Vegetable carbon dot oral cavity eliminating powder as well as preparation method and application thereof
By employing a low-temperature hydrothermal carbonization and high-pressure homogenization process using plant-derived carbon dots, the problems of low stability and low absorption rate of active ingredients in traditional oral instant powders have been solved, achieving efficient and safe preparation of oral instant powders.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- BEIJING XUHUA TIMES TECH CO LTD
- Filing Date
- 2026-03-16
- Publication Date
- 2026-05-12
AI Technical Summary
The active ingredients in traditional oral instant powders are easily degraded by the oral environment, have low mucosal absorption rates, and poor stability after dissolution. The introduction of nanomaterials may pose biosafety risks and is incompatible with the formulation process of herbal medicines.
A plant-derived carbon dot (PCD) preparation method was adopted, which involves low-temperature hydrothermal carbonization, ultrasonic crushing, centrifugal dialysis and other steps, combined with high-pressure homogenization and vacuum drying, to prepare a plant-derived carbon dot powder, ensuring the stability and absorption efficiency of the active ingredients.
It achieves efficient mucosal absorption of active ingredients, with fast dissolution speed and high stability, avoids the biosafety risks of nanomaterials, and is seamlessly integrated with traditional processes, reducing production costs.
Smart Images
Figure CN122005461A_ABST
Abstract
Description
Technical Field
[0001] This application belongs to the field of oral instant dissolving preparation technology, and particularly relates to a plant-based carbon spot oral disinfectant powder, its preparation method and application. Background Technology
[0002] Oral-dissolving formulations, as an important component of modern drug delivery systems, are widely used in oral mucosal drug delivery. However, traditional oral-dissolving powders suffer from several technical bottlenecks: active ingredients are easily degraded by the oral environment (e.g., flavonoids and alkaloids are rapidly inactivated by salivary enzymes), mucosal absorption is low (usually <50%), and post-dissolution stability is poor (e.g., prone to aggregation or precipitation). Current technologies often add nanomaterials (such as metal nanoparticles and silica nanoparticles) to improve solubility and absorption efficiency; however, these nanomaterials may introduce biosafety risks (e.g., metal ion toxicity, accumulation effects of nanoparticles in vivo), and have poor compatibility with plant components, making them difficult to integrate with traditional herbal medicine formulation processes.
[0003] Conventional carbon dot preparation processes (such as high-temperature calcination and microwave methods) are typically carried out at high temperatures (>500℃), which leads to the destruction of the structure of plant active ingredients, making it difficult to retain their original biological activity and functional groups (such as hydroxyl and carboxyl groups). Furthermore, these processes are incompatible with herbal drug formulation processes, requiring additional separation and purification steps, increasing production costs and complexity. Therefore, there is an urgent need to develop a carbon dot preparation method that can both preserve plant active ingredients and seamlessly integrate with formulation processes to address the issues of active ingredient stability, mucosal absorption efficiency, and post-dissolution stability in oral instant dissolving preparations. Summary of the Invention
[0004] To overcome the aforementioned deficiencies in the existing technology, this application provides a plant-based carbon dot powdering agent, its preparation method, and its application. By using plant-derived carbon dots (PCDs), the stability and absorption efficiency of active ingredients are improved, achieving seamless integration of carbon dot preparation with the original process, avoiding side effects such as agglomeration and decreased solubility, and establishing a precise addition and homogeneous dispersion control system at the ten-thousand-level.
[0005] To achieve the above-mentioned objectives, this application provides the following technical solution:
[0006] On the one hand, this application provides a method for preparing a plant-based carbon spot desiccant, comprising the following steps:
[0007] (1) The plant powder was split into two parts, which were used for carbon dot preparation and subsequent processing, respectively;
[0008] (2) The plant powder used for carbon dot preparation is mixed with water to obtain a suspension;
[0009] (3) The suspension is placed in a polytetrafluoroethylene reactor for carbonization reaction;
[0010] (4) The carbonization reaction products were ultrasonically crushed and centrifuged in sequence, and the supernatant was dialyzed to obtain plant carbon dots;
[0011] (5) The plant powder used for subsequent processing in step (1) is nano-pulverized, and the nano-pulverized material is mixed with water to obtain a plant-based dispersion.
