A thin layer identification method for Cynomorium songaricum granules

Abstract

The present invention discloses a thin layer chromatography identification method for Cynomorium songaricum granules, comprising: (1) preparing a test solution: taking the test granules, adding water to dissolve, adjusting the pH of the aqueous phase to 1-6, and extracting with an organic solvent; (2) preparing a control medicinal material solution: taking Cynomorium songaricum medicinal materials, boiling them with water, filtering, concentrating, obtaining a residual liquid, adding water to dissolve, adjusting the pH of the aqueous phase to 1-6, and extracting with an organic solvent; (3) performing thin layer chromatography comparison: taking the test solution and the control medicinal material solution, spotting them on the same silica gel GF 254 On the thin layer plate, toluene: dichloromethane: ethyl acetate: formic acid = 4-6: 4-6: 4-6: 0.8-1.2 is used as the developing agent. This method is used for the identification of Cynomorium songaricum granules. The operation is simple and convenient. The number of thin layer development spots is large, and the detection results are accurate and reliable.

Description

Technical Field

[0001] The invention relates to a drug qualitative analysis method, in particular to a Cynomorium songaricum granule thin layer identification method. Background Art

[0002] Cynomorium songaricum Rupr. is a dried fleshy stem of the Cynomorium songaricum Rupr. plant of the Cynomorium family. It is distributed in Xinjiang, Qinghai, Gansu, Ningxia, Inner Mongolia, Shaanxi and other places. It is sweet and warm in nature, and enters the liver, kidney and large intestine meridians. It has the effects of tonifying kidney yang, benefiting essence and blood, and moistening the intestines and relieving constipation. It is often used for kidney yang deficiency, essence and blood deficiency, waist and knee weakness, impotence and spermatorrhea, dry intestines and constipation. Chemical research has found that the main components of Cynomorium songaricum are flavonoids, triterpenes, steroids, organic acids, tannins, lignans, glycosides and amino acids.

[0003] Chinese medicine formula granules are a breakthrough in the application of traditional Chinese medicine slices. They are usually made of slices as raw materials, and are made through standardized extraction, concentration, drying and granulation. Their nature, flavor, meridians and efficacy are basically consistent with the original slices, and they have the advantages of no need for decoction, easy adjustment, storage and convenient use, and are gradually widely used. However, after the Chinese medicine slices are made into formula granules, the appearance changes greatly, and it is impossible to accurately determine whether a certain medicinal material exists only by appearance. Under the item of Cynomorium songaricum in the first volume of the 2020 edition of the Chinese Pharmacopoeia, there is only a thin layer identification project for Cynomorium songaricum medicinal materials, and there is a lack of corresponding quality control standards for Cynomorium songaricum formula granules. In the prior art, the Chinese medicine (formulated granules) standard issued by the Shanxi Provincial Food and Drug Administration, standard number: SXYPBZ (PFKL) -2021186, regarding the quality control of Cynomorium songaricum formula granules, liquid chromatography is used to determine whether Cynomorium songaricum medicinal materials exist. This method obtains comprehensive information, but the cost is high and the cycle for obtaining test results is long. Liu Shixin et al. (Study on the Quality Control Method of TLC Qualitative Identification of Shenkangning Capsules [J]. Shanghai Journal of Traditional Chinese Medicine, 2021, 55(10): 66-72.) disclosed a method for identifying Cynomorium songaricum in formula granules, including dissolving the formula granules in water, extracting with ethyl acetate to obtain the test solution and the reference medicinal material solution, developing the obtained sample solution by thin layer chromatography, immersing the plate with 0.04% DPPH anhydrous ethanol solution for color development, and finally comparing with gallic acid to determine the presence of Cynomorium songaricum granules. This method uses thin layer chromatography to identify Cynomorium songaricum, which is simple and fast, but gallic acid is not present only in Cynomorium songaricum medicinal materials. There is an error in identifying whether Cynomorium songaricum granules exist by this method. Summary of the invention

[0004] Purpose of the invention: The purpose of the present invention is to provide a fast, simple and accurate thin layer identification method for Cynomorium songaricum formula particles.

