Purification processing method of traditional Chinese medicine decoction pieces
Through a means combining biological, chemical and physical technology, the problems of incomplete removal of ingredients and toxins in traditional Chinese herbal medicine processing methods are solved, and efficient purification of Chinese herbal medicines and retention of active ingredients are achieved.
Patent Information
- Application Number
- CN202510247072.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-04
- Publication Date
- 2025-05-23
AI Technical Summary
Traditional Chinese herbal medicine processing methods have problems such as serious loss of active ingredients, incomplete removal of toxins and blank treatment of aged medicinal materials, especially the poor treatment effect of stubborn aflatoxin (AFB1).
A Chinese herbal medicine purification and processing method is adopted, including medicinal material grading screening and ultrasonic cleaning, alkali-acid synergistic toxin activation treatment, Rhodococcus-complexase co-immobilization biological reaction, gradient solvent extraction and supercritical purification, low-temperature negative pressure drying and pulsed ultraviolet sterilization.
Through the triple defense line of "biodegradation-chemical activation-physical extraction", the toxin molecular structure is systematically destroyed and directionally cleared, significantly reducing the risk of hepatotoxicity and carcinogenicity, while maximizing the effective ingredients in the medicinal materials, ensuring the quality and safety of Chinese herbal medicines.
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Figure CN120022300A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of purification of traditional Chinese medicines, and in particular to a purification and processing method for traditional Chinese medicine pieces. Background Art
[0002] Chinese herbal medicine slices are preparations that can be directly used in clinical practice after processing. Their quality directly affects the effectiveness of Chinese medicine diagnosis and treatment. Traditional processing methods mostly rely on high-temperature steaming and frying to reduce the toxicity of medicinal materials through the effect of moisture and heat. For example, aconite medicinal materials need to be hydrolyzed by high temperature to reduce the toxicity of diester alkaloids. However, this process has significant defects: for example, the loss of effective ingredients is serious: volatile components (such as peppermint oil and perillyl alcohol) escape at high temperatures, and heat-sensitive substances (such as glycosides and enzymes) are easily decomposed and inactivated. Toxin removal is not thorough: aflatoxin (AFB1) is resistant to high temperatures (the decomposition temperature must be ≥268°C), and conventional steaming and frying cannot effectively degrade it. Long-term intake can cause liver cancer. There is a gap in the processing of aged medicinal materials: In order to ensure production continuity, enterprises need to stockpile medicinal materials for a long time, but the AFB1 contamination rate of Chinese medicinal materials stored for more than 1 year is as high as 30%, and traditional processes have no targeted solutions for this.
[0003] Most existing technologies use a single method to deal with the toxin problem, but they all have limitations: Among them, the chemical method: Sodium hydroxide is used to degrade toxins, but strong alkali can easily destroy the fiber structure of medicinal materials, leading to denaturation of polysaccharides and proteins. Biological method: Rhodococcus is used to degrade toxins, but the targeting of fat-soluble AFB1 is poor, and the bacteria are difficult to reuse. Physical method (such as supercritical extraction): Although it can selectively extract toxins, the equipment cost is high, and the removal rate of bound toxins (such as AFB1 bound to the cell wall) is less than 50%. Therefore, it is necessary to design a purification and processing method for Chinese herbal medicines to solve the above problems. Summary of the invention
[0004] In order to solve the above technical problems, the present invention proposes a purification and processing method for Chinese herbal medicine slices.
[0005] To achieve the above object, the present invention provides the following solutions:
[0006] A purification and processing method for Chinese herbal medicine slices, comprising:
[0007] S1. Classification and screening of medicinal materials and ultrasonic cleaning: Classify the medicinal materials according to their parts or years, and place them in the ultrasonic cleaning machine for processing;
[0008] S2, alkali-acid synergistic toxin activation treatment: using alkali to denature aflatoxin, and then using acid to neutralize the alkalinity;
[0009] S3, Rhodococcus-complex enzyme co-immobilization biological reaction; using bacterial enzyme co-immobilized microspheres to prepare embedded Chinese herbal medicine slices to remove aflatoxin;
[0010] S4, gradient solvent extraction and supercritical purification; using the solvent to further absorb the residual aflatoxin in the Chinese herbal medicine pieces;
[0011] S5, low temperature negative pressure drying and pulse ultraviolet sterilization.
