A thin-layer chromatography method for identifying asparagus drugs including formulated granules and its application

By using protodiosgenin as a reference and a specific developing agent, the problems of blurred spots and poor separation effect in the thin-layer identification method of asparagus medicinal materials were solved, and clear identification and efficient separation of saponin components in asparagus medicinal materials were achieved.

CN120214194BActive Publication Date: 2026-03-10BEIJING KANGRENTANG PHARMA
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-04-08
Publication Date
2026-03-10

AI Technical Summary

Technical Problem

Existing thin-layer chromatography methods for identifying Asparagus root have problems such as blurred color spots, poor separation effect, and limited chromatographic information, especially for Asparagus root water extract and formulation granules, which are difficult to identify effectively.

Method used

Using protodiosgenin as a reference standard, thin-layer chromatography was performed using a specific ratio of n-butanol, ethyl acetate, glacial acetic acid, and water as the developing solvent. The specific steps included sample extraction, preparation of the reference standard solution and the reference medicinal material solution, and identification was performed by thin-layer chromatography.

Benefits of technology

It enables the qualitative identification of saponin components in asparagus drugs, with clear color spots, good separation effect, abundant chromatographic information, and simple and efficient operation.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention provides a thin-layer chromatography (TLC) identification method for asparagus drugs, including formulated granules, and its application. The TLC identification method includes the following steps: (1) extracting the sample to be tested to obtain a test solution; (2) mixing a reference standard with an alcohol solvent to obtain a reference solution; (3) extracting a reference medicinal material to obtain a reference medicinal material solution; (4) performing TLC on the test solution, the reference solution, and the reference medicinal material solution, and identifying the sample to be tested based on the chromatographic results; the reference standard includes protodiosgenin. The identification method provided by this invention overcomes the problems of blurred color spots, poor separation effect, and limited chromatographic information in the existing TLC identification technology. It has the advantages of abundant chromatographic information, good separation effect, and clear color spots, and can simultaneously perform qualitative identification of saponin components. The operation is simple and efficient.
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Description

Technical Field

[0001] This invention belongs to the field of pharmaceutical analysis technology, specifically relating to a thin-layer chromatography method for identifying asparagus drugs, including formulation granules, and its application. Background Technology

[0002] Asparagus root is the dried tuberous root of *Asparagus cochinchinensis* Merr., a plant in the Liliaceae family. It is harvested in autumn and winter, washed, and the stem base and fibrous roots are removed. It is then boiled or steamed until thoroughly cooked, the outer skin is removed while hot, washed again, and dried. It has the effects of nourishing yin and moistening dryness, clearing the lungs and promoting fluid production. It is used for dry cough due to lung dryness, persistent cough with sticky phlegm, soreness of the lower back and knees, bone steaming fever, internal heat and thirst, heat-related fluid depletion, dry throat and mouth, and constipation due to intestinal dryness. Modern pharmacological studies have shown that asparagus root has antioxidant, anti-inflammatory, anti-tumor, anti-aging, blood pressure lowering, blood sugar lowering, and antitussive and expectorant effects. The chemical components of asparagus root include various steroidal saponins, amino acids, flavonoids, polypeptides, lignans, sugars, oligosaccharides, vitamins, and minerals. The main components include asparagine, sarsaponin, aspartic acid, glycine, fructose, β-sitosterol, glucose, palmitic acid, carotene, and diosgenin. Its pharmacological effects mainly include anti-inflammatory, antioxidant, antitumor, anti-aging, hypoglycemic, hypotensive, antitussive, and expectorant effects. Asparagus can enhance the phagocytic capacity of mononuclear macrophages and perform non-specific immune regulation. Asparagus water extract can inhibit the secretion of tumor necrosis factor, thereby inhibiting the proliferation of malignant tumor cells such as lung cancer and breast cancer. Simultaneously, it has a significant inhibitory effect on lipid peroxidation and can significantly reduce the number of coughs induced by concentrated ammonia in mice. Total saponins of asparagus can treat leukemia by downregulating the expression of B-cell lymphoma-2 gene mRNA and inducing apoptosis in HL-60 cell lines.

