Preparation method of calcined concha arcae nano-micron particles

Abstract

The invention relates to the technical field of traditional Chinese medicine processing, and particularly discloses a preparation method of calcined concha arcae nano-micron particles. Grinding and pulping: putting the calcined concha arcae powder into a mortar, adding a small amount of purified water, and grinding for 25 minutes to obtain calcined concha arcae pulp; settling and separating; pouring upper-layer turbid liquid; treating coarse particles; freezing and drying; the loose nano-micron calcined concha arcae powder is obtained. According to the method, the calcined concha arcae is taken as a raw material, the preparation process parameters of the calcined concha arcae nano-micron particles are optimized through a single-factor test and an orthogonal test method, and the reliability is high; the preparation method disclosed by the invention is low in cost and simple in preparation process, does not cause the change of the concha arcae structure, and conforms to the concept of sustainable development.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of traditional Chinese medicine processing, in particular to a preparation method of calcined wale nut nano-micron particles. BACKGROUND

[0002] Wale nut, as a typical representative of commonly used marine shell traditional Chinese medicine, is the shell of Arca subcrenata Lischke, Arca granosa Linnaeus or Arca inflata Reeve in Arcidae. It tastes salty and is flat in nature, has the functions of dissipating phlegm and blood stasis, softening and resolving nodules, and relieving acid and pain, and can be used to treat stubborn phlegm and coagulation, viscous and difficult to cough, goiter, scrofula, and mass in the abdomen, stomach pain and acid reflux, etc. There are many traditional Chinese medicine prescriptions containing wale nut in history, such as Hua Hua pill in ZHENG ZHI ZHUN LING, and Wale nut pill in WAN SHI JIA ZHOU FANG, etc. Modern research shows that wale nut has the effect of promoting the shrinkage of liver and spleen, and is effective for liver and spleen enlargement caused by blood fluke disease, and can also be used for other connective tissue hyperplasia diseases; at the same time, it also has the effect of resisting cancer.

[0003] Wale nut has a long history of processing, and its raw product, calcined product and calcined and quenched product are commonly used in clinic. As for its processing, Lei Gong Pao Zhi Lun first proposed the processing method of "burning on the fire and calcining to redness" for the intermediate class, and proposed that "frying is to burn the medicine on the fire until it is red, and the intermediate class is often used in this way". Wale nut belongs to a molecular or nano structure aggregate, which is mainly composed of calcium carbonate crystals (content > 95%) of calcite and / or aragonite phase. After calcination, the original hard texture becomes crisp, greatly improving the crushing efficiency. This physical change not only facilitates the decoction of calcium salt, trace elements and other effective ingredients, but also reduces the content of harmful elements such as arsenic and lead, and reduces or eliminates side effects.

[0004] Wale nut, like most shell medicines, is derived from aquatic processing by-products, and has a large resource quantity but low traditional utilization rate. The effective components in large particles of wale nut have slow dissolution rate and low dissolution degree, resulting in a large amount of effective components being discarded without being released. Studies have shown that the particle size of wale nut is reduced, which increases the surface area, and the effective components such as calcium ions and carbonates are more easily released. This difference in characteristics affects the clinical efficacy. In addition, the increase in surface area is also more conducive to loading other drugs to achieve synergistic treatment of diseases. Therefore, by reducing the particle size of wale nut, the active ingredients therein can be fully released and utilized, and the resource utilization efficiency can be improved, which is not only crucial to improving the clinical efficacy of traditional Chinese medicine, but also in line with the concept of sustainable development, and thus provides a preparation method of calcined wale nut nano-micron particles. SUMMARY

[0005] The purpose of the present application is to overcome the defects of the prior art, and to provide a preparation method of calcined wale nut nano-micron particles to solve the problems in the background art.

