Thin-layer method for identifying rice-grain sprout traditional Chinese medicine formula granules and fried rice-grain sprout traditional Chinese medicine formula granules and preparation method of rice-grain sprout traditional Chinese medicine formula granules and fried rice-grain sprout traditional Chinese medicine formula granules

Abstract

The invention provides a thin-layer method for identifying rice-grain sprout traditional Chinese medicine formula granules and fried rice-grain sprout traditional Chinese medicine formula granules and a preparation method of the rice-grain sprout traditional Chinese medicine formula granules and the fried rice-grain sprout traditional Chinese medicine formula granules. The volume ratio of cyclohexane to ethyl acetate to methanol is 4: 3: 1, a thin-layer plate is taken out after being developed in the developing solvent, the thin-layer plate is aired, a sulfuric acid ethanol solution with the concentration of 10 wt% is sprayed, the thin-layer plate is heated at the temperature of 105 DEG C, the thin-layer plate is placed under an ultraviolet lamp to be inspected, and the rice sprout traditional Chinese medicine formula granules show blue fluorescent spots at the Rf value of 0.17-0.21 and the Rf value of 0.59-0.68. The fried rice sprout traditional Chinese medicine formula granules have no fluorescent spots. The method provided by the invention can be used for successfully distinguishing the rice-grain sprout traditional Chinese medicine formula granules and the fried rice-grain sprout traditional Chinese medicine formula granules.

Description

Technical Field

[0001] This invention belongs to the field of traditional Chinese medicine identification technology, specifically providing a thin-layer chromatography method for identifying rice sprout traditional Chinese medicine formula granules and stir-fried rice sprout traditional Chinese medicine formula granules, as well as a method for preparing rice sprout traditional Chinese medicine formula granules and stir-fried rice sprout traditional Chinese medicine formula granules. Background Technology

[0002] Rice sprouts are the fruit of the grass family, specifically the rice plant. Oryza sativa L. Mature rice fruits, after sprouting and drying, are processed into a product that aids digestion, strengthens the spleen, and stimulates appetite. Fried rice sprouts are made by placing cleaned rice sprouts in a frying container and frying them at 150℃-200℃ for 14-16 minutes until they turn a deep yellow color. They are then removed, cooled, and the resulting product resembles rice sprouts, has a deep yellow surface, often has broken fibrous roots, and retains or loses some white downy hairs, and has a fragrant aroma. Fried rice sprouts are primarily used to aid digestion and are indicated for those with poor appetite or lack of hunger. This demonstrates that the chemical composition of rice sprouts and fried rice sprouts changes during the processing.

[0003] The main chemical components of rice sprouts include amino acids, vitamins, nucleosides, flavonoids, and sugars. Current research on rice sprouts primarily focuses on their medicinal components and efficacy. Shi Jilian et al. experimentally determined the reducing sugar content in raw rice sprouts, roasted rice sprouts, and charred rice sprouts to be 3.73%, 1.29%, and 0.30%, respectively. Chen Tiqiang et al. used an automated amino acid analyzer to determine the γ-aminobutyric acid (GABA) content in roasted and charred rice sprouts to be 0.304 mg / g and 0.209 mg / g, respectively. Li Rui used high-performance liquid chromatography (HPLC) to determine the content of 4-coumaric acid in roasted rice sprout granules; the linear range for GABA content was 0.003948-0.09870 mg / ml (r). 2 =1.0000), with an average recovery rate of 98.8%. However, no effective method for identifying rice sprouts and roasted rice sprout extracts has been reported in the prior art.

[0004] Since roasted rice sprout extract and granules are made from rice sprout medicinal materials through a series of processes, some of which destroy the original physical characteristics, the methods for identifying physical properties are not applicable to the identification of extracts and preparations. Currently, there is no effective method to distinguish between rice sprouts, roasted rice sprout extract, and granules. Therefore, establishing a method to differentiate between rice sprouts, roasted rice sprout extract, and granules is crucial for quality control. Summary of the Invention

[0005] This invention aims to at least partially solve one of the technical problems in the prior art. Therefore, one objective of this invention is to provide a thin-layer chromatography method for identifying rice sprout medicinal formula granules and roasted rice sprout medicinal formula granules, as well as a method for preparing rice sprout medicinal formula granules and roasted rice sprout medicinal formula granules, so as to achieve effective identification of rice sprout medicinal formula granules and roasted rice sprout medicinal formula granules.