[0003] Since Asparagus water extract and granules are made from Asparagus medicinal materials through a series of processes, some of which can damage the original medicinal characteristics, a more convenient and faster identification method is needed to distinguish and identify these damaged medicinal materials, so as to better control quality. Thin-layer chromatography (TLC) is a good identification method due to its ease of operation and speed. Currently, the TLC identification method for Asparagus medicinal materials in the Pharmacopoeia involves eluting with a C18 column using methanol as the solvent, developing with chloroform-methanol-water (13:7:2) as the developing solvent, using a silica gel G TLC plate, spraying with 10% sulfuric acid ethanol solution, heating at 105℃ for color development, and examining under ultraviolet light at 365 nm.

[0004] However, the thin-layer chromatography identification methods for Asparagus root described in the aforementioned pharmacopoeias suffer from blurred color spots and limited chromatographic information, especially for Asparagus root water extracts and granules. Therefore, providing an effective method for identifying Asparagus root water extracts and granules has become an urgent problem to be solved. Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention aims to provide a thin-layer chromatography (TLC) identification method for asparagus drugs, including formulated granules, and its application. The identification method provided by this invention overcomes the problems of blurred color spots, poor separation, and limited chromatographic information in existing TLC identification methods. It offers advantages such as abundant chromatographic information, good separation, and clear color spots, and can simultaneously perform qualitative identification of saponin components. The method is simple and efficient to operate.

[0006] To achieve this objective, the present invention adopts the following technical solution:

[0007] On one hand, the present invention provides a thin-layer chromatography identification method for asparagus drugs including formulation granules, the thin-layer chromatography identification method comprising the following steps:

[0008] (1) Extract the sample to be tested to obtain the test solution;

[0009] (2) The reference standard is mixed with an alcohol solvent to obtain a reference standard solution;

[0010] (3) Extract the reference medicinal material to obtain a reference medicinal material solution;

[0011] (4) Perform thin-layer chromatography on the test solution, reference solution and reference medicinal material solution, and identify the sample to be tested based on the chromatography results;

[0012] Steps (1), (2), and (3) are not in any particular order;

[0013] The reference standard includes diosgenin.

[0014] The above method uses diosgenin as a reference standard to qualitatively identify saponin components in asparagus products. At the same time, the overall identification method overcomes the problems of blurred color spots, poor separation effect and limited chromatographic information in the existing thin-layer chromatography identification technology. It has the advantages of more chromatographic information, better separation effect and clear color spots.

[0015] Preferably, the asparagus medicine includes any one of asparagus raw material, asparagus formula granules, asparagus water extract, or asparagus standard decoction.

[0016] Preferably, the sample to be tested is asparagus water extract or asparagus formula granules, and the extraction step in step (1) specifically includes:

[0017] The sample to be tested was mixed with acetone and refluxed to extract the solution.

[0018] Preferably, the ratio of the sample to acetone is 1:(15-20)g / mL, such as 1:15g / mL, 1:16g / mL, 1:17g / mL, 1:18g / mL, 1:19g / mL or 1:20g / mL, but not limited to the values ​​listed above. Other values ​​not listed above are also applicable.

[0019] Preferably, the sample to be tested is asparagus root, and the extraction step in step (1) specifically includes:

[0020] The sample to be tested was extracted by mixing it with water, and then extracted by reflux with acetone to obtain the test solution.

[0021] Preferably, the ratio of the sample to water is 1:(25-35)g / mL, such as 1:25g / mL, 1:26g / mL, 1:27g / mL, 1:28g / mL, 1:29g / mL, 1:30g / mL, 1:31g / mL, 1:32g / mL, 1:33g / mL, 1:34g / mL, or 1:35g / mL, but not limited to the values ​​listed above. Other unlisted values ​​within the above range are also applicable.

[0022] Preferably, the ratio of the sample to acetone is 1:(15-20)g / mL, such as 1:15g / mL, 1:16g / mL, 1:17g / mL, 1:18g / mL, 1:19g / mL or 1:20g / mL, but not limited to the values ​​listed above. Other values ​​not listed above are also applicable.