[0005] Technical solution: The thin-layer identification method of Cynomorium songaricum granules of the present invention comprises:

[0006] (1) Preparation of test solution: Take the particles to be tested, dissolve them in water, adjust the pH of the aqueous phase to 1-6, and extract with an organic solvent;

[0007] (2) Preparation of control medicinal material solution: Take Cynomorium songaricum, add water to decoct, filter, concentrate, obtain residual liquid, add water to dissolve, adjust the pH of the aqueous phase to 1-6, and extract with organic solvent;

[0008] (3) TLC comparison: Take the test sample solution and the control medicinal material solution and spot them on the same silica gel GF 254 On the thin layer plate, toluene: dichloromethane: ethyl acetate: formic acid = 4-6: 4-6: 4-6: 0.8-1.2 was used as the developing solvent.

[0009] Preferably, in order to obtain the best separation effect and remove some impurities, in the steps (1) and (2), an alcohol extraction step is further included before the water dissolution step, and the alcohol extraction step includes: dissolving with an alcohol solvent, filtering after ultrasonic treatment, and evaporating the filtrate to obtain a residue. Adding an alcohol extraction step before water dissolution helps to show the spots with low specific transfer values.

[0010] Preferably, the pH adjustment range in step (1) and step (2) is 1 to 4. When the pH is adjusted within the range of 1 to 4, the thin layer chromatography spots are clearest.

[0011] Preferably, by volume, the developing agent is toluene: dichloromethane: ethyl acetate: formic acid = 4.5-5.5: 4.5-5.5: 4.5-5.5: 0.9-1.1. Experiments have confirmed that when the components of the developing agent are within this ratio range, the clarity and separation of the spots after development are optimal. When toluene and dichloromethane are below this ratio, the spots after development are diffused. When ethyl acetate is below this ratio, the developing agent will be stratified and cannot be used for development.

[0012] Preferably, in step (1) and step (2), the pH adjuster is dilute hydrochloric acid with a mass fraction of less than 20%.

[0013] Preferably, in step (1) and step (2), the organic solvent used for extraction is ethyl acetate.

[0014] Preferably, in the step (2), the mass volume ratio of the Cynomorium songaricum medicinal material to the water used for decoction is 1-5 g:100 mL, and the decoction time is 20-40 minutes.

[0015] Preferably, in the alcohol extraction step, the ultrasonic treatment time is 20 to 40 minutes.

[0016] Preferably, in the alcohol extraction step, the alcohol solvent is added in a ratio of 1 g: 20-30 mL.

[0017] Preferably, the step (3) further comprises: drying after unfolding, and inspecting under ultraviolet light, and the test solution and the control medicinal material solution have the same spots at the same ratio shift value position of the thin layer chromatography.

[0018] Beneficial effects: Compared with the prior art, the present invention has the following significant advantages: 1. Effectively extract chemical substances in Cynomorium songaricum, with many thin layer chromatography spots, which is helpful for qualitative identification of Cynomorium songaricum medicinal materials; 2. It can be analyzed by placing it under ultraviolet light, and the operation method is simple; 3. Good specificity and wide application range. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 The thin layer analysis (TLC) spectrum of Example 1 of the present invention;

[0020] Figure 2 Thin layer analysis (TLC) patterns of Examples 2 and 3 of the present invention;

[0021] Figure 3 Thin layer analysis (TLC) spectrum of Example 3 of the present invention;

[0022] Figure 4 The thin layer analysis (TLC) spectrum of Example 4 of the present invention;

[0023] Figure 5 The thin layer analysis (TLC) spectrum of Example 4 of the present invention;

[0024] Figure 6 The thin layer analysis (TLC) spectrum of Example 4 of the present invention;

[0025] Figure 7 The thin layer analysis (TLC) spectrum of Example 5 of the present invention;

[0026] Figure 8 Thin layer analysis (TLC) spectrum of Comparative Example 1 of the present invention. DETAILED DESCRIPTION

[0027] The technical solution of the present invention is further described below in conjunction with the accompanying drawings.

[0028] Instruments and reagents: TLC VISUALIZER, METTLERTOLEDO, KQ-250E ultrasonic cleaner (Kunshan Ultrasonic Electronics Co., Ltd.), silica gel GF254 thin layer plate (Qingdao Kangyexin Pharmaceutical Silica Gel Desiccant Co., Ltd., Merck, Germany).