[0006] In a first aspect, the present invention provides a thin-layer chromatography method for identifying rice sprout traditional Chinese medicine formula granules and roasted rice sprout traditional Chinese medicine formula granules, comprising: using a developing solvent of cyclohexane, ethyl acetate, and methanol in a volume ratio of 4:3:1; developing the thin-layer plate in the developing solvent, removing and drying it, spraying it with a 10wt% sulfuric acid ethanol solution, heating it at 105°C, and examining it under a UV lamp; and then, observing the rice sprout traditional Chinese medicine formula granules under UV light. f The values ​​at 0.17-0.21 and 0.59-0.68 show blue fluorescent spots, while the fried rice sprout herbal formula granules do not have fluorescent spots.

[0007] According to the thin-layer chromatography method for identifying rice sprout medicinal formula granules and roasted rice sprout medicinal formula granules provided by the present invention, a mixture of cyclohexane, ethyl acetate, and methanol is used as the developing solvent, and the volume ratio of the three is controlled at 4:3:1. This method can effectively separate the chemical components of rice sprout medicinal formula granules and roasted rice sprout medicinal formula granules. After developing and drying, the mixture is sprayed with a 10wt% sulfuric acid ethanol solution, heated at 105°C, and examined under ultraviolet light. Clearly separated spots can be seen on the thin-layer plate, thus identifying rice sprout medicinal formula granules and roasted rice sprout medicinal formula granules by the difference in the spots. Specifically, the rice sprout medicinal formula granules on the thin-layer plate are... f The values ​​at 0.17-0.21 and 0.59-0.68 show blue fluorescent spots, while the stir-fried rice sprout herbal formula granules show no fluorescent spots. This was confirmed by thin-layer chromatography (TLC) at R... f Whether blue fluorescent spots appear at values ​​of 0.17-0.21 and 0.59-0.68 successfully distinguishes between rice sprout traditional Chinese medicine formula granules and stir-fried rice sprout traditional Chinese medicine formula granules.

[0008] It should be noted that the thin-layer method provided by the present invention is also applicable to the detection of rice sprouts and roasted rice sprout extracts, as well as the standard decoction of rice sprout traditional Chinese medicine formula granules and roasted rice sprout traditional Chinese medicine formula granules. The standard decoction is a liquid mixture used for formula granules dried into granules.

[0009] In some embodiments of the present invention, the wavelength of the ultraviolet lamp is 365 nm.

[0010] In some embodiments of the present invention, the thin film includes a silicone G thin film.

[0011] The preferred silicone G thin-layer plate is selected from Merck thin-layer plates in Germany.

[0012] In some embodiments of the present invention, the sample amount on the thin-layer plate is 10 μl-20 μl.

[0013] In some embodiments of the present invention, the ambient temperature at which the thin-film plate is expanded in the expanding agent is 4-35°C.

[0014] In some embodiments of the present invention, the ambient humidity during the unfolding of the thin plate in the unfolding agent is 32-75%.

[0015] In some embodiments of the present invention, the preparation processes of the rice sprout traditional Chinese medicine formula granules and the spotting solution of the stir-fried rice sprout traditional Chinese medicine formula granules each independently include: The Chinese herbal formula granules were dissolved in water and then extracted with ethyl acetate. The extract was evaporated to dryness and then dissolved in methanol to obtain the spotting solution.

[0016] In some embodiments of the present invention, the mass ratio of the traditional Chinese medicine formula granules to the volume ratio of the water is 2g:(10-30)ml.

[0017] In some embodiments of the present invention, the ethyl acetate is extracted 2-3 times.

[0018] In some embodiments of the present invention, the mass ratio of the pharmaceutical formulation granules to the volume ratio of the methanol is 2g:(0.5-1.5)ml.