[0012] Preferably, in step S1, the medicinal material classification standard is:
[0013] Root vegetables: storage period ≤ 3 years, water content ≤ 12%;
[0014] Fruits: storage period ≤ 2 years, sugar content ≥ 15%;
[0015] Leaves: Storage period ≤ 1 year, chlorophyll retention rate ≥ 80%;
[0016] The cleaning solution for ultrasonic cleaning is 0.1% tea polyphenols solution;
[0017] Processing time: 15 minutes for rhizomes, 8 minutes for leaves, 10 minutes for fruits.
[0018] Preferably, in step S2,
[0019] Alkaline treatment: the medicinal material was immersed in a 2% NaOH solution at 45°C and shaken at 200 rpm for 90 s to destroy the AFB1 lactone ring structure;
[0020] Acid neutralization: add 10% citric acid solution to adjust the pH to 6.8, let stand for 60 seconds to neutralize the residual alkali and chelate the metal ions to prevent oxidation reaction;
[0021] Water washing: countercurrent rinsing process is adopted, with a water-to-material ratio of 5:1, and three-stage gradient washing is performed until the conductivity is ≤50μS / cm.
[0022] Preferably, in step S3,
[0023] Preparation of bacterial enzyme co-immobilized microspheres: Carrier composition: 3% sodium alginate, 5% chitosan, nano-SiO 2 0.2%;
[0024] Bacterial enzyme load: Rhodococcus erythropolis inoculation amount 10 8 CFU / g, complex enzyme immobilized by adsorption-cross-linking method;
[0025] Molding process: dripping 3% CaCl 2 The solution solidified for 30 min, the microsphere size was 2.0 ± 0.2 mm, and the bacterial survival rate was ≥ 90%;
[0026] Dynamic embedding reaction: slice the medicinal material into 2mm-3mm thick slices and put them into the airlift bioreactor with microspheres at a ratio of 1:5;
[0027] Reaction parameters: temperature 32°C, dissolved oxygen 5 mg / L, stirring rate 150 rpm, time 24 h;
[0028] Feeding strategy: add 0.1% glucose and 0.05% yeast extract powder every 6 hours to maintain the metabolic activity of the bacteria.
[0029] Preferably, primary extraction: solvent composition: acetone-n-hexane ratio is 1:4, solid-liquid ratio is 1:8, stirring at 40°C for 60min;
[0030] Secondary extraction: solvent composition: 0.5% Tween 80 in ethanol, ultrasonic-assisted treatment for 20 min;
[0031] Three-stage extraction: Parameters: pressure 25MPa, temperature 45℃, CO 2 Flow rate 20L / min, time 90min;
[0032] Secondary centrifugation: The centrifuge was operated at a speed of 20,000 rpm and a temperature of 4°C for 30 min to separate the solvent-aflatoxin complex.
[0033] Preferably, in step 5, low temperature negative pressure drying and pulse ultraviolet sterilization segmented drying are performed:
[0034] The first stage: drying to a moisture content of 15% at 40°C and vacuum degree -0.08MPa;
[0035] The second stage: 30℃, 30% humidity for 4 hours to allow the internal moisture gradient to diffuse, and the final moisture content is ≤8%;
[0036] Pulse UV sterilization: Parameters: wavelength 254nm, pulse cycle 5s on / 2s off, cumulative dose 8000μW·s / cm 2 .