[0023] Preferably, the alcohol solvent in step (2) includes methanol.

[0024] Preferably, the developing solvent for the thin-layer chromatography in step (4) is a mixed solution of n-butanol, ethyl acetate, glacial acetic acid and water.

[0025] Preferably, the volume ratio of n-butanol, ethyl acetate, glacial acetic acid, and water is (18-20):(2-4):(4-6):(6-8), wherein the number of parts of n-butanol can be 18, 18.5, 19, 19.5, or 20, the number of parts of ethyl acetate can be 2, 2.5, 3, 3.5, or 4, the number of parts of glacial acetic acid can be 4, 4.5, 5, 5.5, or 6, and the number of parts of water can be 6, 6.5, 7, 7.5, or 8, but is not limited to the values ​​listed above. Other unlisted values ​​within the above range are also applicable.

[0026] The aforementioned specific developing solvent and its ratio can effectively overcome the problems of blurred color spots, poor separation effect, and insufficient chromatographic information in the existing thin-layer chromatography identification technology, increase chromatographic information, improve separation effect, and make the identification method have the advantage of clear color spots.

[0027] On the other hand, the present invention also provides the application of the thin-layer chromatography identification method for asparagus drugs as described above in the quality control of asparagus drugs.

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] This invention provides a thin-layer chromatography method for identifying asparagus drugs including formulation granules. By using protodiosgenin as a reference standard, the saponin components in asparagus drugs can be qualitatively identified. At the same time, the overall identification method overcomes the problems of blurred color spots, poor separation effect and limited chromatographic information in the existing thin-layer chromatography identification technology. It has the advantages of more chromatographic information, better separation effect and clear color spots. Attached Figure Description

[0030] Figure 1 This is a graph showing the identification results of the first five batches of freeze-dried Asparagus standard decoction powder in Example 1;

[0031] Figure 2 This is a graph showing the identification results of the last five batches of freeze-dried Asparagus standard decoction powder in Example 1.

[0032] Figure 3 This is a graph showing the identification results of three batches of asparagus formula granules in Example 1.

[0033] Figure 4 This is a graph showing the results of the sample quantity assessment in Example 1;

[0034] Figure 5 This is a diagram showing the results of the investigation of the silicone G thin film (Merck KGaA) in Example 1;

[0035] Figure 6 This is a diagram showing the results of the investigation of the silicone G thin film (Huanghai Jiangyou Silicone Development and Testing Plant) in Example 1;

[0036] Figure 7 This is a diagram showing the results of the investigation of the silica gel G thin film plate (Yantai Chemical Industry Research Institute) in Example 1;

[0037] Figure 8 This is a graph showing the results of the investigation at different temperatures and humidity levels (T: 22.3℃, RH: 50%) in Example 1;

[0038] Figure 9 This is a graph showing the results of the investigation at different temperatures and humidity levels (T: 21.8℃, RH: 28.9%) in Example 1;

[0039] Figure 10 This is a graph showing the results of the investigation at different temperatures and humidity levels (T: 22.0℃, RH: 76%) in Example 1;

[0040] Figure 11 This is a graph showing the results of the investigation at different temperatures and humidity levels (T: 8.4℃, RH: 59%) in Example 1;

[0041] Figure 12 This is a diagram showing the identification results of Example 2;

[0042] Figure 13 This is a diagram showing the identification results of Example 3;

[0043] Figure 14 This is a diagram showing the identification results of Example 4;

[0044] Figure 15 This is an image showing the identification results of Example 5;

[0045] Figure 16 This is a diagram showing the identification results of Example 6;

[0046] Figure 17 This is a diagram showing the identification results of Example 7;

[0047] Figure 18 This is a diagram showing the identification results of Example 8;

[0048] Figure 19 This is a graph showing the identification results of Comparative Examples 1-2 in developing solvent 1;

[0049] Figure 20 This is a graph showing the identification results of Comparative Examples 1-2 in developing solvent 2. Detailed Implementation

[0050] The technical solution of the present invention will be further illustrated below through specific embodiments. Those skilled in the art should understand that the embodiments described are merely illustrative of the present invention and should not be construed as limiting the invention in any way.