[0019] In some embodiments of the present invention, the preparation process of the rice sprout control medicinal material solution includes: taking rice sprout control medicinal material, adding water and boiling it, cooling and filtering it, adding ethyl acetate to the filtrate and shaking to extract it, evaporating it to dryness, and dissolving the residue in methanol.

[0020] In a second aspect, the present invention provides a method for preparing rice sprout traditional Chinese medicine formula granules in the above-mentioned thin-layer chromatography method for identifying rice sprout traditional Chinese medicine formula granules and stir-fried rice sprout traditional Chinese medicine formula granules, comprising: Take rice sprout slices, add water and decoct, filter the resulting aqueous extract and concentrate under reduced pressure to obtain a concentrated solution; The concentrated solution was spray-dried to obtain spray-dried rice sprout powder. The rice sprout spray-dried powder and maltodextrin are mixed evenly and then dry granulated.

[0021] In some embodiments of the present invention, the decoction process includes a first decoction and a second decoction. The amount of water added in the first decoction is 4-6 times that of the rice sprout slices, and the first decoction time is 25-35 minutes. The amount of water added in the second decoction is 3-5 times that of the rice sprout slices, and the second decoction time is 10-20 minutes. The decoction temperature is 98-102°C.

[0022] In some embodiments of the present invention, the mesh size of the filter screen is 200 mesh.

[0023] In some embodiments of the present invention, the temperature of the vacuum concentration is 55-80°C, and the vacuum concentration is carried out to a density of 1.08-1.11.

[0024] In some embodiments of the present invention, the inlet air temperature of the spray dryer is 185-195°C and the outlet air temperature is 75-85°C.

[0025] In some embodiments of the present invention, the amount of maltodextrin added is 5-10%.

[0026] In a third aspect, the present invention provides a method for preparing the roasted rice sprout traditional Chinese medicine formula granules used in the above-mentioned thin-layer chromatography method for identifying rice sprout traditional Chinese medicine formula granules and roasted rice sprout traditional Chinese medicine formula granules, comprising: Take stir-fried rice sprout slices, add water and decoct. Filter the resulting aqueous extract and concentrate under reduced pressure to obtain a concentrated solution. The concentrated liquid was spray-dried to obtain roasted rice sprout spray-dried powder. The roasted rice sprout spray-dried powder and maltodextrin are mixed evenly and then dry granulated.

[0027] In some embodiments of the present invention, the decoction process includes a first decoction and a second decoction. The amount of water added in the first decoction is 4-6 times that of the stir-fried rice sprout slices, and the first decoction time is 25-35 minutes. The amount of water added in the second decoction is 3-5 times that of the stir-fried rice sprout slices, and the second decoction time is 10-20 minutes. The decoction temperature is 98-102°C.

[0028] In some embodiments of the present invention, the mesh size of the filter screen is 200 mesh.

[0029] In some embodiments of the present invention, the temperature of the vacuum concentration is 55-80°C, and the vacuum concentration is carried out to a density of 1.08-1.11.

[0030] In some embodiments of the present invention, the inlet air temperature of the spray dryer is 185-195°C and the outlet air temperature is 75-85°C.

[0031] In some embodiments of the present invention, the amount of maltodextrin added is 5-10%.

[0032] Compared with the prior art, the present invention can achieve at least one of the following beneficial effects: This invention uses a mixture of cyclohexane, ethyl acetate, and methanol as the developing solvent, which enables effective separation of the chemical components of rice sprout traditional Chinese medicine granules and roasted rice sprout traditional Chinese medicine granules, thereby facilitating the separation of chemical components through a thin-layer plate on R... fThe presence of blue fluorescent spots at values ​​of 0.17-0.21 and 0.59-0.68 successfully distinguished between rice sprout and roasted rice sprout traditional Chinese medicine granules. The thin-layer chromatography method provided by this invention can rapidly and effectively identify rice sprouts, roasted rice sprout extracts, and rice sprout and roasted rice sprout traditional Chinese medicine granules. This method is highly specific, stable, precise, convenient, and easy to master, enabling more standardized quality control of rice sprout and roasted rice sprout-related preparations and ensuring the efficacy of the drugs. Attached Figure Description