[0037] Compared with the prior art, the present invention has the following advantages and technical effects:
[0038] 1. Comprehensive and thorough removal of toxins, and leapfrog improvement in safety
[0039] In order to eliminate stubborn aflatoxins (AFB1) and other harmful substances in aged medicinal materials, the technology breaks through the single method of traditional high-temperature steaming and frying, and systematically disintegrates the molecular structure of toxins and removes them in a targeted manner through the triple defense of "biodegradation-chemical activation-physical extraction". Compared with the limitation that traditional processes can only deal with free toxins, this technology can deeply remove complex forms of toxins such as bound and fat-soluble toxins, eliminate the hidden dangers of drug safety from the root, and significantly reduce the risks of hepatotoxicity and carcinogenicity.
[0040] 2. The medicinal ingredients are completely preserved and the quality is restored to its natural properties
[0041] Abandoning the "extensive" processing mode of high temperature and high pressure, the low-temperature biological reaction and intelligent temperature control drying technology are adopted to retain the volatile essential oils, heat-sensitive active ingredients (such as saponins, flavonoids) and natural colors in the medicinal materials to the maximum extent. The medicinal properties of the processed pieces are closer to the original medicinal materials, and the loss rate of effective ingredients is reduced by more than 80% compared with the traditional process, ensuring that the theoretical basis of "differentiation and treatment" in clinical Chinese medicine can be accurately implemented.
[0042] 3. Universal compatibility of complex medicinal materials to solve common problems in the industry
[0043] In view of the differences in characteristics of medicinal materials of different textures such as rhizomes, fruits, and whole herbs, the technology realizes flexible processing of "one material, one policy" through a modular process parameter adjustment system (such as solvent polarity gradient and dynamic optimization of bacterial enzyme ratio). Especially for aged medicinal materials stored for more than 3 years, it can effectively reverse the oxidation and mildew deterioration of ingredients caused by long-term storage, providing a new path for the sustainable use of Chinese medicine resources.
[0044] 4. Green process closed-loop operation to promote low-carbon transformation of the industry
[0045] The core technology uses renewable biological resources (Rhodococcus) and a circulating solvent system. The bacterial enzyme carrier can be reused more than 5 times, the organic solvent recovery rate exceeds 85%, and the waste discharge is reduced by 60%. At the same time, supercritical CO 2 The application of extraction and pulsed ultraviolet sterilization technology completely gets rid of the traditional process's excessive dependence on fossil energy and chemical reagents. BRIEF DESCRIPTION OF THE DRAWINGS
[0046] The drawings constituting a part of the present application are used to provide a further understanding of the present application. The illustrative embodiments and descriptions of the present application are used to explain the present application and do not constitute an improper limitation on the present application. In the drawings:
[0047] Figure 1 It is a process flow chart of the present invention. DETAILED DESCRIPTION
[0048] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present application will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.
[0049] It should be noted that all components in the technical solution of this application require the necessary additional facilities of water supply, oil supply, electricity supply and gas supply to be driven and / or controlled. If there is no further explanation, it is assumed that the existing technology is used and equipped without special explanation.
[0050] It should be noted that, in order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments.
[0051] Embodiment 1:
[0052] Depend on Figure 1 A purification and processing method for Chinese herbal medicine pieces shown comprises the following steps:
[0053] Step 1: Classification and ultrasonic cleaning
[0054] Classification of medicinal materials:
[0055] Roots and tubers (such as Angelica sinensis and Astragalus membranaceus): storage period ≤ 3 years, water content ≤ 12%.
[0056] Fruits (such as wolfberry and hawthorn): storage period ≤ 2 years, sugar content ≥ 15%.
[0057] Leaves (such as mint and mugwort): storage life ≤ 1 year, chlorophyll retention rate ≥ 80%.
[0058] Ultrasonic cleaning:
[0059] Equipment parameters: frequency 40kHz, power 300W, cleaning liquid is 0.1% tea polyphenol solution (antibacterial and antioxidant).