[0029] Methanol (Sinopharm Chemical Reagent Co., Ltd.), ethanol (Sinopharm Chemical Reagent Co., Ltd.), ethyl acetate (Sinopharm Chemical Reagent Co., Ltd.), dichloromethane (Sinopharm Chemical Reagent Co., Ltd.), formic acid (Sinopharm Chemical Reagent Co., Ltd.), hydrochloric acid (Shanghai Lingfeng Chemical Reagent Co., Ltd.), and toluene (Shanghai Lingfeng Chemical Reagent Co., Ltd.) were all analytically pure. Cynomorium songaricum reference medicinal material (batch number: 121393-200401) was purchased from the China Food and Drug Administration. Cynomorium songaricum formula granules (batch numbers: 19100019, 19100029, 19100039) were provided by Jiangyin Tianjiang Pharmaceutical Co., Ltd. Cynomorium songaricum formula granules include Cynomorium songaricum medicinal material extract and pharmaceutical excipients, with a Cynomorium songaricum extract content of 70% to 75%.

[0030] Example 1: Method for identifying samples to be tested

[0031] Preparation of test solution: Take 1 g of Cynomorium songaricum granules (batch number: 19100019), grind it into powder, add 20 ml of water to dissolve it, adjust the pH value to 1-2 with dilute hydrochloric acid, shake and extract with ethyl acetate twice, 20 ml each time, combine the ethyl acetate liquid, evaporate to dryness, add 1 ml of methanol to dissolve the residue, and use it as the test solution.

[0032] Preparation of control medicinal material solution: Take 1g of Cynomorium songaricum control medicinal material, add 50ml of water, heat and boil for 30 minutes, filter, concentrate the filtrate to about 20ml, adjust the pH value to 1-2 with dilute hydrochloric acid, shake and extract with ethyl acetate twice, 20ml each time, combine the ethyl acetate liquid, evaporate to dryness, add 1ml of methanol to the residue to dissolve it, and use it as the control medicinal material solution.

[0033] Take 2 μL, 5 μL, 10 μL, and 20 μL of the test solution, marked as 1 to 4, and 1 μL, 2 μL, 5 μL, and 10 μL of the control drug solution, marked as S1 to S4, and spot them on the same silica gel GF 254 On the thin layer plate, toluene-dichloromethane-ethyl acetate-formic acid (5:5:5:1) was used as the developing agent. The plate was developed, taken out, dried, and examined under ultraviolet light (254nm) (room temperature 24.8℃, humidity 66%). The results are shown in Figure 1 .

[0034] As can be seen from the figure, the method used to identify Cynomorium songaricum Granules has more TLC spots and more reliable results, but spots with lower transfer values ​​on the TLC of the test solution are missing, which needs further optimization.

[0035] Example 2: Adding an alcohol extraction step to identify the sample to be tested

[0036] Preparation of test solution: Take 1 g of Cynomorium songaricum granules (batch number: 19100019), grind it into powder, add 25 ml of methanol, ultrasonically treat it for 30 minutes, filter it, evaporate the filtrate to dryness, dissolve the residue in 20 ml of water, adjust the pH value to 1-2 with dilute hydrochloric acid, extract it with ethyl acetate by shaking twice, 20 ml each time, combine the ethyl acetate solutions, evaporate them to dryness, dissolve the residue in 1 ml of methanol, and use it as the test solution.

[0037] Preparation of control medicinal material solution: Take 1g of Cynomorium songaricum control medicinal material, add 50ml of water, heat and boil for 30 minutes, filter, concentrate the filtrate to near dryness, add 25ml of methanol, ultrasonically treat for 30 minutes, filter, evaporate the filtrate to dryness, add 20ml of water to the residue to dissolve it, adjust the pH value to 1-2 with dilute hydrochloric acid, shake and extract with ethyl acetate twice, 20ml each time, combine the ethyl acetate solutions, evaporate to dryness, add 1ml of methanol to the residue to dissolve it, and use it as the control medicinal material solution.

[0038] Preparation of negative control solution: Take 1 g of negative granule sample of Cynomorium songaricum and prepare negative control solution by the method of "Preparation of test solution" in this example.

[0039] 8 μL of the test solution of this example, recorded as 3, 5 μL of the control medicinal material solution, recorded as S2, and 5 μL of the control medicinal material solution in Example 1, recorded as S1, were applied to the same silica gel GF 254 The thin layer plate was developed with toluene-dichloromethane-ethyl acetate-formic acid (5:5:5:1) as the developing agent, taken out and dried, and examined under ultraviolet light (254nm) (room temperature 24.8℃, humidity 66%). The results are shown in Figure 2 Part a.

[0040] 8 μL of the test solution in this example was taken and spotted in triplicate, marked as 1, 2, and 3, 8 μL of the negative control solution was marked as 4, and 5 μL of the control medicinal material solution was marked as S, and spotted on the same silica gel GF 254 The thin layer plate was developed with toluene-dichloromethane-ethyl acetate-formic acid (5:5:5:1) as the developing agent, taken out and dried, and examined under ultraviolet light (254nm) (room temperature 24.8℃, humidity 66%). The results are shown in Figure 2 Part b.