[0033] Figure 1 This is a thin-layer chromatogram of Example 1 of the present invention; Figure 2 This is a thin-layer chromatogram of Example 2 of the present invention; Figure 3 The following are thin-layer chromatograms of different thin-layer plates in Example 3 of the present invention; Figure 4 This is a thin-layer chromatogram of the Merck thin-layer plate of Example 3 of the present invention; Figure 5 This is a thin-layer chromatogram of Example 4 of the present invention; Figure 6 This is a thin-layer chromatogram of Example 5 of the present invention; Figure 7 This is a thin-layer chromatogram of Example 6 of the present invention; Figure 8 This is a thin-layer chromatogram of Comparative Example 1 of the present invention; Figure 9 This is a thin-layer chromatogram of Comparative Example 2 of the present invention. Detailed Implementation

[0034] Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without inventive effort are within the scope of protection of this invention. The invention will now be described with reference to specific embodiments. It should be noted that these embodiments are merely descriptive and do not limit the invention in any way.

[0035] The materials used in the embodiments and comparative examples of this invention are as follows: (1) Instruments Heating plate, mortar and pestle, thin-layer imaging system: CAMAG TLC Visualizer, semi-automatic thin-layer spotting instrument: CAMAGLionmat-5, silica gel G thin-layer plates (Zhejiang Taizhou Luqiao Sijia Biochemical Plastics Factory, batch number: 2024-12-21, Tianjin Slida Technology Co., Ltd., batch number: 20250602, Merck, batch numbers: HX46121653, HX44363653).

[0036] (2) Reagents Cyclohexane, ethyl acetate, and methanol were all of analytical grade, and water was ultrapure water (prepared in the laboratory).

[0037] (3) Drug testing Rice sprout control material (Chengdu Desite Biotechnology Co., Ltd., batch number: DSTYD003601), rice sprout traditional Chinese medicine formula granules (Sichuan Xinlvse Pharmaceutical Technology Development Co., Ltd., batch numbers: DY-KL-01; DY-KL-02; DY-KL-03), and stir-fried rice sprout traditional Chinese medicine formula granules (Sichuan Xinlvse Pharmaceutical Technology Development Co., Ltd., batch numbers: CDY-KL-01; CDY-KL-02; CDY-KL-03).

[0038] (5) Preparation method of rice sprout traditional Chinese medicine formula granules Processing: Take rice sprouts and remove impurities.

[0039] Extraction and Concentration: Take 7500g of rice sprout slices. For the first decoction, add 5 times the amount of water, heat to 98℃ and start timing, maintain the decoction for 30 minutes, controlling the temperature range between 98-102℃. For the second decoction, add 4 times the amount of water, heat to 98℃ and start timing, maintain the decoction for 15 minutes, controlling the temperature range between 98-102℃, to obtain an aqueous extract of rice sprouts. Filter the aqueous extract through a 200-mesh filter, and concentrate under reduced pressure at 55-80℃ until the thermal relative density reaches 1.08-1.11 to obtain a concentrated rice sprout solution.

[0040] Drying: Take the concentrated liquid and spray dry it at an inlet temperature of 190±5℃ and an outlet temperature of 80±5℃ to obtain rice sprout spray-dried powder.

[0041] Preparation of rice sprout traditional Chinese medicine formula granules: Take the spray-dried powder, add 5% maltodextrin, mix well, and perform dry powdering to obtain rice sprout traditional Chinese medicine formula granules.

[0042] (6) Preparation method of stir-fried rice sprout Chinese medicine formula granules Preparation: Take clean rice sprouts and stir-fry them at a temperature of 150℃-200℃ until they turn dark yellow.

[0043] Extraction and Concentration: Take 6700g of rice sprout slices. For the first decoction, add 5 times the amount of water and heat to 98℃, then start timing and maintain the decoction for 30 minutes, controlling the temperature range between 98-102℃. For the second decoction, add 4 times the amount of water and heat to 98℃, then start timing and maintain the decoction for 15 minutes, controlling the temperature range between 98-102℃, to obtain an aqueous extract of roasted rice sprouts. Filter the aqueous extract through a 200-mesh filter and concentrate under reduced pressure at 55-80℃ until the thermal relative density reaches 1.08-1.12 to obtain a concentrated roasted rice sprout solution.