[0060] Processing time: 15 minutes for rhizomes, 8 minutes for leaves, and 10 minutes for fruits.
[0061] Technical effect: Ultrasonic cavitation removes surface mold spores and pollutants, and tea polyphenols inhibit oxidation reactions during the cleaning process.
[0062] Step 2: Alkali-acid synergistic toxin activation
[0063] Alkali treatment:
[0064] The medicinal material was immersed in a 1.2% NaOH solution (45° C.) and shaken at 200 rpm for 90 seconds to destroy the AFB1 lactone ring structure (reaction formula: AFB1+NaOH→AFB1-8,9-epoxide).
[0065] Acid neutralization:
[0066] Add 10% citric acid solution to adjust the pH to 6.8 and let stand for 60 seconds to neutralize the residual alkali and chelate metal ions (such as Fe 3+ , Cu 2+ ), to prevent oxidation reaction.
[0067] Washable:
[0068] The countercurrent rinsing process was adopted with a water-to-solid ratio of 5:1, and the gradient cleaning was carried out in three stages (pH 7.0→6.5→6.0) until the conductivity was ≤50μS / cm.
[0069] Innovation: NaOH concentration and treatment time were optimized by orthogonal experiment (L9(3 4 )), while ensuring the activation of toxins, the loss rate of medicinal polysaccharides is less than 3%.
[0070] Step 3: Rhodococcus-complex enzyme co-immobilization bioreaction
[0071] Preparation of bacterial enzyme co-immobilized microspheres:
[0072] Carrier composition: sodium alginate 3% (w / v), chitosan 1.5% (w / v), nano-SiO 2 0.2% (to enhance mechanical strength).
[0073] Bacterial enzyme loading: Rhodococcus erythropolis (CGMCC 1.1781) inoculation volume 10 8 CFU / g, the complex enzyme (phospholipase A 18 mg / L + proteinase K 12 mg / L) was immobilized by adsorption-cross-linking method.
[0074] Molding process: dripping 3% CaCl 2 The solution solidified for 30 minutes, the microsphere particle size was 2.0±0.2mm, and the bacterial survival rate was ≥90%.
[0075] Dynamic embedding reaction:
[0076] The medicinal material slices (thickness 2 mm) and microspheres were placed into the airlift bioreactor at a ratio of 1:5 (w / w).
[0077] Reaction parameters: temperature 32°C, dissolved oxygen 5 mg / L (controlled by microporous aeration), stirring rate 150 rpm, time 24 h.
[0078] Feeding strategy: add 0.1% glucose + 0.05% yeast extract powder every 6 hours to maintain the metabolic activity of the bacteria.
[0079] Technical principle:
[0080] The peroxidase (POD) secreted by Rhodococcus catalyzes the furan ring opening reaction of AFB1 to generate the low-toxic metabolite AFB1-8,9-dihydrodiol (confirmed by LC-MS / MS).
[0081] The complex enzyme hydrolyzes cell wall cellulose and pectin, releasing bound toxins and improving degradation efficiency.
[0082] Step 4: Gradient solvent extraction and supercritical purification
[0083] Primary extraction (polar solvent):
[0084] Solvent composition: acetone-n-hexane (1:4, v / v), solid-liquid ratio 1:8, stirring at 40°C for 60 min.
[0085] Objective: To remove water-soluble toxins (such as ochratoxin A) and free AFB1.
[0086] Secondary extraction (surfactant assisted):
[0087] Solvent composition: 0.5% Tween 80 in ethanol solution, ultrasonic-assisted (300 W, 40 kHz) treatment for 20 min.
[0088] Objective: To extract cell membrane-bound AFB1 by micellar solubilization.
[0089] Three-stage extraction (supercritical CO 2 ):
[0090] Parameters: pressure 25MPa, temperature 45℃, CO 2 Flow rate: 20L / min, time: 90min.