[0051] The instruments and reagents used in the following examples are as follows:

[0052] Instruments: CAMAG thin-layer imaging system, ME104E electronic balance (Mettler Toledo), JY20002 electronic balance (Mettler Toledo), BSA124S electronic balance (Sartorius Instruments (Beijing) Co., Ltd.), BT25S electronic balance (Sartorius Instruments (Beijing) Co., Ltd.), DZKW-4 constant temperature water bath (Beijing Zhongxing Weiye Instrument Co., Ltd.), KQ-500DB ultrasonic cleaner (Kunshan Ultrasonic Instrument Co., Ltd.), silicone G plate (Merck KGaA, Yantai Chemical Industry Research Institute, Yantai Zhifu Huangwu Silicone Development and Experiment Plant).

[0053] Test drug: Asparagus reference material (batch number: 121139-201906, China National Institutes for Food and Drug Control)

[0054] Protodiosgenin (batch number: 111937-202102, China National Institutes for Food and Drug Control, purity 94.8%)

[0055] Asparagus standard decoction freeze-dried powder: 10 batches of Asparagus slices (batch numbers 190116-445400-01, 190116-537600-02, 190116-674200-03, 190116-537600-04, 190116-445400-05, 190117-541500-06, 190117-535400-07, 190117-448000-08, 190117-646500-) 09 and 190117-441000-10) were placed in a clay pot and soaked for 30 minutes. For the first decoction, add 10 times the amount of water as the amount of medicinal slices, bring to a boil over high heat, then simmer over low heat for 60 minutes. Filter while hot and cool quickly for later use. For the second decoction, add 6 times the amount of water as the amount of medicinal slices, bring to a boil over high heat, then simmer over low heat for 40 minutes. Filter while hot and cool quickly for later use. Combine the filtrates and concentrate (65℃) until the material-to-liquid ratio is about 1:1 (relative density between 1.05 and 1.10). Freeze-dry to obtain the standard decoction freeze-dried powder of the corresponding batch number.

[0056] Reagents: Acetone, n-butanol, ethyl acetate, methanol, glacial acetic acid, and 10% sulfuric acid ethanol were all of analytical grade, and water was distilled water.

[0057] Example 1

[0058] This embodiment provides a thin-layer chromatography method for the identification of asparagus drugs, and the specific steps are as follows:

[0059] Preparation method of test solution: Take 1g of freeze-dried powder of Asparagus standard decoction, add 2mL of water to moisten the sample, add 18mL of acetone and reflux for 1 hour, cool, filter, concentrate the filtrate to dryness, and dissolve the residue in 5mL of methanol to obtain the test solution.

[0060] Preparation method of reference herbal solution: Take 1g of reference herbal material, add 30mL of water, boil for 60 minutes, cool, filter, concentrate the filtrate to dryness, add 2mL of water and 18mL of acetone, reflux for 1 hour, cool, filter, concentrate the filtrate to dryness, dissolve the residue in 5mL of methanol to obtain the reference herbal solution.

[0061] Preparation method of reference solution: Take 1 mg of diosgenin reference standard and add 1 mL of methanol to prepare reference solution.

[0062] Thin-layer plate product name: Silicone G plate, manufacturer: Yantai Chemical Industry Research Institute, specifications: 10×20cm, batch number: 20181211;

[0063] Sampling method: contact sampling, with a sampling volume of 6 μL for the test solution and the reference medicinal material solution, and a sampling volume of 4 μL for the reference solution;

[0064] Developing solvent: n-Butanol-ethyl acetate-glacial acetic acid-water (volume ratio 19:3:5:7);

[0065] Temperature: 20℃;

[0066] Relative humidity: 59%;

[0067] Development tank specifications: Double-slot;

[0068] Unfolding method and spacing: Unfolding upwards, spacing 15cm;

[0069] Colorimetric reagent: 10% sulfuric acid in ethanol;

[0070] Color development method: Examined under ultraviolet light at 365nm.