[0044] Drying: Take the concentrated liquid and spray dry it at an inlet temperature of 190±5℃ and an outlet temperature of 80±5℃ to obtain roasted rice sprout spray dry powder.

[0045] Fried rice sprout traditional Chinese medicine formula granules: Take the spray-dried powder, add 5% maltodextrin, mix well, and perform dry powdering to obtain fried rice sprout traditional Chinese medicine formula granules.

[0046] Example 1 (1) Preparation of the test solution Take 2g of rice sprout traditional Chinese medicine formula granules and stir-fried rice sprout traditional Chinese medicine formula granules respectively, grind them into fine powder, add 20ml of water, heat to dissolve, add ethyl acetate and shake to extract twice, 30ml each time, combine the ethyl acetate solutions, evaporate to dryness, add 1.0ml of methanol to dissolve the residue to obtain rice sprout traditional Chinese medicine formula granule spotting solution and stir-fried rice sprout traditional Chinese medicine formula granule spotting solution.

[0047] (2) Preparation of reference standards and reference drug solutions Take another 2g of rice sprouts as a reference herb, add 50ml of water, decoct for 30 minutes, cool, filter, add ethyl acetate to the filtrate and shake to extract twice, 30ml each time, combine the ethyl acetate extracts, evaporate to dryness, add 1.0ml of methanol to dissolve the residue, and prepare the reference herb solution.

[0048] Negative sample: Take 0.75g of maltodextrin, add 20ml of water, then add ethyl acetate and shake to extract twice, 30ml each time. Combine the ethyl acetate extracts, evaporate to dryness, and dissolve the residue in 1.0ml of methanol.

[0049] (3) Thin-layer chromatography method According to the thin-layer chromatography method (Appendix VIB of Part I of the 2010 edition of the Chinese Pharmacopoeia), 15 μl each of the above-mentioned rice sprout traditional Chinese medicine formula granule spotting solution, stir-fried rice sprout traditional Chinese medicine formula granule spotting solution, control medicinal material solution and negative sample were spotted onto the same silica gel G thin-layer plate. Cyclohexane-ethyl acetate-methanol (volume ratio of 4:3:1) was used as the developing solvent. After development, the plate was removed, dried, sprayed with 10% sulfuric acid ethanol, heated at 105℃, and examined under a UV lamp (365nm).

[0050] Thin-layer chromatography results are shown in Figure 1 , Figure 1 In the table, 1 is a negative control solution, 2 is a rice sprout control solution, 3 is a rice sprout traditional Chinese medicine granule solution, and 4 is a stir-fried rice sprout traditional Chinese medicine granule solution. Figure 1 It can be seen that the rice sprout traditional Chinese medicine formula granules showed blue fluorescent spots at the ratio shift values ​​of 0.201 and 0.647, while the stir-fried rice sprout traditional Chinese medicine formula granules did not show spots. Furthermore, the negative sample did not interfere with the rice sprout and stir-fried rice sprout traditional Chinese medicine formula granule test samples, indicating that the method has good specificity.

[0051] Example 2 (Sampling Quantity Investigation) The only difference between Example 2 and Example 1 is that 10 μl, 15 μl, and 20 μl of rice sprout traditional Chinese medicine formula granule solution and fried rice sprout traditional Chinese medicine formula granule solution were respectively spotted on the same silica gel G thin-layer plate.

[0052] The thin-layer chromatography of Example 2 is shown in [reference needed]. Figure 2 , Figure 2 In the sample, 1-3 were 10 μl, 15 μl, and 20 μl of the herbal formula granule solution of roasted rice sprouts; 4-6 were 10 μl, 15 μl, and 20 μl of the herbal formula granule solution of rice sprouts. The sample volume of the herbal formula granule solution of rice sprouts and the herbal formula granule solution of roasted rice sprouts were 10-20 μl. At the PI0 values ​​of 0.178 and 0.615, the herbal formula granule of rice sprouts showed blue fluorescent spots, while the herbal formula granule of roasted rice sprouts showed no spots. This was used to distinguish the herbal formula granule of rice sprouts from the herbal formula granule of roasted rice sprouts.