[0091] Objective: To selectively extract fat-soluble toxins (such as aflatoxin M1) and collect the bottom residue.
[0092] Differential centrifugation purification:
[0093] First stage centrifugation: 8000rpm, 10min, to remove plant residues.
[0094] Secondary centrifugation: 20,000 rpm, 4°C, 30 min, to separate the solvent-toxin complex, with a toxin removal rate of ≥98%.
[0095] Step 5: Low temperature negative pressure drying and pulsed UV sterilization
[0096] Sectional drying:
[0097] The first stage: 40°C, vacuum degree -0.08MPa, drying to a moisture content of 15% (to prevent surface crusting).
[0098] The second stage: 30℃, 30% humidity for 4 hours to allow the internal moisture gradient to diffuse and the final moisture content ≤8%.
[0099] Pulsed UV sterilization:
[0100] Parameters: wavelength 254nm, pulse period 5s on / 2s off, cumulative dose 8000μW·s / cm 2 .
[0101] Advantages: Compared with continuous irradiation, pulse mode can reduce the temperature rise of medicinal materials (ΔT≤3℃) and avoid browning caused by Maillard reaction.
[0102] Further, the extraction process in step 4 is specifically as follows:
[0103] Primary extraction: polar solvent targeted extraction (removal of water-soluble and free toxins)
[0104] Solvent system:
[0105] Composition: Acetone (polar solvent) and n-hexane (non-polar solvent) are mixed in a volume ratio of 1:4.
[0106] Mechanism of action:
[0107] Acetone (polarity index 5.1) can effectively dissolve water-soluble toxins (such as ochratoxin A) and some free AFB1;
[0108] n-Hexane (polarity index 0.1) is used as a co-solvent to reduce the polarity of the mixed solvent and prevent the fat-soluble components (such as volatile oils) in the medicinal materials from being excessively extracted.
[0109] Basis for solvent ratio optimization: Response surface methodology (RSM) experiments determined that when the acetone ratio exceeded 25%, the volatile oil loss rate increased significantly (>10%), so a 1:4 ratio was selected to balance toxin removal and component retention.
[0110] Operation process:
[0111] Material-liquid ratio: The mass ratio of medicinal materials to solvent is 1:8.
[0112] Processing conditions:
[0113] Temperature: 40℃ (temperature control accuracy ±1℃), to avoid high temperature causing solvent volatilization;
[0114] Stirring rate: 300 rpm, time 60 min, to ensure that the solvent fully penetrates the medicinal material slices.
[0115] End point determination: The concentration change of AFB1 in the solvent was detected by HPLC, and the extraction was terminated when the difference between two consecutive samples was less than 5%.
[0116] Separation and recycling:
[0117] The upper layer of solvent-toxin mixture was separated by decantation, and the lower layer of medicinal materials entered the secondary extraction.
[0118] Solvent recovery: Acetone-n-hexane was recovered by rotary evaporation (40°C, -0.09 MPa), with a recovery rate of ≥85%.
[0119] Secondary extraction: Surfactant-assisted ultrasonic extraction (removal of bound toxins)
[0120] Solvent system:
[0121] Composition: 0.5% Tween 80 ethanol solution (volume fraction 75%).
[0122] Mechanism of action:
[0123] Tween 80, as a nonionic surfactant, formed micelles (critical micelle concentration CMC = 0.012%) and solubilized cell wall-bound AFB1;
[0124] Ethanol (polarity index 5.2) destroys the phospholipid bilayer of the herbal cell membrane, releasing bound toxins;
[0125] Ultrasonic cavitation effect (40kHz, 300W) generates microjets to accelerate solvent penetration.
[0126] Operation process:
[0127] Material-liquid ratio: The mass ratio of medicinal materials to solvent is 1:10.
[0128] Processing conditions:
[0129] Ultrasonic power: 300 W, frequency 40 kHz, treatment time 20 min (pulse mode: working 5 s, rest 2 s);
[0130] Temperature: 35°C (controlled by circulating water in the jacket).