[0071] The above 10 batches of freeze-dried powder of standard Asparagus decoction and 3 batches of Asparagus formula granules were identified, and the results are as follows: Figure 1-3 As shown ( Figure 1-2In the following table, 1: Protodiospin reference solution 111937-202102; 2: Asparagus reference medicinal material solution 121490-201906; 3: Asparagus standard decoction freeze-dried powder 190116-445400-01; 4: Asparagus standard decoction freeze-dried powder 190116-537600-02; 5: Asparagus standard decoction freeze-dried powder 190116-674200-03; 6: Asparagus standard decoction freeze-dried powder 190116-537600-04; 7: Asparagus standard decoction freeze-dried powder 190116-445400-05; 8: Protodiospin reference solution 111937-202102; 9: Protodiospin reference solution 111937-202102; 10: Dioscorea saponin reference solution 111937-202102; 11: Asparagus reference medicinal material solution 121490-201906; 12: Asparagus standard decoction freeze-dried powder 190117-541500-06; 13: Asparagus standard decoction freeze-dried powder 190117-535400-07; 14: Asparagus standard decoction freeze-dried powder 190117-448000-08; 15: Asparagus standard decoction freeze-dried powder 190117-646500-09; 16: Asparagus reference medicinal material solution 190117-441000-10; 17: Protodioscorea saponin reference solution 111937-202102; Figure 3 Among them, 1: diosgenin reference solution (111937-202102); 2: asparagus reference medicinal material solution (121490-201906); 3: asparagus granules (190116-445400-01); 4: asparagus granules (190116-537600-02); 5: asparagus granules (190116-674200-03).

[0072] As can be seen from the figure, the spots in the obtained spectrum are clear, well separated, and correspond well with the spots of the reference standard and the reference medicinal material. The chemical information is rich and all of them are the original components of the material itself.

[0073] Then, 3 μL, 6 μL, and 9 μL of the test solution and the control herbal solution were taken for spotting analysis, and the results are as follows. Figure 4 As shown (where 1-3, diosgenin reference solution (2 / 4 / 6 μL); 4-6, asparagus reference material (3 / 6 / 9 μL); 7-9, asparagus formula granules 01 (3 / 6 / 9 μL); 10-12, asparagus formula granules 02 (3 / 6 / 9 μL); 13-15, asparagus formula granules 03 (3 / 6 / 9 μL); 16, blank).

[0074] Depend on Figure 4 As shown, through the investigation of the sample amount, when the sample of Asparagus was 6 μL and the reference medicinal material was 4 μL, the thin-layer chromatographic spots were clear, the spot size was moderate, the separation was good, the Rf was moderate, and the other conditions were acceptable.

[0075] Next, silica gel G thin-layer plates produced by Yinlong-Yantai Chemical Industry Research Institute, Yantai Zhifu Huangwu Silica Gel Development and Testing Plant, and Merck KGaA were developed under the above conditions, and the results are as follows. Figure 5-7 As shown (where 1: diosgenin reference solution (111937-202102); 2: asparagus reference medicinal material solution (121490-201906); 3: asparagus test solution (190116-445400-01); 4: asparagus test solution (190116-537600-02); 5: asparagus test solution (190116-674200-03)).

[0076] As shown in the figure, silica gel G thin-layer plates produced by different manufacturers (Yantai Chemical Industry Research Institute, Huanghai Jiangyou Silica Gel Development and Testing Plant, Merck KGaA) can all achieve good separation results for aspartic acid samples. This thin-layer identification method has good durability for thin-layer plates produced by different manufacturers.

[0077] Following the above method, 10 μL each of the asparagus test solution, reference solution, and asparagus reference herb solution were spotted onto the same silica gel G thin-layer plate (Yantai Chemical Industry Research Institute). The development under different temperatures and relative humidity conditions was investigated. The plates were then removed, air-dried, sprayed with 10% sulfuric acid ethanol solution, dried with hot air, and examined under UV light at 365 nm. The thin-layer chromatogram results are shown below. Figure 8-11 The following are examples: 1. Dioscorea saponin reference solution (111937-202102); 2. Asparagus reference medicinal material solution (121490-201906); 3. Asparagus test solution (190116-445400-01); 4. Asparagus test solution (190116-537600-02); 5. Asparagus test solution (190116-674200-03).