[0012] (6) The plant-based carbon dots are mixed with the plant-based dispersion, and then stirred, ultrasonically dispersed, homogenized and dried in sequence to obtain the plant-based carbon dots powder removal agent.
[0013] Optionally, in step (1), the plant powder is derived from at least one of Ganoderma lucidum spores, Astragalus membranaceus, Salvia miltiorrhiza, Polygonatum sibiricum, black wolfberry, honeysuckle, licorice, Angelica sinensis, and ginseng.
[0014] The particle size of the plant powder is 8~12μm;
[0015] The amount of plant powder used for carbon dot preparation is 5-10% of the total mass of plant powder.
[0016] In this application, the plant powder is diverted by setting a diversion valve or diversion pipe, diverting 5-10% of the total powder to the carbon dot preparation system. The diversion process is realized by an automated control system to ensure that the diversion ratio is precise and controllable.
[0017] Optionally, in step (2), the mass concentration of the plant powder used for carbon dot preparation in the suspension is 5-10%.
[0018] Optionally, in step (3), the filling degree of the suspension in the polytetrafluoroethylene reactor is 70-80%;
[0019] The carbonization reaction temperature is 180~220℃;
[0020] The carbonization reaction takes 6 to 12 hours.
[0021] In this application, by controlling the filling degree of the reactor to 70-80%, the pressure during the reaction process can be kept stable, and abnormal pressure caused by overfilling can be avoided.
[0022] In this application, the carbonization temperature range is selected as 180~220℃, which is lower than the degradation temperature of plant heat-sensitive components (>250℃), thus ensuring that the active ingredients are not destroyed.
[0023] Optionally, in step (4), the power of the ultrasonic breaking is 450~550W, and the ultrasonic breaking time is 55~65min;
[0024] The centrifugation speed is 11000~13000 rpm, and the centrifugation time is 15~25 min;
[0025] The dialysis membrane used in the dialysis has a molecular weight cutoff of 1000 Da, the dialysis temperature is 23~27℃, and the dialysis time is 45~50h;
[0026] The plant-based carbon dots are carbon dots with a molecular weight of <1000 Da in the dialysis solution.
[0027] Optionally, in step (5), the particle size of the nanoparticles is 8~12nm;
[0028] The mass concentration of nanoparticles in the plant-based dispersion is 2-5%.
[0029] Optionally, in step (6), the amount of plant-based carbon dots added is 0.01 to 0.05% of the total mass of plant-based carbon dots and plant-based dispersion.
[0030] In this application, carbon dots are added using a micro-feeding device (accuracy ±0.001g). 0.01~0.05% is the optimal range for carbon dot addition. Experiments have shown that below 0.01% the effect is not significant, while above 0.05% it leads to carbon dot agglomeration, affecting product stability.
[0031] Optionally, in step (6), the stirring speed is 250~350 rpm and the stirring time is 8~12 min;
[0032] The ultrasonic dispersion power is 400~500W, and the ultrasonic dispersion time is 25~35min;
[0033] The homogenization pressure is 100~120MPa, the homogenization is performed 2~4 times, and the homogenization time is 40~80min each time.
[0034] The drying process involves drying to a moisture content of ≤1%;
[0035] The drying process is vacuum drying;
[0036] The vacuum degree of the vacuum drying is ≤50Pa, and the temperature of the vacuum drying is 40~50℃.
[0037] In this application, the combination of 400~500W ultrasound and 100~120MPa high-pressure homogenization is the key to achieving high dispersibility, which can ensure that carbon dots and plant powders are uniformly mixed with a dispersibility of >95%.
[0038] Secondly, this application provides a plant-based carbon spot desiccant, prepared by any of the preparation methods described above.
[0039] Thirdly, this application provides the application of the above-mentioned plant-based carbon spot oral disinfectant powder in the preparation of a drug for treating oral mucosal diseases.