[0131] End point determination: The process is terminated when the AFB1 concentration in the solvent reaches 80% of that in the primary extract.
[0132] Separation and recycling:
[0133] The solid and liquid phases were separated by centrifugal filtration (4000 rpm, 10 min), and the liquid phase was collected for toxin enrichment;
[0134] Solvent recovery: Ethanol was recovered by vacuum distillation (50°C, -0.08 MPa), and Tween 80 was recovered and reused through an ultrafiltration membrane (molecular weight cutoff 10 kDa).
[0135] Three-stage extraction: supercritical CO 2 Selective extraction (removal of fat-soluble residual toxins)
[0136] Supercritical CO 2 parameter:
[0137] Pressure: 25MPa (critical pressure 7.38MPa, supercritical state ensures high diffusivity);
[0138] Temperature: 45°C (critical temperature 31.1°C, higher than the critical point to maintain supercritical state);
[0139] Entrainer: 5% ethanol (volume fraction) was added as a polar modifier to improve the solubility of AFB1.
[0140] Operation process:
[0141] Loading: Load the medicinal materials after secondary extraction into the extraction kettle, with a bulk density of ≤0.4g / cm 3 To ensure CO 2 Even flow;
[0142] Dynamic extraction:
[0143] CO 2 Flow rate: 20L / min (standard state), extraction time 90min;
[0144] Separation kettle parameters: pressure 6MPa, temperature 30℃, CO 2 The extract is evaporated and precipitated.
[0145] Collection: The fat-soluble residue containing toxins is collected from the bottom of the separation kettle, and the medicinal materials are retained in the extraction kettle.
[0146] CO 2 cycle:
[0147] Gaseous CO 2 After being liquefied by the condenser (-10℃), it returns to the storage tank, and the recycling rate is ≥95%;
[0148] System losses through liquid CO 2 Automatic refilling of the tank.
[0149] Differential Centrifugation Purification Process
[0150] First stage centrifugation (coarse separation):
[0151] Parameters: 8000rpm, 10min, room temperature;
[0152] Purpose: To remove large impurities (particle size > 50 μm) such as medicinal material fragments and plant fibers;
[0153] Equipment: Horizontal screw centrifuge, differential speed 15rpm, liquid phase clarity ≥90% (turbidity ≤20NTU).
[0154] Secondary centrifugation (fine separation):
[0155] Parameters: 20000rpm, 30min, 4℃;
[0156] Purpose: To separate solvent-toxin complex (particle size 0.1-1 μm) from the active ingredients of medicinal materials;
[0157] Critical Control Points:
[0158] The centrifugation temperature is ≤4°C to prevent inactivation of heat-sensitive components (such as enzymes);
[0159] Titanium alloy rotor is used to avoid metal ion contamination.
[0160] Liquid Phase Processing:
[0161] After centrifugation, the liquid phase is divided into three layers:
[0162] Upper layer: lipid-soluble toxins (AFB1-enriched layer);
[0163] Middle layer: solvent-water mixed phase (containing a small amount of polar toxins);
[0164] Lower layer: Suspension of active ingredients of medicinal materials.
[0165] Separation strategy:
[0166] The upper liquid phase is drawn off for toxin inactivation treatment (e.g., ozone oxidation);
[0167] The middle liquid phase returns to the solvent recovery system;
[0168] The lower liquid phase is sterilized by a 0.22 μm filter membrane and then combined with the medicinal materials to enter the drying process.
[0169] 3. Process synergy analysis
[0170] Polarity Gradient Design:
[0171] Acetone-n-hexane (polarity index 5.1→0.1)→ethanol-Tween 80 (polarity index 5.2+ micellar solubilization)→supercritical CO 2 (polarity index ≈ 0), gradually covering the solubility range from polar to non-polar toxins.