[0078] As shown in the figure, the separation effect of the asparagus sample is good under different temperature and humidity conditions, and this thin-layer identification method has good durability under temperature and humidity.

[0079] Example 2

[0080] This embodiment provides a thin-layer chromatography method for the identification of asparagus. The specific steps are identical to those in Example 1, except that the volume ratio of n-butanol-ethyl acetate-glacial acetic acid-water is 18:2:4:6. The results are as follows: Figure 12 As shown.

[0081] Example 3

[0082] This embodiment provides a thin-layer chromatography method for the identification of asparagus. The specific steps are identical to those in Example 1, except that the volume ratio of n-butanol-ethyl acetate-glacial acetic acid-water is 20:4:6:8. The results are as follows: Figure 13 As shown.

[0083] Example 4

[0084] This embodiment provides a thin-layer chromatography method for the identification of asparagus. The specific steps are the same as in Example 1, except that the developing solvent does not include n-butanol, and the portion is reduced and proportionally allocated to ethyl acetate, glacial acetic acid, and water. The results are as follows: Figure 14 As shown.

[0085] Example 5

[0086] This embodiment provides a thin-layer chromatography method for the identification of asparagus. The specific steps are the same as in Example 1, except that the developing solvent does not include ethyl acetate, and the fraction is reduced and proportionally allocated to n-butanol, glacial acetic acid, and water. The results are as follows: Figure 15 As shown.

[0087] Example 6

[0088] This embodiment provides a thin-layer chromatography method for the identification of asparagus. The specific steps are the same as in Example 1, except that the developing solvent does not include glacial acetic acid, and the portion is reduced and proportionally allocated to ethyl acetate, n-butanol, and water. The results are as follows: Figure 16 As shown.

[0089] Example 7

[0090] This embodiment provides a thin-layer chromatography method for the identification of asparagus. The specific steps are the same as in Example 1, except that the developing solvent does not include water and the proportions of water to ethyl acetate, glacial acetic acid, and n-butanol are reduced. The results are as follows: Figure 17 As shown.

[0091] Example 8

[0092] This embodiment provides a thin-layer chromatography method for the identification of asparagus. The specific steps are the same as in Example 1, except that n-butanol in the developing solvent is replaced with an equal volume of methanol. The results are as follows: Figure 18 As shown.

[0093] Comparing the spectra of Examples 2-8, it can be seen that Example 4, due to the reduction of the proportion of n-butanol, shows fewer chemical components and less clear spots in the spectrum; in Example 5, removing ethyl acetate reduced the number of polar spots in the sample and decreased the separation; in Example 6, reducing the proportion of glacial acetic acid prevented the polar spots in the sample from developing well, resulting in a slight reduction in chemical information in the spectrum; in Example 7, reducing the proportion of water resulted in fewer spots at the reference standard position in the spectrum, and the corresponding effect was poor; in Example 8, replacing n-butanol in the developing solvent with methanol resulted in almost no effective chemical information in the obtained spectrum; while the developing effects of Examples 2 and 3 were both good. Therefore, it can be seen that the ratio of n-butanol:ethyl acetate:glacial acetic acid:water in the developing solvent can present a good separation effect when it is between (18-20):(2-4):(4-6):(6-8).

[0094] Comparative Examples 1-2

[0095] Take 1.0g of freeze-dried powder of Asparagus standard decoction, add the corresponding solvent according to the method in the table below (the rest is the same as in Example 1) to prepare the sample, evaporate the filtrate to dryness, and dissolve the residue in the corresponding solvent to obtain the test solution.

[0096]

[0097] Preparation of reference solution: Take appropriate amounts of arginine, leucine and alanine respectively, add 70% ethanol to dissolve them to prepare a solution containing 1 mg per 1 mL, which is used as the reference solution.

[0098] Preparation of developing systems: Prepare developing solvents by adding the corresponding reagents according to the table below to obtain different developing systems:

[0099]

[0100] The results are as follows Figures 19-20 As shown (where 1: test solution of Comparative Example 1; 2: test solution of Comparative Example 2; 3: asparagus reference material solution; 4: leucine reference solution; 5: arginine reference solution; 6: alanine reference solution).

