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CN-121987691-A - Preparation method of nanometer micropowder based on composite smelting purification of traditional Chinese medicine and sea salt

CN121987691ACN 121987691 ACN121987691 ACN 121987691ACN-121987691-A

Abstract

The application relates to the technical field of nano-material-based preparation, and in particular discloses a preparation method of nano-powder based on composite smelting and purification of traditional Chinese medicine and sea salt, which comprises the steps of matching astragalus mongholicus, ganoderma lucidum, barbed skullcap herb, oldenlandia diffusa, red-rooted salvia root, ligusticum wallichii and deep sea salt according to the principle of monarch, minister, assistant and guide in traditional Chinese medicine; the preparation method comprises the steps of obtaining traditional Chinese medicine extract powder by supercritical CO2 extraction and vacuum freeze drying, obtaining high-purity sea salt mineral concentrate by electrolytic purification and molecular distillation, mixing the two in a ratio of 3:1 to 5:1, preparing composite micro powder with a particle size of 50-200 nanometers by high-energy ball milling and jet milling, and establishing a quality control system comprising properties, identification, content measurement and stability. By the technical scheme, the application realizes the efficient compounding of the active ingredients of the traditional Chinese medicine and sea salt minerals, remarkably improves the bioavailability, the treatment effect and the product stability of the medicine, and provides a safe and efficient novel nanometer traditional Chinese medicine formulation for treating tumors and chronic diseases.

Inventors

  • LI XIAOCHENG
  • WANG XIAOMING
  • LIU XIANGYANG

Assignees

  • 西杭医学研究(杭州)有限公司

Dates

Publication Date
20260508
Application Date
20251230

Claims (10)