[0040] Compared with the prior art, this application has the following advantages:
[0041] The carbon dot raw materials used in this application are directly derived from the formulation production line, reducing costs while avoiding the introduction of impurities from purchased nanomaterials. Furthermore, the use of plant-derived carbon dots avoids the biosafety risks associated with metal nanomaterials, ensuring high safety. The hydrothermal carbonization temperature (180~220℃) and the degradation temperature of the plant's heat-sensitive components (typically >250℃) form a safety window, ensuring that the plant's active ingredients are not destroyed. The carbon dot preparation process in this application is seamlessly integrated with the original process, requiring no additional equipment or process steps, and exhibits good process compatibility. Moreover, the preparation process of this application is applicable to various plant-derived powders such as Ganoderma lucidum spore powder, Astragalus membranaceus, Salvia miltiorrhiza, Polygonatum sibiricum, black goji berries, honeysuckle, licorice, Angelica sinensis, and ginseng, and can be extended to even more plants, making it widely applicable. In addition, experiments have demonstrated that the plant-based carbon dot oral disinfectant powder prepared in this application dissolves rapidly in the oral cavity, has high mucosal absorption efficiency, and retains a high rate of active ingredients. Attached Figure Description
[0042] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.
[0043] Figure 1 This is a flowchart illustrating the overall preparation process of this application;
[0044] Figure 2 This is a schematic diagram of the preparation equipment configuration for this application;
[0045] Figure 3 This is a characterization diagram of the Ganoderma lucidum spore powder by electrochemical in-situ Raman spectra in this application;
[0046] Figure 4 TEM characterization image of plant carbon dots prepared by hydrothermal carbonization method of Ganoderma lucidum spore powder in this application;
[0047] Figure 5 A comparison of the morphology of Ganoderma lucidum spore powder before and after preparation in this application;
[0048] Figure 6 Comparison of microscopic images (600x) before and after preparation of Ganoderma lucidum spore powder in this application;
[0049] Figure 7 The TIC chromatogram of the cell wall-removed Ganoderma lucidum spore powder of this application (comparison before and after preparation);
[0050] Figure 8 This is a line graph comparing the thirty Ganoderma lucidum triterpenes described in this application. Detailed Implementation
[0051] The present application is further illustrated below with reference to specific embodiments. The following descriptions are merely a few embodiments of the present application and are not intended to limit the present application in any way. Although the present application discloses preferred embodiments as follows, they are not intended to limit the present application. Any modifications or variations made by those skilled in the art without departing from the scope of the technical solution of the present application using the disclosed technical content are equivalent to equivalent implementation cases and all fall within the scope of the technical solution.
[0052] Unless otherwise specified, the raw materials used in the embodiments of this application are all purchased commercially and used directly without any special treatment.
[0053] Unless otherwise specified, the analytical methods in the embodiments all adopt conventional instrument or equipment settings and conventional analytical methods.
[0054] Figure 1 This is a flowchart of the overall preparation process of this application.
[0055] Figure 2 This is a schematic diagram of the preparation equipment configuration for this application, showing the combination and matching of the equipment's raw material pulping system, gas supply system, functional group grafting system, homogenization system, concentration and drying system, and finished product packaging system. Figure 1 The technological process.
[0056] Example 1
[0057] (Taking Ganoderma lucidum spore powder oral instant powder as an example)
[0058] Step 1: Carbon dot preparation
[0059] (1) Take 10μm of Ganoderma lucidum spore powder (5% of the total powder; in this example, take 100g of Ganoderma lucidum spore powder and separate 5g).
[0060] (2) Prepare (1) into a 10% aqueous suspension (powder mass concentration).
[0061] (3) React (2) with hydrothermal reaction at 200℃ for 8 hours (reaction vessel filling degree 80%).
[0062] (4) Then, the mixture was subjected to ultrasonic disruption (500W, 60min) and centrifugation (12000rpm, 20min) in sequence. The supernatant was then purified by dialysis (1000Da dialysis membrane, 25±2℃, 48h) to obtain Ganoderma lucidum spore powder carbon dots (particle size 5.0±0.5nm, carboxyl content 8.5mmol / g, suspended in aqueous solution).