[0053] Example 3 (Different Thin-Layer Plates) Cuttable thin-layer chromatography plates from Tianjin Slida Technology Co., Ltd., Merck, and prefabricated silica gel G plates from Luqiao Sijia Biochemical Plastics Factory in Taizhou City, Zhejiang Province were selected and tested according to the test method in Example 1.

[0054] Thin-layer chromatography (TLC) Figure 3 , Figure 3 In the table, 1 represents the rice sprout control solution, 2 represents the rice sprout traditional Chinese medicine granule solution, and 3 represents the stir-fried rice sprout traditional Chinese medicine granule solution. The results showed that while the Tianjin Slida and Zhejiang Taizhou thin-layer plates could distinguish between rice sprouts and stir-fried rice sprout traditional Chinese medicine granules, they could not show identification points at both locations. Therefore, different batches of Merck thin-layer plates were used for thin-layer identification experiments, and the results are shown below. Figure 4 ,Depend on Figure 3 and Figure 4 It can be seen that the rice sprout herbal medicine granules at shift values ​​of 0.207, 0.175, 0.674, and 0.650 show blue fluorescent spots, while the stir-fried rice sprout herbal medicine granules show no spots. Therefore, this method confirms that the thin-layer plate is a Merck thin-layer plate.

[0055] Example 4 (Different Temperatures) After sampling, the thin-layer plate was developed in temperature environments of low temperature 4°C and high temperature 35°C, respectively, according to the thin-layer method of Example 1.

[0056] Thin-layer chromatography (TLC) Figure 5 , Figure 5 In the table, 1 is the rice sprout control medicinal material solution, 2 is the rice sprout traditional Chinese medicine formula granule solution, and 3 is the stir-fried rice sprout traditional Chinese medicine formula granule solution. Figure 5 It can be seen that the method has good adaptability to different temperatures, and the rice sprout Chinese medicine formula granules show blue fluorescent spots at specific values ​​of 0.206, 0.204; 0.616, 0.659, while the fried rice sprout Chinese medicine formula granules do not have spots.

[0057] Example 5 (Different Humidities) After sampling, the thin-layer plates were developed in humidity environments of 32% RH and 75% RH, respectively, according to the thin-layer method of Example 1.

[0058] Thin-layer chromatography (TLC) Figure 6 , Figure 6 In the table, 1 is a control solution of rice sprouts, 2 is a granule solution of rice sprouts used in traditional Chinese medicine, and 3 is a granule solution of stir-fried rice sprouts used in traditional Chinese medicine. Figure 6 It can be seen that the method has good adaptability to different temperatures, and the rice sprout Chinese medicine formula granules show blue fluorescent spots at specific values ​​of 0.175, 0.177; 0.613, 0.604, while the fried rice sprout Chinese medicine formula granules do not have spots.

[0059] Example 6 The rice sprout control solution, different batches of rice sprout traditional Chinese medicine granule solutions, and different batches of roasted rice sprout traditional Chinese medicine granule solutions were spotted separately on the same silica gel G thin-layer plate and analyzed according to the established method. The experimental results are shown in [Figure 1]. Figure 7 , Figure 7 In the table, 1 represents the control solution of rice sprouts, 2-4 represent solutions of rice sprout traditional Chinese medicine granules, and 5-7 represent solutions of stir-fried rice sprout traditional Chinese medicine granules. The results showed that the rice sprout traditional Chinese medicine granules had a higher specific gravity (R0). f The 0.182 and 0.596 ions have blue fluorescent spots, while the stir-fried rice sprout Chinese medicine formula granules do not have these spots. These fluorescent spots can be used to distinguish between the two.