[0041] The results show that the chromatogram of the test solution obtained in this example and the chromatogram of the reference medicinal material solution have a corresponding number of ultraviolet absorption spots ( Figure 2 Part a), negative control without interference ( Figure 2 Part b), therefore, the method in this embodiment was selected as the test solution, and the preparation method of the control medicinal material solution was used. The thin layer chromatographic information was clear and comprehensive, and the identification specificity was good.

[0042] Example 3: Effect of pH Adjustment on Identification Method

[0043] 3.1 pH adjustment steps

[0044] Test solution 1: Take 1 g of Cynomorium songaricum granules (batch number: 19100019), grind it into powder, add 25 ml of methanol, treat it with ultrasound for 30 minutes, filter it, evaporate the filtrate to dryness, add 1 ml of methanol to dissolve the residue, and use it as the test solution.

[0045] Test solution 2: Take 1 g of Cynomorium songaricum granules (batch number: 19100019), grind it into powder, add 25 ml of ethanol, treat it with ultrasound for 30 minutes, filter it, evaporate the filtrate to dryness, add 1 ml of ethanol to the residue to dissolve it, and use it as the test solution.

[0046] 8 μL of the test solution 1 in this example, recorded as 1, 8 μL of the test solution 2, recorded as 2, and 5 μL of the control medicinal material solution obtained in Example 2, recorded as S2, were respectively taken and applied to the same silica gel GF 254 The thin layer plate was developed with toluene-dichloromethane-ethyl acetate-formic acid (5:5:5:1) as the developing agent, taken out and dried, and examined under ultraviolet light (254nm) (room temperature 24.8℃, humidity 66%). The results are shown in Figure 2 Part a.

[0047] The results show that if the pH adjustment step is omitted, the components in the sample cannot be accurately extracted and effective thin layer chromatography cannot be obtained, so the pH adjustment step cannot be omitted.

[0048] 3.2 pH adjustment range

[0049] Test solution 1: Same as Example 2 "Preparation of test solution".

[0050] Test solution 2: Same as Example 2 "Preparation of test solution", except that the pH adjustment range is 3-4.

[0051] Test solution 3: Same as Example 2 "Preparation of test solution", except that the pH adjustment range is 5-6.

[0052] 8 μL of the test solution of this example, 1, 2, and 3, respectively, and the control medicinal material solution of Example 2, denoted as S, were taken and spotted on the same silica gel GF 254 The thin layer plate was developed with toluene-dichloromethane-ethyl acetate-formic acid (5:5:5:1) as the developing agent, taken out and dried, and examined under ultraviolet light (254nm) (room temperature 24.8℃, humidity 66%). The results are shown in Figure 3 .

[0053] The results showed that compared with pH values ​​1 to 4, the spots of samples with pH values ​​5 to 6 were significantly lighter, so the best pH adjustment range was 1 to 4.

[0054] Example 4: Factors affecting the expansion results

[0055] 4.1 Sample volume

[0056] Take 2 μL, 3 μL, 10 μL, and 20 μL of the test solution in Example 2, respectively, and record them as 1 to 4, and 1 μL, 2 μL, 5 μL, and 10 μL of the control medicinal material solution, and record them as 5 to 8, respectively, and spot them on the same silica gel GF 254 The thin layer plate was developed with toluene-dichloromethane-ethyl acetate-formic acid (5:5:5:1) as the developing agent, taken out and dried, and examined under ultraviolet light (254nm) (room temperature 24.8℃, humidity 66%). The results are shown in Figure 4 .

[0057] It can be seen from the figure that when the sample solution spotting volume is 10 μL and the control medicinal material solution spotting volume is 5 μL, the spots at the corresponding positions in the test sample chromatogram and the control medicinal material chromatogram clearly correspond to each other without other interference. Therefore, the sample solution spotting volume is selected to be 10 μL and the control medicinal material solution spotting volume is selected to be 5 μL.