[0063] Step 2: Integration Process
[0064] (1) Take 0.05% of Ganoderma lucidum spore powder carbon dots (the 0.05% refers to the carbon dots of Ganoderma lucidum spore powder accounting for 0.05% of the total mass of carbon dots of Ganoderma lucidum spore powder and Ganoderma lucidum spore powder dispersion);
[0065] (2) Add (1) to a 10nm Ganoderma lucidum spore powder dispersion prepared by nano-pulverization of the remaining 95% of the 10μm Ganoderma lucidum spore powder (powder mass concentration 5%, 5g Ganoderma lucidum spore powder is prepared into 100mL dispersion);
[0066] (3) Stir at low speed (300 rpm, 10 min);
[0067] (4) Perform ultrasound at 500W for 30 minutes;
[0068] (5) Perform 3 cycles of high-pressure homogenization at 120MPa;
[0069] (6) Then, perform vacuum drying at 50℃ for 2 hours (vacuum degree ≤ 50Pa);
[0070] (7) Then packaged in aluminum-plastic composite film (containing 3g / 100g silica gel desiccant).
[0071] Effect verification:
[0072] Original process (i.e., traditional process):
[0073] (1) Ganoderma lucidum spore powder 10μm powder is dispersed in water (powder mass concentration 2%).
[0074] (2) Stir at 300 rpm for 10 min;
[0075] (3) Vacuum dry at 40℃ for 12 hours;
[0076] (4) Aluminum-plastic packaging.
[0077] Dissolution time test: Take 1g of sample and add 10mL of physiological saline, incubate in a 37℃ constant temperature water bath, and record the complete dissolution time. Result: 30 seconds (original process 70 seconds).
[0078] Oral absorption rate test of Ganoderma lucidum triterpenes: Using an isolated porcine oral mucosa model, the cumulative absorption of Ganoderma lucidum triterpenes in the mucosa was determined by HPLC. Result: 88.5% (40.5% in the original process).
[0079] Active ingredient retention test: The product was stored at 25℃ and 60% humidity for 12 months, and the content of Ganoderma lucidum triterpenes was determined by HPLC. Result: Attenuation after 12 months <5% (30% attenuation in the original process).
[0080] Dispersion uniformity test: The particle size distribution after dispersion was measured using a laser particle size analyzer. Result: Dispersion > 98% (original process 80%-85%).
[0081] Example 1 was compared with the original process, and the results are shown in Tables 1 and 2.
[0082] Table 1 Comparison of Triterpenoid Content in Thirty Kinds of Ganoderma Lucidum
[0083]
[0084]
[0085] Note: ND indicates not detected.
[0086] As shown in Table 1, the content of active ingredients in the Ganoderma lucidum spore powder of Example 1 of this application is significantly higher than that of the traditional process, indicating that the process of this application is superior and the retention rate of active ingredients is higher.
[0087] Table 2 Summary of Test Results
[0088]
[0089] As shown in Table 2, the total sugar and polysaccharide content of the Ganoderma lucidum spore powder of Example 1 of this application is 1.46 times that of the Ganoderma lucidum spore powder produced by the traditional process. Meanwhile, the insoluble matter content of the Ganoderma lucidum spore powder produced by this application is 4.5%, while that of the Ganoderma lucidum spore powder produced by the traditional process is 38.0%. Therefore, the insoluble matter content of the Ganoderma lucidum spore powder produced by this application is 33.5% less than that of the Ganoderma lucidum spore powder produced by the traditional process.
[0090] In addition, three polypeptides were detected in the Ganoderma lucidum spore powder of this application, and their information is shown in Table 3.
[0091] Table 3. Peptide Information
[0092]
[0093] Other results such as Figures 3-8 As shown.
[0094] Figure 3This is the electrochemical in-situ Raman spectrometry characterization diagram of Ganoderma lucidum spore powder in this application, by... Figure 3 Raman spectroscopy revealed that at 1574 cm⁻¹ -1 The peak at 2686 cm⁻¹ is the G band of graphene carbon dots. -1 The peak at that point represents the 2D band of graphene carbon dots.