[0172] Physical-chemical synergy:
[0173] Ultrasonic cavitation (physical effect) destroys cell structure, Tween 80 (chemical effect) solubilizes toxins, supercritical CO 2 (Physical dissolution) Selective extraction to form a multi-level detoxification network.
[0174] Toxin removal efficiency verification:
[0175] Detection method: HPLC-MS / MS (AFB1 quantification limit 0.1 μg / kg);
[0176] result:
[0177]
[0178]
[0179] Embodiment 2:
[0180] A modification additive based on diatomite, sepiolite and citric acid solution is prepared, wherein: 1. Raw material preparation:
[0181] Diatomaceous earth and sepiolite are mixed evenly in a mass ratio of 1:1 to 1:3 as the main adsorption matrix.
[0182] Prepare a citric acid solution with a mass concentration of 15%-20% as a modifier.
[0183] 2. Preliminary soaking:
[0184] The mixed diatomaceous earth and sepiolite are placed in the inner cavity of the reactor, and citric acid solution is added in a solid-liquid ratio of 1:4 to 1:6.
[0185] Stir and soak at room temperature (about 25°C) for 1-1.5 hours to ensure that the mixture is fully soaked.
[0186] 3. Heating reaction:
[0187] The internal temperature of the reactor is gradually raised to 80°C to 100°C, and the reaction is stirred and maintained in this temperature range for 2-3 hours to promote the chemical reaction between citric acid and the surfaces of diatomaceous earth and sepiolite to enhance the adsorption performance.
[0188] Addition of surfactant:
[0189] Sodium dodecylbenzene sulfonate (DBSAS) equivalent to 0.05%-0.1% of the total mass of the reactants is added into the reactor as a surfactant to improve the dispersibility and adsorption efficiency of the product.
[0190] Continue to raise the temperature to 120°C to 140°C, maintain the absolute vacuum degree less than 15Kpa, and stir the reaction for 1.5-2.5 hours to allow the surfactant to fully act.
[0191] 4. Washing and neutralization:
[0192] After the reaction is completed, the product is washed with deionized water until the pH value of the washing solution reaches 6-8 to remove excess citric acid and surfactant.
[0193] If necessary, a small amount of sodium hydroxide solution can be added to adjust the pH value to ensure that the final product is neutral or slightly alkaline, which is conducive to long-term storage and application.
[0194] 5. Drying and screening:
[0195] The washed product is dried, which may be done by hot air drying or vacuum drying, until the water content is less than 5%.
[0196] After drying, the modified auxiliary product with a particle size of 0.05 mm to 0.1 mm is obtained by sieving.
[0197] The modification aid is added to pure water to form a suspension, and the Chinese herbal medicine slices after step 3 or 4 are added thereto, and the mass ratio of the modification aid to water and the Chinese herbal medicine slices is 1-5:100:50 respectively. The mixing time is 30min-60min.
[0198] Then the mixture is passed into an electric field, the electric field parameters are electric field strength of 500-1500V / cm, and the sedimentation time is 20-60s. The modified auxiliary agent is used to adsorb aflatoxin, and the aflatoxin is separated by sedimentation under the action of the electric field, thereby achieving the re-purification of the Chinese herbal medicine slices.
[0199] The above are only preferred specific implementations of the present application, but the protection scope of the present application is not limited thereto. Any changes or substitutions that can be easily thought of by a person skilled in the art within the technical scope disclosed in the present application should be included in the protection scope of the present application. Therefore, the protection scope of the present application should be based on the protection scope of the claims.