[0060] The ratio shift values ​​of various parameters in the thin-layer chromatography method investigations of Examples 1-6 are summarized, and the results are shown in Table 1. Based on the summarized results, the ratio shift value (R0) for the identification spots of rice sprout traditional Chinese medicine granules was determined. f It should be within 10%, with specified values ​​of 0.190 and 0.63.

[0061] Table 1

[0062] Comparative Example 1 The test solution was prepared according to the method in Example 1. 10 μL of the test solution was spotted onto the same silica gel G thin-layer plate and developed using cyclohexane:ethyl acetate (4:3) as the developing solvent. The plate was removed, dried, sprayed with 10% sulfuric acid ethanol solution, and heated at 105°C until the spots were clearly visible. The test sample chromatogram showed spots of the same color at the corresponding positions as the rice sprout control chromatogram. Results are shown below. Figure 8 , Figure 8 In the middle, 1-4 are rice sprout traditional Chinese medicine formula granule solutions; 5-8 are stir-fried rice sprout traditional Chinese medicine formula granule solutions. Figure 8It can be seen that, using the above-mentioned developing agent, rice sprouts and roasted rice sprouts medicinal formula granules have no obvious spots, and the two cannot be distinguished.

[0063] Comparative Example 2 Take 2g of rice sprout herbal formula granules and stir-fried rice sprout herbal formula granules, grind them into a fine powder, add 25ml of ethanol, sonicate for 30min, cool, filter, and concentrate the filtrate to 1ml as the test solution. Separately, take 2g of rice sprout control material, add 50ml of water, decoct for 30min, filter, evaporate the filtrate to dryness, add 25ml of ethanol, and prepare the control material solution using the same method. Take 10μL of the test solution and spot it on the same silica gel G thin-layer plate. Develop using cyclohexane:ethyl acetate:methanol (4:3:1) as the developing solvent. Remove, air dry, spray with 10% sulfuric acid ethanol solution, and heat at 105°C until the spots are clearly visible. Results are shown below. Figure 9 , Figure 9 In the table, 1 represents rice sprout as a control material, 2 represents rice sprout as a traditional Chinese medicine formula granule solution, and 3 represents stir-fried rice sprout as a traditional Chinese medicine formula granule solution. Figure 9 It can be seen that, using the thin-layer chromatography method of Comparative Example 2, there are no obvious distinguishing spots between rice sprouts and roasted rice sprout herbal formula granules, and the two cannot be distinguished.

[0064] Any numerical value mentioned in this invention, if there is only a two-unit interval between any minimum and any maximum value, includes all values ​​that increase by one unit each time from the minimum to the maximum value. For example, if the amount of a component, or the value of a process variable such as temperature, pressure, or time, is stated as 50-90, in this specification it means specifically listing values ​​such as 51-89, 52-88… and 69-71 and 70-71, etc. For non-integer values, it may be appropriately considered that a unit is 0.1, 0.01, 0.001, or 0.0001. These are merely some specifically specified examples. In this application, in a similar manner, all possible combinations of numerical values ​​between the listed minimum and maximum values ​​are considered to have been disclosed.

[0065] It should be noted that the embodiments described above are only for explaining the present invention and do not constitute any limitation on the present invention. The present invention has been described with reference to typical embodiments, but it should be understood that the words used therein are descriptive and explanatory terms, not limiting terms. Modifications can be made to the present invention within the scope of the claims, and revisions can be made to the present invention without departing from the scope and spirit of the present invention. Although the present invention described herein relates to specific methods, materials, and embodiments, it does not mean that the present invention is limited to the specific examples disclosed herein; on the contrary, the present invention can be extended to all other methods and applications with the same function.

Claims

1. A thin-layer chromatography method for distinguishing between rice sprout traditional Chinese medicine formula granules and stir-fried rice sprout traditional Chinese medicine formula granules, characterized in that, include: The thin-layer chromatography method uses a mixture of cyclohexane, ethyl acetate, and methanol as the developing solvent, with a volume ratio of 4:3:

1. After development in the solvent, the thin-layer plate is removed, dried, sprayed with a 10wt% sulfuric acid ethanol solution, heated at 105°C, and examined under ultraviolet light. The rice sprout traditional Chinese medicine granules are then analyzed using UV light. f The values ​​at 0.17-0.21 and 0.59-0.68 show blue fluorescent spots, while the fried rice sprout herbal formula granules do not have fluorescent spots.