[0095] Figure 4 This application describes the preparation of plant carbon point TEM characterization images using the hydrothermal carbonization method for Ganoderma lucidum spore powder. This is for TEM observation of the material's microstructure, lattice fringes, lattice defects, and the morphology and size of nanoparticles. Figure 3 The following conclusions can be drawn from the Raman spectra:
[0096] (1) Raman characterization peaks and TEM electron microscopy combined observation showed that the lattice stripes were clear and regular and the graphene was in sheet form, with 3 to 5 layers.
[0097] (2) The ID / IG ratio = 0.32 indicates that the crystal quality is excellent and the degree of graphitization is high.
[0098] (3) The size of the wafer is controllable when the diameter is greater than 10nm.
[0099] Figure 5 These are comparative images of the morphology of Ganoderma lucidum spore powder before and after preparation in this application. Figure 5 As can be seen, the water-soluble Ganoderma lucidum spore powder of Example 1 of this application is the result of nano-processing of Ganoderma lucidum spore powder with cell wall removed, and its color changes from dark red to semi-transparent yellow compared to Ganoderma lucidum spore powder with cell wall removed.
[0100] Figure 6 For the comparison of microscopic images (600x) of the Ganoderma lucidum spore powder before and after preparation in this application, the two sample solutions were observed under an optical microscope at 600x magnification. Figure 6 It is evident that the decelled Ganoderma lucidum spore powder contains a small amount of damaged or relatively intact spore walls; however, the water-soluble Ganoderma lucidum spore powder of this application has completely nanoscaled the spore powder and residual spore walls.
[0101] Figure 7 The TIC chromatogram of the cell-wall-removed Ganoderma lucidum spore powder in this application (comparison before and after preparation) was obtained by Q-TOF MS liquid chromatography-mass spectrometry analysis and comparison with mass spectrometry databases. Regarding the compound composition of water-soluble and cell-wall-removed Ganoderma lucidum spore powders, the water-soluble spore powder showed the detection of three additional polypeptide compounds with high response within the retention time of 0-2 min (see Table 3); the composition of other compounds was basically the same. The BPI chromatogram of the liquid chromatography is shown below. Figure 4 The additional peptides may be products of enzymatic or hydrolytic breakdown of proteins in the cell-wall-removed Ganoderma lucidum spore powder during the preparation process.
[0102] Figure 8The line graph comparing the thirty Ganoderma lucidum triterpenes in this application, combined with the data analysis in Tables 1, 2, and 3, shows that the total amount of the 30 Ganoderma lucidum triterpenes in water-soluble Ganoderma lucidum spore powder is 1.27 times that of Ganoderma lucidum spore powder with cell wall removed, and the total sugar and polysaccharide content is 1.46 times that of Ganoderma lucidum spore powder. Among them, the first 27 Ganoderma lucidum triterpenes (from ganoderic acid I to ganoderic acid triol) and the moderately polar triterpenes of ganoderic acid J are all found in higher amounts in water-soluble Ganoderma lucidum spore powder, while the contents of the latter three (ganoderic acid E, ganoderic acid DM, and ganoderic acid TR) are almost negligible.
[0103] In summary:
[0104] Microscopic observation revealed that the outer shell of the water-soluble Ganoderma lucidum spore powder had been removed or "dissolved".
[0105] The results of the insoluble matter test showed that the solubility of water-soluble Ganoderma lucidum spore powder was significantly improved;
[0106] The total sugar and polysaccharide content of water-soluble Ganoderma lucidum spore powder is approximately 1.46 times that of cell-wall-removed Ganoderma lucidum spore powder;
[0107] The total amount of 30 Ganoderma triterpenes in water-soluble Ganoderma lucidum spore powder is 1.27 times that in cell-wall-removed Ganoderma lucidum spore powder.
[0108] Example 2
[0109] (Taking Astragalus oral instant powder as an example)
[0110] Step 1: Carbon dot preparation
[0111] (1) Take 10μm powder of Astragalus membranaceus (5% of the total powder; in this example, take 100g of Astragalus membranaceus powder and decompose 5g);
[0112] (2) Prepare (1) into a 10% aqueous suspension (powder mass concentration);
[0113] (3) React (2) with hydrothermal heat at 200℃ for 8 hours (reaction vessel filling degree 80%).