  1. 1. The preparation method of the nanometer micro powder based on the composite smelting and purification of the traditional Chinese medicine and the sea salt is characterized by comprising the following specific steps: step 1, selecting and matching raw materials, namely selecting astragalus, ganoderma lucidum, barbed skullcap herb, oldenlandia diffusa, medicinal materials of red sage root and ligusticum wallichii for activating blood and dissolving stasis, and simultaneously selecting sea salt raw materials which are taken from a deep sea pollution-free area and are rich in trace elements, and matching according to the principle of monarch, minister, assistant and guide of traditional Chinese medicine; step 2, extracting the effective components of the traditional Chinese medicine, extracting the effective components in the traditional Chinese medicine by adopting supercritical fluid extraction, and combining a vacuum freeze drying process to obtain traditional Chinese medicine extract powder; step 3, sea salt mineral purification, namely, performing electrolytic purification treatment on sea salt raw materials, and then obtaining high-purity mineral concentrate through a molecular distillation technology; Step 4, preparing composite micropowder, namely mixing the traditional Chinese medicine extract powder obtained in the step 2 with the high-purity mineral concentrate obtained in the step 3 according to an optimized proportion, and preparing nanoscale composite micropowder by a high-energy ball milling technology and a pneumatic jet milling technology; step 5, detecting the product performance, namely detecting the particle size distribution of the final product by using a laser particle size analyzer, and ensuring the particle size distribution to be in the range of 50-200 nanometers; And 6, physical and chemical characteristic analysis, namely observing the physical and chemical characteristics of the micropowder by a scanning electron microscope, confirming a crystal structure formed by the active ingredients of the traditional Chinese medicine and sea salt minerals by adopting X-ray diffraction analysis, performing an in-vitro dissolution experiment to evaluate dissolution performance, and performing a stability experiment to verify the retention rate of the active ingredients in the shelf life of the product.
  2. 2. The method for preparing nanometer powder based on traditional Chinese medicine and sea salt composite smelting purification according to claim 1, wherein in the step 1, the traditional Chinese medicine is prepared from 15 to 25 parts by weight of astragalus mongholicus, 10 to 20 parts by weight of ganoderma lucidum, 8 to 15 parts by weight of sculellaria barbata, 5 to 12 parts by weight of oldenlandia diffusa, 8 to 15 parts by weight of red-rooted salvia root, 5 to 10 parts by weight of ligusticum wallichii, and the sea salt mineral addition amount is 5 to 15 parts by weight of the total weight.
  3. 3. The method for preparing nanometer powder based on traditional Chinese medicine and sea salt composite smelting purification according to claim 1, wherein the supercritical fluid extraction technology in the step 2 adopts carbon dioxide as supercritical fluid, the extraction pressure is 20-35 MPa, the extraction temperature is 35-55 ℃, the extraction time is 2-4 hours, the entrainer is ethanol solution with the volume concentration of 70-90%, the prefreezing temperature of the vacuum freeze drying process is minus 40-minus 60 ℃, the prefreezing time is 2-4 hours, the vacuum degree of the sublimation drying stage is 10-50 Pa, and the material temperature of the analytical drying stage is not more than 40 ℃.
  4. 4. The method for preparing nanometer powder based on traditional Chinese medicine and sea salt composite smelting purification, which is disclosed in claim 1, is characterized in that in the step 3, an ion exchange membrane electrolytic tank is adopted for electrolytic purification treatment, the electrolytic voltage is 3-5V, the current density is 100-200 amperes per square meter, the temperature of electrolyte is 25-45 ℃, a wiped film molecular distillation device is adopted for the molecular distillation technology, the evaporation temperature is 80-120 ℃, the vacuum degree is 0.1 Pa-1 Pa, the feeding rate is 1 ml-3 ml per minute, and the cooling medium temperature is 5-15 ℃.
  5. 5. The method for preparing nanometer powder based on the composite smelting purification of traditional Chinese medicine and sea salt according to claim 1, wherein the mass ratio of the traditional Chinese medicine extract powder to the high-purity mineral concentrate in the step 4 is 3:1 to 5:1, the high-energy ball milling process adopts zirconia ball milling media, the ball material ratio is 10:1 to 15:1, the ball milling rotating speed is 300-500 rpm, and the ball milling time is 4-8 hours.
  6. 6. The method for preparing nanometer powder based on the composite smelting purification of Chinese medicine and sea salt according to claim 5, wherein the jet milling technology adopts a fluidized bed jet mill, the milling pressure is 0.6 megapascal to 1.0 megapascal, the feeding rate is 2 kg per hour to 5 kg per hour, and the rotating speed of a classification wheel is 3000 rpm to 6000 rpm.
  7. 7. The method for preparing nanometer powder based on the composite smelting purification of traditional Chinese medicine and sea salt according to claim 1, wherein the laser particle size analyzer in the step 5 adopts a wet dispersion mode, a dispersion medium is deionized water, 0.1-0.5% of sodium dodecyl sulfate is added as a dispersing agent, the ultrasonic dispersion time is 3-5 minutes, the measuring angle is 90 degrees, and the measuring times are 3 times for averaging.
  8. 8. The method for preparing nanometer powder based on traditional Chinese medicine and sea salt composite smelting purification according to claim 1, wherein in the step 6, a scanning electron microscope is adopted for scanning electron microscope observation, the accelerating voltage is 5-15 kv, the working distance is 8-12 mm, the sample is fixed by conductive adhesive and subjected to metal spraying treatment, the metal spraying thickness is 10-20 nm, the X-ray diffraction analysis adopts copper target K alpha rays, the tube voltage is 40 kv, the tube current is 40 mA, the scanning range is 5-80 degrees, the scanning speed is 2 degrees per minute, and the step length is 0.02 degrees.
  9. 9. The method for preparing the nanometer powder based on the composite smelting purification of the traditional Chinese medicine and the sea salt, which is disclosed in claim 1, is characterized in that in the step 6, an in vitro dissolution experiment adopts a spin basket method, a dissolution medium is hydrochloric acid solution with a pH value of 1.2 and phosphate buffer with a pH value of 6.8, the volume of the dissolution medium is 900 milliliters, the rotation speed is 50-100 revolutions per minute, the temperature is 37 ℃ and is 0.5 ℃ and the sampling time is 5 minutes, 10 minutes, 15 minutes, 30 minutes, 45 minutes and 60 minutes, the stability experiment comprises an acceleration experiment and a long-term experiment, the acceleration experiment condition is that the temperature is 40 ℃ and 2 ℃, the relative humidity is 75% and 5%, the long-term experiment condition is that the temperature is 25 ℃ and 2 ℃, the relative humidity is 60% and 5%, the test period is 6 months, and the sampling and the detection are carried out once every month.
  10. 10. The method for preparing nanometer powder based on the compound smelting and purifying of Chinese medicine and sea salt according to claim 1, further comprising establishing quality control standards, wherein the quality control standards comprise properties, identification, inspection, content measurement and microorganism limitation items, and the content measurement adopts high performance liquid chromatography to simultaneously measure the contents of astragaloside IV, ganoderic acid and barbed skullcap herb alkaloid.