[0006] To achieve the above object, the present application provides the following technical solutions: a preparation method of calcined Eurycoma longifolia nanometer microparticles, the specific steps are as follows:

[0007] S1: raw material preparation: collect Eurycoma longifolia, wash with tap water, remove sediment and residual soft flesh, then rinse with purified water, dry at room temperature, calcine in a muffle furnace, crush and sieve to obtain calcined Eurycoma longifolia powder;

[0008] S2: grinding and slurry preparation: put the calcined Eurycoma longifolia powder into a mortar, add a small amount of purified water and grind for 25 min to obtain a calcined Eurycoma longifolia slurry;

[0009] S3: sedimentation separation: add purified water to the calcined Eurycoma longifolia slurry of step S2, the solid-liquid ratio is 1:180 (g / ml), stir and then stand still, so that the coarse particles sink and the target nanometer microparticles are suspended in the purified water;

[0010] S4: decant the upper suspension liquid containing the target nanometer microparticles;

[0011] S5: coarse particle treatment: repeat steps S2-S4 four times for the coarse particles that sink in S3, and combine all the collected suspensions in a clean beaker; the grinding time, solid-liquid ratio and grinding times in steps S2, S3 and S5 are determined by single factor experiment combined with orthogonal test analysis;

[0012] S6: freeze-drying: put the suspension liquid of step S5 into a freeze-drying machine for freeze-drying treatment to obtain loose nanometer microparticles of calcined Eurycoma longifolia.

[0013] As a preferred technical solution of the present application, in step S1, the calcination temperature is 750°C, the calcination time is 0.5 h, and the sieve size is 200 mesh.

[0014] As a preferred technical solution of the present application, the single factor experiment is used to optimize the initial preparation parameters of Eurycoma longifolia nanometer microparticles, and the optimized parameters after single factor optimization are as follows: grinding time 15-25 min, solid-liquid ratio 1:(160-200) (g / ml), and grinding times 2-4 times; then, based on the preparation conditions optimized by single factor, the D90 value and yield of Eurycoma longifolia nanometer microparticles are used as comprehensive evaluation indexes, and the orthogonal test method is used to further optimize the preparation parameters of Eurycoma longifolia nanometer microparticles, and the finally optimized parameters are as follows: grinding time 25 min, solid-liquid ratio 1:180 (g / ml), and grinding times 4 times.

[0015] As a preferred technical solution of the present application, in step S3, the standing time after stirring is 30 min.

[0016] The Goutengzi nano microparticles prepared by the preparation method have a D90 value of 942.51 nm and a yield of 10.03%.

[0017] Compared with the prior art, the method has the following beneficial effects:

[0018] The method uses Goutengzi as a raw material, and optimizes the preparation process parameters of the Goutengzi nano microparticles through single-factor experiments and orthogonal experiments, and has high reliability. The preparation method is low in cost, simple in preparation process, and does not cause changes in the structure of Goutengzi, and meets the concept of sustainable development. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 is a flowchart of the application;

[0020] Figure 2 is a graph of the influence of the grinding times on the D90 of the Goutengzi nano microparticles;

[0021] Figure 3 is a graph of the influence of the grinding times on the yield of the Goutengzi nano microparticles;

[0022] Figure 4 is a graph of the influence of the grinding times on the D90 of the Goutengzi nano microparticles;

[0023] Figure 5 is a graph of the influence of the grinding times on the yield of the Goutengzi nano microparticles;

[0024] Figure 6 is a graph of the influence of the liquid-solid ratio on the D90 of the Goutengzi nano microparticles;

[0025] Figure 7 is a graph of the influence of the liquid-solid ratio on the yield of the Goutengzi nano microparticles. DETAILED DESCRIPTION

[0026] The preferred embodiments of the application will be described in detail below with reference to the accompanying drawings, so that the advantages and features of the application can be more easily understood by those skilled in the art, and the protection scope of the application can be more clearly defined.

[0027] Embodiment: A method for preparing Goutengzi nano microparticles, comprising the following steps:

[0028] S1: Raw material preparation: collect Goutengzi, wash with tap water, remove sediment and residual soft flesh, then rinse with purified water, dry at room temperature, calcine in a muffle furnace at 750 DEG C for 0.5h, crush and pass through a 200-mesh sieve to obtain Goutengzi powder;

[0029] S2: Grinding slurry: Put the calcined Goutengzi powder into a mortar and add a small amount of purified water to grind for 25 min to obtain a calcined Goutengzi slurry;