[0114] (4) Then, ultrasonic disruption (500W, 60min) and centrifugation (12000rpm, 20min) were performed in sequence. The supernatant was then purified by dialysis (1000Da dialysis membrane, 25±2℃, 48h) to obtain Astragalus carbon dots (particle size 5.0±0.5nm, carboxyl content 8.5mmol / g, suspended in aqueous solution).
[0115] Step 2: Integration Process
[0116] (1) Add 0.05% of Astragalus carbon dots (the 0.05% refers to the 0.05% of Astragalus carbon dots in the total mass of Astragalus carbon dots and Astragalus dispersion) to a 10nm Astragalus dispersion (5% powder mass concentration, 5g Astragalus powder is prepared into 100mL dispersion) obtained by nano-pulverization of the remaining 95% of 10μm Astragalus powder;
[0117] (2) Stir at low speed (300 rpm, 10 min);
[0118] (3) Perform ultrasound at 500W for 30 minutes;
[0119] (4) Perform 3 cycles of high-pressure homogenization at 120MPa;
[0120] (5) Then, perform vacuum drying at 50℃ for 2 hours (vacuum degree ≤ 50Pa);
[0121] (6) Then packaged in aluminum-plastic composite film (containing 3g / 100g silica gel desiccant).
[0122] Effect verification:
[0123] Original process:
[0124] (1) Astragalus membranaceus 10μm powder was dispersed in water (powder mass concentration 2%).
[0125] (2) Stir at 300 rpm for 10 min;
[0126] (3) Vacuum dry at 40℃ for 12 hours;
[0127] (4) Aluminum-plastic packaging.
[0128] Dissolution time test: Take 1g of sample and add 10mL of physiological saline, incubate in a 37℃ constant temperature water bath, and record the complete dissolution time. Result: 36 seconds (original process 60 seconds).
[0129] Astragalone oral absorption rate test: Using an isolated porcine oral mucosa model, the cumulative absorption of astragalone in the mucosa was determined by HPLC. Result: 78.3% (47.1% in the original process).
[0130] Active ingredient retention test: The product was stored at 25℃ and 60% humidity for 12 months, and the astragalone content was determined by HPLC. Result: Attenuation after 12 months <10% (30% attenuation in the original process).
[0131] Dispersion uniformity test: The particle size distribution after dispersion was measured using a laser particle size analyzer. Result: Dispersion > 95% (original process 80%-85%).
[0132] Example 3
[0133] (Taking Danshen oral instant powder as an example)
[0134] Step 1: Carbon dot preparation
[0135] (1) Take 10μm powder of Salvia miltiorrhiza (5% of the total powder; in this example, take 100g of Salvia miltiorrhiza powder and separate 5g);
[0136] (2) Prepare 1) into a 10% aqueous suspension (powder mass concentration);
[0137] (3) React 2) with hydrothermal heat at 220℃ for 10 hours (reaction vessel filling degree 80%).
[0138] (4) Then, ultrasonic disruption (500W, 60min) and centrifugation (12000rpm, 20min) were performed in sequence. The supernatant was then purified by dialysis (1000Da dialysis membrane, 25±2℃, 48h) to obtain tanshinone carbon dots (particle size 5.2±0.8nm, carboxyl content 6.2mmol / g, suspended in aqueous solution).
[0139] Step 2: Integration Process
[0140] (1) Add 0.05% of tanshinone carbon dots (the 0.05% refers to the 0.05% of the total mass of tanshinone carbon dots and tanshinone dispersion) to a 10nm tanshinone dispersion (5% of the powder mass concentration, 5g of tanshinone powder is prepared into 100mL dispersion) obtained by nano-pulverizing the remaining 95% of 10μm tanshinone powder;
[0141] (2) Stir at low speed (300 rpm, 10 min);
[0142] (3) Perform ultrasound at 500W for 30 minutes;
[0143] (4) Perform 3 cycles of high-pressure homogenization at 120MPa;
[0144] (5) Then, perform vacuum drying at 50℃ for 2 hours (vacuum degree ≤ 50Pa);
[0145] (6) Then packaged in aluminum-plastic composite film (containing 3g / 100g silica gel desiccant).