[0058] 4.2 Developing agent type and ratio

[0059] Take the test solution and the control medicinal material solution in Example 2 and apply them to the same silica gel GF 254 Thin layer plates, where the sample solution was spotted in 10 μL, three times in parallel, marked as 1, 2, and 3, and the control drug solution was spotted in 5 μL, one time, marked as S. Different types of developing agents were used for development, taken out and dried, and examined under ultraviolet light (254 nm) (room temperature 24.8°C, humidity 66%). The types and proportions of developing agents were as follows:

[0060] Developing agent 1: cyclohexane-ethyl acetate-methanol-formic acid = 8:6:1:1 Development results are shown in Figure 5 Part a;

[0061] Developing agent 2: dichloromethane-ethyl acetate-formic acid = 5:5:1 Development results are shown in Figure 5 Part b;

[0062] Developing agent 3: toluene-ethyl acetate-formic acid = 5:5:1, the development results are shown in Figure 5 middle c part;

[0063] Developing agent 4: toluene-dichloromethane-ethyl acetate-formic acid = 5:5:2:1, the development results are shown in Figure 5 Part d.

[0064] Depend on Figure 5 It can be seen from parts a and c that when the developing solvent type and ratio are changed and dichloromethane is omitted, the UV absorption point diffusion exists on the TLC developing plate of the test solution and the control medicinal material solution, which is not conducive to subsequent observation. Figure 5 In parts b and d, if toluene is removed or the proportion of ethyl acetate is reduced, the UV absorption points cannot be separated and the number of spots is small, which is not conducive to subsequent comparison and qualitative analysis. Therefore, toluene-dichloromethane-ethyl acetate-formic acid 5:5:5:1 is the best developing agent. The appropriate range of developing agent ratio is: toluene: dichloromethane: ethyl acetate: formic acid = 4.5~5.5:4.5~5.5:4.5~5.5:0.9~1.1. Within this range, the clarity of the spots after development and the separation between the spots are the best. If toluene and dichloromethane are lower than this ratio, the spots after development will diffuse and be inconvenient to observe. If ethyl acetate is lower than this ratio, the developing agent will be stratified and cannot be used for development.

[0065] 4.3 Temperature

[0066] Take the test solution and the control medicinal material solution in Example 2 and apply them to the same silica gel GF 254 Thin layer plate, where the sample solution was spotted in 10 μL, three times in parallel, marked as 1, 2, 3, and the control drug solution was spotted in 5 μL, marked as S. Toluene-dichloromethane-ethyl acetate-formic acid (5:5:5:1) was used as the developing agent, and the plates were developed at an ambient temperature of 35°C and 4°C, respectively. The plates were taken out and dried, and examined under ultraviolet light (254 nm). The results are shown in Table 1. Figure 6 Part a and part b.

[0067] As can be seen from the figure, under different temperature conditions, the spots of the same color appear at the corresponding positions of the chromatogram of the test sample and the control medicinal material, and the separation effect is good. The experimental results show that temperature has no effect on the thin layer identification of the Cynomorium songaricum formula granules, indicating that the thin layer identification method has good durability at different temperatures.

[0068] 4.3 Humidity

[0069] The development was carried out according to the development conditions in Section 4.2 of this embodiment, except that the two silica gel plates were developed at the same temperature and the development humidity was 18% and 88% respectively. The development results are shown in Figure 6 Part c and part d.

[0070] As can be seen from the figure, under different humidity conditions, the spots of the same color appear at the corresponding positions of the chromatogram of the test sample and the control medicinal material, and the separation effect is good. The experimental results show that humidity has no effect on the thin layer identification of the Cynomorium songaricum formula granules, indicating that the thin layer identification method has good durability under different humidity conditions.

[0071] 4.4 Silicone sheets from different sources

[0072] The development was carried out according to the development conditions in Section 4.2 of this Example. The difference was that the development temperature of the two silica gel plates was the same. The development results were shown in Table 1. Figure 6 Part e and part f.

[0073] As can be seen from the figure, under different TLC plate conditions, the spots of the same color appear at the corresponding positions of the chromatogram of the test sample and the control medicinal material of the Cynomorium songaricum formula granules, and the separation effect is good. The experimental results show that the TLC plate has no significant effect on the TLC identification of Cynomorium songaricum formula granules, indicating that the TLC identification method has good durability for different TLC plates.

[0074] Example 5: Scope of application

[0075] Test solution 1: Same as Example 2 "Preparation of test solution".

[0076] Test solution 2: Same as Example 2 "Preparation of test solution", except that the batch number of Cynomorium songaricum formula granules is: 19100029.

[0077] Test solution 3: Same as Example 2 "Preparation of test solution", except that the batch number of Cynomorium songaricum formula granules is: 19100039.

