the ice crystal area of the ice crystal shape and the ice crystal length. The ice crystal shape includes dispersed ice crystals and round ice crystals, and the ice crystal length is the longest length of a single ice crystal.
6. The drying method for the deer blood freeze-dried powder according to claim 5, characterized in that, The process of detecting the rehydration of the deer blood freeze-dried after the secondary sublimation to obtain the rehydration time and the rehydration rate includes, The deer blood freeze-dried block is placed in clean water at a preset temperature, the time taken for the deer blood freeze-dried block to completely dissolve in the clean water is calculated to obtain the rehydration time, the same batch of deer blood freeze-dried blocks are placed in clean water, the deer blood freeze-dried blocks are taken out according to the preset rehydration absorption time, and the rehydration rate is determined according to the ratio of the weight of the dried deer blood freeze-dried block before being placed in the clean water to the weight of the rehydrated freeze-dried block after being placed in the clean water.
7. The drying method for the deer blood freeze-dried powder according to claim 6, characterized in that, The process of determining whether to adjust the temperature rising rate of the primary sublimation according to the comparison result of the temperature rising rate evaluation value includes, For the case that the temperature rising rate evaluation value is less than the minimum value of the standard temperature rising rate evaluation value interval, the temperature rising rate is increased according to the difference between the minimum value of the standard temperature rising rate evaluation value interval and the temperature rising rate evaluation value; For the case that the temperature rising rate evaluation value is in the standard temperature rising rate evaluation value interval, the original temperature rising rate is maintained; For the case that the temperature rising rate evaluation value is greater than the maximum value of the standard temperature rising rate evaluation value interval, the temperature rising rate is decreased according to the difference between the temperature rising rate evaluation value and the maximum value of the standard temperature rising rate evaluation value interval.
Citation Information
Patent Citations
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