[0146] Effect verification:
[0147] Original process:
[0148] (1) 10μm powder of Salvia miltiorrhiza was dispersed in water (powder mass concentration 2%).
[0149] (2) Stir at 300 rpm for 10 min;
[0150] (3) Vacuum dry at 40℃ for 12 hours;
[0151] (4) Aluminum-plastic packaging.
[0152] Dissolution time test: 42 seconds (original process 56 seconds).
[0153] Tanshinone oral absorption rate test: 68.3% (47.1% in the original process).
[0154] Active ingredient retention test: 12-month attenuation <10% (original process attenuation 30%).
[0155] Dispersion uniformity test: Dispersion > 95% (original process 80%-85%).
[0156] Example 4
[0157] (Taking Polygonatum and Black Goji Berry Compound Carbon Dot Oral Instant Powder as an example)
[0158] (1) Take equal amounts of 10μm powder of Polygonatum sibiricum (10% of the total powder) and 10μm powder of black goji berries (10% of the total powder);
[0159] (2) Mix (1) to prepare a 10% aqueous suspension (powder mass concentration);
[0160] (3) React (2) with hydrothermal heat at 200℃ for 8 hours (reaction vessel filling degree 80%).
[0161] (4) Then, ultrasonic disruption (500W, 60min) and centrifugation (12000rpm, 20min) were performed in sequence. The supernatant was then purified by dialysis (1000Da dialysis membrane, 25±2℃, 48h) to obtain Polygonatum sibiricum-black wolfberry composite carbon dots (particle size 5.5±0.7nm, carboxyl content 7.8mmol / g, suspended in aqueous solution).
[0162] Step 2: Integration Process
[0163] (1) Add 0.01% of the polygonatum-black goji berry composite carbon dots (the 0.01% refers to the 0.05% of the total mass of the polygonatum-black goji berry composite carbon dots and the composite dispersion) to a 10nm composite dispersion (powder mass concentration 2%, 2g of composite powder is prepared into 100mL dispersion) obtained by nano-pulverizing the remaining 90% of the 10μm polygonatum-black goji berry powder;
[0164] (2) Stir at low speed (300 rpm, 10 min);
[0165] (3) Perform ultrasound at 500W for 30 minutes;
[0166] (4) Perform 3 cycles of high-pressure homogenization at 120MPa;
[0167] (5) Then, perform vacuum drying at 50℃ for 2 hours (vacuum degree ≤ 50Pa);
[0168] (6) Then packaged in aluminum-plastic composite film (containing 3g / 100g silica gel desiccant).
[0169] Effect verification:
[0170] Original process:
[0171] (1) Take equal amounts of 10μm powder of Polygonatum sibiricum and 10μm powder of black wolfberry and disperse them in water (the total mass of the two powders in water is 2%).
[0172] (2) Stir at 300 rpm for 10 min;
[0173] (3) Vacuum dry at 40℃ for 12 hours;
[0174] (4) Aluminum-plastic packaging.
[0175] Dissolution time test: 32 seconds (original process 55 seconds).
[0176] Active ingredient absorption rate test: 82.5% (original process 45.2%).
[0177] Active ingredient retention test: 12-month attenuation <8% (original process attenuation 28%).
[0178] Comparative Example 1
[0179] Compared with Example 1, the only difference is that the carbonization temperature was replaced with 150°C. The test results are shown in Table 4.
[0180] Table 4 Test Results
[0181]
[0182] Comparative Example 2
[0183] Compared with Example 1, the only difference is that the carbonization temperature was replaced with 250°C. The test results are shown in Table 5.
[0184] Table 5 Test Results
[0185]
[0186] Comparative Example 3
[0187] Compared with Example 1, the only difference is that the high-pressure homogenization step was removed. The test results are shown in Table 6.
[0188] Table 6 Test Results
[0189]
[0190] As can be seen from the results in Tables 4-6, the data results obtained by the process in this application embodiment are optimal.