2. The method according to claim 1, characterized in that, The wavelength of the ultraviolet lamp is 365nm; And / or, the thin film includes a silicone G thin film, preferably a Merck silicone G thin film.

3. The method according to claim 1, characterized in that, The sample amount on the thin-layer plate is 10 μl-20 μl.

4. The method according to any one of claims 1-3, characterized in that, The thin-layer plate is expanded in the developing agent at an ambient temperature of 4-35℃. And / or, the ambient humidity during which the thin-layer plate is developed in the developing agent is 32-75%.

5. The method according to any one of claims 1-3, characterized in that, The preparation processes of the rice sprout traditional Chinese medicine formula granules and the spotting solutions of the stir-fried rice sprout traditional Chinese medicine formula granules each independently include: The Chinese herbal formula granules were dissolved in water and then extracted with ethyl acetate. The extract was evaporated to dryness and then dissolved in methanol to obtain the spotting solution.

6. The method according to claim 5, characterized in that, The mass ratio of the herbal formula granules to the volume ratio of the water is 2g:(10-30)ml; And / or, the ethyl acetate is extracted 2-3 times; And / or, the mass ratio of the pharmaceutical formulation granules to the volume ratio of the methanol is 2g:(0.5-1.5)ml.

7. A method for preparing rice sprout traditional Chinese medicine formula granules in a thin-layer chromatography method for identifying rice sprout traditional Chinese medicine formula granules and roasted rice sprout traditional Chinese medicine formula granules according to any one of claims 1-6, characterized in that, include: Take rice sprout slices, add water and decoct, filter the resulting aqueous extract and concentrate under reduced pressure to obtain a concentrated solution; The concentrated solution was spray-dried to obtain spray-dried rice sprout powder. The rice sprout spray-dried powder and maltodextrin are mixed evenly and then dry granulated.

8. The method according to claim 7, characterized in that, The decoction process includes a first decoction and a second decoction. The amount of water added in the first decoction is 4-6 times that of the rice sprout slices, and the first decoction time is 25-35 minutes. The amount of water added in the second decoction is 3-5 times that of the rice sprout slices, and the second decoction time is 10-20 minutes. The decoction temperature is 98-102℃. And / or, the mesh size of the filter screen is 200 mesh; And / or, the vacuum concentration temperature is 55-80°C, and the vacuum concentration is carried out to a density of 1.08-1.11; And / or, the inlet air temperature of the spray dryer is 185-195℃, and the outlet air temperature is 75-85℃; And / or, the amount of maltodextrin added is 5-10%.

9. A method for preparing the roasted rice sprout traditional Chinese medicine formula granules in a thin-layer chromatography method for identifying rice sprout traditional Chinese medicine formula granules and roasted rice sprout traditional Chinese medicine formula granules according to any one of claims 1-6, characterized in that, include: Take stir-fried rice sprout slices, add water and decoct. Filter the resulting aqueous extract and concentrate under reduced pressure to obtain a concentrated solution. The concentrated liquid was spray-dried to obtain roasted rice sprout spray-dried powder. The roasted rice sprout spray-dried powder and maltodextrin are mixed evenly and then dry granulated.

10. The method according to claim 9, characterized in that, The decoction process includes a first decoction and a second decoction. The amount of water added in the first decoction is 4-6 times that of the stir-fried rice sprout slices, and the first decoction time is 25-35 minutes. The amount of water added in the second decoction is 3-5 times that of the stir-fried rice sprout slices, and the second decoction time is 10-20 minutes. The decoction temperature is 98-102℃. And / or, the mesh size of the filter screen is 200 mesh; And / or, the vacuum concentration temperature is 55-80°C, and the vacuum concentration is carried out to a density of 1.08-1.11; And / or, the inlet air temperature of the spray dryer is 185-195℃, and the outlet air temperature is 75-85℃; And / or, the amount of maltodextrin added is 5-10%.

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