[0030] S3: Sedimentation separation: Add purified water to the calcined Goutengzi slurry of S2, with a solid-liquid ratio of 1:180 (g / ml). After stirring, stand for 30 min to allow the coarse particles to sink, and the target nanometer microparticles are suspended in the purified water;

[0031] S4: Decant the upper suspension liquid: Carefully decant the upper suspension liquid containing the target nanometer microparticles;

[0032] S5: Coarse particle treatment: Repeat steps S2-S4 four times for the coarse particles that have sunk in S3, and combine all the collected suspension liquids into a clean beaker;

[0033] S6: Freeze-drying: Place the suspension liquid of S5 into a freeze-drying machine for freeze-drying treatment to obtain loose nanometer calcined Goutengzi powder.

[0034] According to the above technical solution, the preparation process parameters of calcined Goutengzi nanometer particles are studied, which involves single-factor experiments. Under the premise of fixed basic process parameters, the optimization space of grinding time, solid-liquid ratio, and grinding times is investigated.

[0035] According to the above technical solution, the effect of grinding time on the preparation process: Set the grinding time to 10 min, 15 min, 20 min, 25 min, and 30 min, with a solid-liquid ratio of 1:160 (g / ml) and grinding 3 times for single-factor experiments to determine the optimal grinding time.

[0036] According to the above technical solution, the effect of solid-liquid ratio on the preparation process: Set the solid-liquid ratio to 1:120 (g / ml), 1:140 (g / ml), 1:160 (g / ml), 1:180 (g / ml), and 1:200 (g / ml), with a grinding time of 20 min and grinding 3 times for single-factor experiments to determine the optimal solid-liquid ratio.

[0037] According to the above technical solution, the effect of grinding times on the preparation process: Set the grinding times to 1, 2, 3, 4, and 5 times, with a grinding time of 20 min and a solid-liquid ratio of 1:160 (g / ml) for single-factor experiments to determine the optimal grinding times.

[0038] According to the above technical solution, based on the single-factor experiment results, taking the D90 value and yield of calcined Goutengzi nanometer particles as the comprehensive evaluation index, and taking the grinding time, solid-liquid ratio, and grinding times as the investigation factors, an orthogonal experiment is designed.

[0039] Table 1: Orthogonal factor level table

[0040]

[0041]

[0042] Results analysis:

[0043] Single factor test:

[0044] The effect of grinding times on D90 value and yield of calcined walnuts nanometer particles:

[0045] The relationship between D90 value and yield of calcined walnuts nanometer particles and grinding times was shown in Figure 2 , Figure 3 . It was known from Figure 2 , Figure 3 that the D90 value of calcined walnuts nanometer particles showed a downward trend with the increase of grinding times, and when the grinding times was more than 3 times, the D90 value increased slightly. The yield of calcined walnuts nanometer particles showed an upward trend with the increase of grinding times.

[0046] The effect of grinding time on D90 value and yield of calcined walnuts nanometer particles:

[0047] The relationship between D90 value and yield of calcined walnuts nanometer particles and grinding time was shown in Figure 4 , Figure 5 . It was known from Figure 4 , Figure 5 that the D90 value of calcined walnuts nanometer particles showed a downward trend with the increase of grinding time, and when the grinding time was more than 20 min, the downward trend of D90 value tended to be flat. The yield of calcined walnuts nanometer particles showed an upward trend with the increase of grinding time, and when the grinding time was more than 20 min, the upward trend of yield tended to be flat.

[0048] The effect of solid-liquid ratio on D90 value and yield of calcined walnuts nanometer particles:

[0049] The relationship between D90 value and yield of calcined walnuts nanometer particles and solid-liquid ratio was shown in Figure 6 , Figure 7 . It was known from Figure 6 , Figure 7 that the D90 value of calcined walnuts nanometer particles showed a downward trend with the increase of solid-liquid ratio, and when the solid-liquid ratio reached 1:180(g / ml), the D90 value began to increase. The yield of calcined walnuts nanometer particles showed an upward trend with the increase of solid-liquid ratio, and when the solid-liquid ratio reached 1:180(g / ml), the yield decreased slightly.

[0050] In summary, the optimal parameter range after single factor optimization was: grinding times: 2-4 times, grinding time 15-25 min, solid-liquid ratio 1:(160-200)(g / ml).