[0101] Under developing solvent 2, neither comparative examples 1 nor 2 showed spots of the same color at the corresponding positions as the chromatograms of the reference medicinal materials, and the separation of the reference standards was poor. Under developing solvent 1, the chromatograms of the test sample showed spots of the same color at the corresponding positions as the chromatograms of the reference medicinal materials, but leucine and alanine reference standards did not show any colored spots, and arginine did not show spots of the same color at the same positions as the sample and the reference medicinal materials, making it impossible to confirm the type of components identified by asparagus thin-layer chromatography.

[0102] The results above show that the method provided by the present invention can qualitatively identify saponin components in asparagus products. At the same time, the overall identification method overcomes the problems of blurred color spots, poor separation effect and limited chromatographic information in the thin-layer chromatography identification of the prior art. It has the advantages of more chromatographic information, better separation effect and clear color spots. Comparing Examples 1-8 and Comparative Examples 1-2, it can be found that the present invention further improves the separation effect and the clarity of color spots by selecting a specific developing system.

[0103] The applicant declares that this invention illustrates the thin-layer chromatography identification method for asparagus drugs, including formulated granules, and its application through the above embodiments. However, this invention is not limited to the above embodiments, meaning that this invention does not necessarily rely on the above embodiments for implementation. Those skilled in the art should understand that any improvements to this invention, equivalent substitutions of raw materials for the product, addition of auxiliary components, and selection of specific methods all fall within the protection and disclosure scope of this invention.

[0104] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0105] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

Claims

1. A thin layer identification method of asparagus drugs, characterized in that, The asparagus medicine is any one of asparagus medicinal material, asparagus formula granule, asparagus water extract or asparagus standard decoction; The thin layer identification method comprises the following steps: (1) extracting the to-be-tested sample to obtain a test sample solution; (2) mixing the control sample with an alcohol solvent to obtain a control sample solution; (3) extracting the control medicinal material to obtain a control medicinal material solution; (4) performing thin layer chromatography on the test sample solution, the control sample solution and the control medicinal material solution, and identifying the to-be-tested sample according to the chromatography result; Steps (1), (2) and (3) are not distinguished in sequence; The control sample is proto-dioscin; The to-be-tested sample is asparagus water extract or asparagus formula granule, and the extracting step in step (1) is specifically as follows: mixing the to-be-tested sample with acetone for reflux extraction to obtain the test sample solution; The to-be-tested sample is asparagus medicinal material or asparagus standard decoction, and the extracting step in step (1) is specifically as follows: mixing the to-be-tested sample with water for extraction, and then refluxing extraction with acetone to obtain the test sample solution; The developing agent for the thin layer chromatography in step (4) is a mixed solution of n-butanol, ethyl acetate, glacial acetic acid and water, and the volume ratio of the n-butanol, the ethyl acetate, the glacial acetic acid and the water is (18-20):(2-4):(4-6):(6-8). The thin layer plate used in the thin layer chromatography in step (4) is a silica gel G plate.

2. The thin layer method for identifying aspartame drugs according to claim 1, characterized in that, The to-be-tested sample is asparagus water extract or asparagus formula granule, and the solid-liquid ratio of the to-be-tested sample to acetone is 1:(15-20) g / mL.

3. The thin layer method for identifying aspartame drugs according to claim 1, characterized in that, The solid-liquid ratio of the to-be-tested sample to water is 1:(25-35) g / mL.

4. The thin layer method for identifying aspartame drugs according to claim 1, wherein, The to-be-tested sample is asparagus medicinal material or asparagus standard decoction, and the solid-liquid ratio of the to-be-tested sample to acetone is 1:(15-20) g / mL.

5. The thin layer identification method of aspartic drugs according to claim 1, characterized in that, The alcohol solvent in step (2) comprises methanol.

6. Application of the thin layer identification method of the asparagus medicine according to any one of claims 1-5 in quality control of the asparagus medicine.

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