[0191] The above description is merely a few embodiments of this application and is not intended to limit this application in any way. Although this application discloses preferred embodiments as described above, it is not intended to limit this application. Any changes or modifications made by those skilled in the art without departing from the scope of the technical solution of this application using the disclosed technical content are equivalent to equivalent implementation cases and fall within the scope of the technical solution.
Claims
1. A method for preparing a plant-based carbon spot disinfectant, characterized in that, Includes the following steps: (1) The plant powder was split into two parts, which were used for carbon dot preparation and subsequent processing, respectively; (2) The plant powder used for carbon dot preparation is mixed with water to obtain a suspension; (3) The suspension is placed in a polytetrafluoroethylene reactor for carbonization reaction; (4) The carbonization reaction products were ultrasonically crushed and centrifuged in sequence, and the supernatant was dialyzed to obtain plant carbon dots; (5) The plant powder used for subsequent processing in step (1) is nano-pulverized, and the nano-pulverized material is mixed with water to obtain a plant-based dispersion. (6) The plant-based carbon dots are mixed with the plant-based dispersion, and then stirred, ultrasonically dispersed, homogenized and dried in sequence to obtain the plant-based carbon dots powder removal agent.
2. The method for preparing a plant-based carbon spot disinfectant powder according to claim 1, characterized in that, In step (1), the plant powder is derived from at least one of the following: Ganoderma lucidum spores, Astragalus membranaceus, Salvia miltiorrhiza, Polygonatum sibiricum, black wolfberry, honeysuckle, licorice, Angelica sinensis, and ginseng. The particle size of the plant powder is 8~12μm; The amount of plant powder used for carbon dot preparation is 5-10% of the total mass of plant powder.
3. The method for preparing a plant-based carbon spot disinfectant powder according to claim 1, characterized in that, In step (2), the mass concentration of the plant powder used for carbon dot preparation in the suspension is 5-10%.
4. The method for preparing a plant-based carbon spot disinfectant powder according to claim 1, characterized in that, In step (3), the filling degree of the suspension in the polytetrafluoroethylene reactor is 70-80%; The carbonization reaction temperature is 180~220℃; The carbonization reaction takes 6 to 12 hours.
5. The method for preparing a plant-based carbon spot disinfectant powder according to claim 1, characterized in that, In step (4), the power of the ultrasonic crushing is 450~550W, and the ultrasonic crushing time is 55~65min; The centrifugation speed is 11000~13000 rpm, and the centrifugation time is 15~25 min; The dialysis membrane used in the dialysis has a molecular weight cutoff of 1000 Da, the dialysis temperature is 23~27℃, and the dialysis time is 45~50h; The plant-based carbon dots are carbon dots with a molecular weight of <1000 Da in the dialysis solution.
6. The method for preparing a plant-based carbon spot disinfectant powder according to claim 1, characterized in that, In step (5), the particle size of the nanoparticles is 8~12nm; The mass concentration of nanoparticles in the plant-based dispersion is 2-5%.
7. The method for preparing a plant-based carbon spot disinfectant powder according to claim 1, characterized in that, In step (6), the amount of plant-based carbon dots added is 0.01 to 0.05% of the total mass of plant-based carbon dots and plant-based dispersion.
8. The method for preparing a plant-based carbon spot disinfectant powder according to claim 1, characterized in that, In step (6), the stirring speed is 250~350 rpm, and the stirring time is 8~12 min; The ultrasonic dispersion power is 400~500W, and the ultrasonic dispersion time is 25~35min; The homogenization pressure is 100~120MPa, the homogenization is performed 2~4 times, and the homogenization time is 40~80min each time. The drying process involves drying to a moisture content of ≤1%; The drying process is vacuum drying; The vacuum degree of the vacuum drying is ≤50Pa, and the temperature of the vacuum drying is 40~50℃.
9. A plant-based carbon spot desiccant, characterized in that, It is prepared by the preparation method according to any one of claims 1 to 9.
10. The use of the plant-based carbon spot oral disinfectant powder according to claim 9 in the preparation of a medicament for treating oral mucosal diseases.