[0051] Orthogonal test:

[0052] On the basis of single factor test, the preparation process parameters of calcined Wanezi nano-microparticles were optimized by orthogonal test, and the experimental results and variance analysis results are shown in Table 2 and Table 3.

[0053] Table 2: Orthogonal test results

[0054]

[0055]

[0056] Table 3: Variance analysis results

[0057]

[0058] According to the orthogonal test results and variance analysis results, the influence order of each factor on the comprehensive score of calcined Wanezi nano-microparticles is grinding time (B) > grinding times (A) > liquid-solid ratio (C), and the grinding time (B) has a significant influence on the comprehensive score of calcined Wanezi nano-microparticles (P < 0.05), while the grinding times (A) and the total water consumption (C) have no significant influence (P > 0.05). According to the above results, the optimal preparation process of calcined Wanezi nano-microparticles is A3B3C2.

[0059] Verification test:

[0060] According to the optimal combination obtained by the orthogonal experiment, the grinding times is 4 times, the grinding time is 25 min, and the liquid-solid ratio is 1:180 (g / ml), and the verification experiment is carried out, and finally the D90 value of the obtained calcined Wanezi nano-microparticles is 942.51 nm, and the yield is 10.03%.

[0061] The above examples only express the embodiments of the present application, and the description is more specific and detailed, but it cannot be understood as the limitation of the scope of the patent. It should be noted that for ordinary skilled in the art, without departing from the concept of the present application, a number of modifications and improvements can be made, which are within the scope of the present application.

Claims

1. A method for the preparation of calcined talc nanomicro-particles, characterized by: The specific steps are as follows: S1: raw material preparation: collect the corrugated sub, wash with tap water, remove the sediment and residual soft meat, then rinse with purified water, dry at room temperature, calcine in a muffle furnace, crush and sieve to obtain calcined corrugated sub powder; S2: grinding and pulping: put the calcined corrugated sub powder into a mortar, add a small amount of purified water and grind for 25 min to obtain a calcined corrugated sub slurry; S3: sedimentation separation: add purified water to the calcined corrugated sub slurry of step S2, the solid-liquid ratio is 1:180 (g / ml), stir and then stand still, so that the coarse particles sink and the target nanometer microparticles are suspended in the purified water; S4: decant the upper suspension liquid containing the target nanometer microparticles; S5: coarse particle treatment: repeat steps S2-S4 four times for the coarse particles that have sunk in S3, and combine all the collected suspensions in a clean beaker; the grinding time, solid-liquid ratio, and grinding times in steps S2, S3, and S5 are determined by single-factor experiments combined with orthogonal test analysis; S6: freeze-drying: put the suspension liquid of step S5 into a freeze-drying machine for freeze-drying treatment to obtain loose nanometer microparticles of calcined corrugated sub.

2. The method of claim 1, wherein the calcined talc nanoparticles are prepared by the process comprising: In step S1, the calcination temperature is 750℃, the calcination time is 0.5h, and the sieve size is 200 mesh.

3. The method for preparing calcined corrugated nanoparticles according to claim 1, characterized in that: The single-factor experiment optimizes the initial preparation parameters of the calcined corrugated sub nanometer microparticles. After single-factor optimization, the parameters are: grinding time 15-25 min, solid-liquid ratio 1:(160-200) (g / ml), and grinding times 2-4 times; then, based on the single-factor optimized preparation conditions, the D90 value and yield of the calcined corrugated sub nanometer microparticles are used as comprehensive evaluation indexes, and the orthogonal test method is used to further optimize the preparation parameters of the calcined corrugated sub nanometer microparticles. The finally optimized parameters are: grinding time 25 min, solid-liquid ratio 1:180 (g / ml), and grinding times 4 times.

4. The method of claim 1, wherein the calcined talc nanoparticles are prepared by the process comprising: In step S3, the stirring and standing time is 30 min.

5. Calcined tourmaline nanoparticles prepared by the method according to any one of claims 1 to 4, characterized by: The D90 value of the calcined corrugated sub nanometer microparticles is 942.51 nm, and the yield is 10.03%.

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