[0078] 10 μL of the test solution 1, 2, and 3 of this example are taken respectively, and 5 μL of the control medicinal material solution in Example 2 is recorded as S, and then spotted on the same silica gel GF 254 The thin layer plate was developed with toluene-dichloromethane-ethyl acetate-formic acid (5:5:5:1) as the developing agent, taken out and dried, and examined under ultraviolet light (254nm) (room temperature 24.8℃, humidity 66%). The results are shown in Figure 7 .

[0079] As can be seen from the figure, the TLC development results of different batches of Cynomorium songaricum formula granules are consistent with those of the control medicinal materials, indicating that this method is suitable for the identification of different batches of Cynomorium songaricum formula granules.

[0080] Comparative Example 1: Pharmacopoeia Test Method (2020 Edition)

[0081] Preparation of test solution: Take 1 g of Cynomorium songaricum granules, grind them into powder, add 20 ml of ethyl acetate, treat with ultrasound for 30 minutes, filter, and concentrate the filtrate to 1 ml as the test solution.

[0082] Preparation of reference solution: Take ursolic acid reference substance and add methanol to make a solution containing 0.5 mg per 1 ml as the reference solution.

[0083] According to the thin layer chromatography method (General Rule 0502), 10 μl of the test solution was taken and spotted three times in parallel, marked as 1, 2, and 3. 4 μl of the reference solution was taken and marked as T. It was spotted on the same silica gel G thin layer plate, and toluene-ethyl acetate-formic acid (20:4:0.5) was used as the developing agent. After development, it was taken out, dried, sprayed with 10% sulfuric acid ethanol solution, and heated until the spots were clearly colored. In the chromatogram of the test sample, the same purple-red spot appeared at the corresponding position of the chromatogram of the reference. The results are shown in Figure 8 .

[0084] Depend on Figure 8 It can be seen that after the test solution and the reference solution were developed by the same thin layer chromatography, the same R f At the value, there is no corresponding color development point between the test solution and the reference solution, so this method cannot identify whether the test solution contains Cynomorium songaricum.

Claims

1. A thin layer identification method for Cynomorium songaricum granules, characterized in that: include: (1) Preparation of test solution: Take the particles to be tested, dissolve them in water, adjust the pH of the aqueous phase to 1-4, and extract with ethyl acetate; (2) Preparation of control medicinal material solution: Take Cynomorium songaricum, add water to decoct, filter, concentrate, obtain residual liquid, add water to dissolve, adjust the pH of the aqueous phase to 1-4, and extract with ethyl acetate; (3) TLC comparison: Take the test sample solution and the control medicinal material solution and spot them on the same silica gel GF 254 On the thin layer plate, toluene: dichloromethane: ethyl acetate: formic acid = 4.5~5.5: 4.5~5.5: 4.5~5.5:0.9~1.1 was used as the developing solvent; After unfolding, air-dry and inspect under ultraviolet light, the test solution and the control medicinal material solution have the same spots at the same ratio value position of the thin layer chromatogram; In steps (1) and (2), an alcohol extraction step is also included before the water dissolution step, and the alcohol extraction step includes: dissolving with an alcohol solvent, filtering after ultrasonic treatment, and evaporating the filtrate to obtain a first residue.

2. The Cynomorium songaricum granule thin layer identification method according to claim 1, characterized in that: In the steps (1) and (2), the pH adjuster is dilute hydrochloric acid with a mass fraction of less than 20%.

3. The Cynomorium songaricum granule thin layer identification method according to claim 1, characterized in that: In the step (2), the mass volume ratio of the Cynomorium songaricum medicinal material to the water used for decoction is 1-5 g:100 mL, and the decoction time is 20-40 minutes.

4. The thin layer identification method of Cynomorium songaricum granules according to claim 1, characterized in that: In the alcohol extraction step, the ultrasonic treatment time is 20 to 40 minutes.

5. The thin layer identification method of Cynomorium songaricum granules according to claim 1, characterized in that: In the alcohol extraction step, the alcohol solvent is added in a ratio of 1 g: 20-30 mL.

6. The thin layer identification method of Cynomorium songaricum granules according to claim 1, characterized in that: In the step (1) and the step (2), after extraction with ethyl acetate, the ethyl acetate is evaporated to dryness to obtain a second residue, and 1 mL of methanol is added to the second residue to dissolve, thereby obtaining a test solution and a control medicinal material solution, respectively.

7. The thin layer identification method of Cynomorium songaricum granules according to claim 6 is characterized in that: In the step (3), the sample volume of the test solution is 10 μL, and the sample volume of the control medicinal material solution is 5 μL.

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