Description

Preparation method of nanometer micropowder based on composite smelting purification of traditional Chinese medicine and sea salt Technical Field The invention belongs to the technical field of nano material preparation, and in particular relates to a preparation method of nano micro powder based on composite smelting and purification of traditional Chinese medicine and sea salt. Background Along with the acceleration of the modernization process of traditional Chinese medicine, the combination of traditional Chinese medicine and modern material science and nanotechnology has become a key path for improving the curative effect and clinical applicability of traditional Chinese medicine. The traditional Chinese medicine compound has unique potential in preventing and treating tumor and chronic diseases by virtue of the advantages of multiple components, multiple targets and overall regulation, but is limited by the problems of low bioavailability, slow dissolution of active ingredients, uneven in-vivo distribution and the like of the traditional formulation, and the clinical conversion efficiency is restricted for a long time. Meanwhile, the marine mineral resources such as sea salt are rich in various microelements with physiological activities, show a synergistic effect in the aspects of immunoregulation, antioxidation and microenvironment steady state maintenance, and provide a new material basis for the functional expansion of the traditional Chinese medicine preparation. The preparation technology of the nanometer micro powder based on the composite smelting and purifying of the traditional Chinese medicine and sea salt aims to realize the efficient integration and structural reconstruction of the active ingredients and mineral elements of the traditional Chinese medicine by a physical and chemical means. The technical direction focuses on improving the drug solubility, permeability and targeted enrichment capacity by utilizing the nanoscale effect, and simultaneously constructing a novel drug delivery system with dual functions of treatment and conditioning by means of the regulation and control effects of elements such as magnesium, zinc, selenium and the like in sea salt on cell metabolism and immune functions. The core of the method is that a stable composite structure is formed by the traditional Chinese medicine extract and the high-purity sea salt mineral under the nanoscale by a specific process, so that pharmacodynamic release dynamics is optimized and the multi-target synergistic effect is enhanced. However, the existing traditional Chinese medicine nanocrystallization technology generally has the problems of serious component loss, unstable crystal form, wide particle size distribution and the like, and consistency among batches and clinical repeatability are difficult to ensure. The traditional crushing or embedding method can not realize the effective fusion of the complex components of the traditional Chinese medicine and inorganic mineral substances, so that the composite system is easy to generate phase separation or activity attenuation in the gastrointestinal environment. In addition, the lack of special purification and smelting technology for a traditional Chinese medicine-mineral composite system makes the final product difficult to combine high purity, high dispersibility and good stability, and severely restricts the application potential of the final product in accurate treatment of tumors and chronic diseases. Therefore, a preparation method of nanometer micro powder capable of realizing efficient combination of traditional Chinese medicine and sea salt, controllable structure and stable performance is needed. Disclosure of Invention The invention aims to provide a preparation method of nanometer micropowder based on composite smelting purification of traditional Chinese medicine and sea salt, which can effectively solve the problems in the background technology. In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: A preparation method of nanometer micropowder based on traditional Chinese medicine and sea salt composite smelting purification comprises the following specific steps: Step 1, selecting and matching raw materials, namely selecting Chinese medicinal materials with definite antitumor activity, including astragalus membranaceus, ganoderma lucidum, barbed skullcap herb, oldenlandia diffusa, medicinal materials with functions of promoting blood circulation and removing blood stasis, namely salvia miltiorrhiza and ligusticum wallichii, and simultaneously selecting sea salt raw materials which are taken from a deep sea pollution-free area and are rich in more than 60 trace elements, matching according to a monarch, minister, assistant and guide principle of traditional Chinese medicine, taking astragalus membranaceus and ganoderma lucidum as monarch, performing functions of strengthening body resistance and consolidating constit