Claims
1. A method for purifying and processing Chinese herbal medicine slices, characterized in that: include: S1. Classification and screening of medicinal materials and ultrasonic cleaning: Classify the medicinal materials according to their parts or years, and place them in the ultrasonic cleaning machine for processing; S2, alkali-acid synergistic toxin activation treatment: using alkali to denature aflatoxin, and then using acid to neutralize the alkalinity; S3, Rhodococcus-complex enzyme co-immobilization biological reaction; using bacterial enzyme co-immobilized microspheres to prepare embedded Chinese herbal medicine slices to remove aflatoxin; S4, gradient solvent extraction and supercritical purification; using the solvent to further absorb the residual aflatoxin in the Chinese herbal medicine pieces; S5, low temperature negative pressure drying and pulse ultraviolet sterilization.
2. The purification and processing method of Chinese herbal medicine slices according to claim 1, characterized in that: In step S1, the classification standard of medicinal materials is: Root vegetables: storage period ≤ 3 years, water content ≤ 12%; Fruits: storage period ≤ 2 years, sugar content ≥ 15%; Leaves: Storage period ≤ 1 year, chlorophyll retention rate ≥ 80%; The cleaning solution for ultrasonic cleaning is 0.1% tea polyphenols solution; Processing time: 15 minutes for rhizomes, 8 minutes for leaves, 10 minutes for fruits.
3. The purification and processing method of Chinese herbal medicine slices according to claim 1, characterized in that: In step S2, Alkali treatment: the medicinal material was immersed in 1.2% NaOH solution at 45°C and shaken at 200 rpm for 90 s to destroy the AFB1 lactone ring structure; Acid neutralization: add 10% citric acid solution to adjust the pH to 6.8, let stand for 60 seconds to neutralize the residual alkali and chelate the metal ions to prevent oxidation reaction; Water washing: countercurrent rinsing process is adopted, with a water-to-material ratio of 5:1, and three-stage gradient washing is performed until the conductivity is ≤50μS / cm.
4. The purification and processing method of Chinese herbal medicine slices according to claim 1, characterized in that: In step S3, Preparation of bacterial enzyme co-immobilized microspheres: Carrier composition: Sodium alginate 3%, chitosan 1.5%, nano-SiO2 0.2%; Bacterial enzyme load: Rhodococcus erythropolis inoculation amount 10 8 CFU / g, complex enzyme immobilized by adsorption-cross-linking method; Molding process: drip 3% CaCl2 solution and solidify for 30 minutes, microsphere particle size 2.0±0.2mm, bacterial survival rate ≥90%; Dynamic embedding reaction: slice the medicinal material into 2mm-3mm thick slices and put them into the airlift bioreactor with microspheres at a ratio of 1:5; Reaction parameters: temperature 32°C, dissolved oxygen 5 mg / L, stirring rate 150 rpm, time 24 h; Feeding strategy: add 0.1% glucose and 0.05% yeast extract powder every 6 hours to maintain the metabolic activity of the bacteria.
5. The method for purifying and processing Chinese medicinal pieces according to claim 1, characterized in that: The extraction process in step S4 includes: Primary extraction: solvent composition: acetone-n-hexane ratio of 1:4, solid-liquid ratio of 1:8, stirring at 40°C for 60 min; Secondary extraction: solvent composition: 0.5% Tween 80 in ethanol, ultrasonic-assisted treatment for 20 min; Three-stage extraction: parameters: pressure 25MPa, temperature 45℃, CO2 flow rate 20L / min, time 90min; Secondary centrifugation: The centrifuge was operated at a speed of 20,000 rpm and a temperature of 4°C for 30 min to separate the solvent-aflatoxin complex.
6. The purification and processing method of Chinese herbal medicine slices according to claim 1, characterized in that: In step 5, low temperature negative pressure drying and pulsed UV sterilization staged drying: The first stage: drying to a moisture content of 15% at 40°C and vacuum degree -0.08MPa; The second stage: 30℃, 30% humidity for 4 hours to allow the internal moisture gradient to diffuse, and the final moisture content is ≤8%; Pulsed UV sterilization: Parameters: wavelength 254nm, pulse period 5s on / 2s off, cumulative dose 8000μW·s / cm 2 .