Quality detection method for degreasing and hair growing tablets

Abstract

The invention discloses a quality detection method for degreasing and hair growing tablets, and belongs to the technical field of quality detection of traditional Chinese medicine preparations. According to the present invention, the optimal test sample preparation method and the optimal chromatography development condition are screened for each medicinal material in the fat removing and hair growing tablet, methodology investigation is further performed, and the results prove that the detection method has characteristics of strong specificity, good durability, high accuracy, good stability, reasonable design, strong operability and low detection cost. By applying the technology, the scientificity and universality of the quality standard of the degreasing and hair growing tablets can be remarkably improved, the quality can be better controlled, and a technical support is provided for guaranteeing the component stability and clinical curative effect consistency of a traditional Chinese medicine compound preparation.

Description

Technical Field

[0001] This invention belongs to the field of quality testing technology for traditional Chinese medicine preparations, and specifically relates to a quality testing method for a hair growth and degreasing tablet. Background Technology

[0002] As a traditional Chinese medicine compound preparation, the formula for Zhizhi Shengfa Pian (Quzhi Shengfa Tablets) is made from 13 Chinese medicinal herbs, including Angelica sinensis, Paeonia suffruticosa, Ligusticum chuanxiong, Dictamnus dasycarpus, and Cicadae periostracum, processed through a series of steps. Clinically, Zhizhi Shengfa Pian is mainly used to treat seborrheic alopecia, and it also has significant effects on scalp itching, dandruff, and excessive sebum secretion. Its mechanism of action is based on the synergistic effects of multiple herbs, such as Angelica sinensis' yin-nourishing and blood-tonifying properties, Paeonia suffruticosa's heat-clearing and blood-cooling properties, Ligusticum chuanxiong's blood-activating and qi-regulating properties to promote scalp blood circulation, Dictamnus dasycarpus and Cicadae periostracum's wind-dispelling and itching-relieving properties, and Sophora flavescens and Kochia scoparia's dampness-drying and sebum-removing properties, all working together to improve the scalp environment and promote healthy hair growth.

[0003] Existing thin-layer chromatography (TLC) identification methods for hair growth and degreasing tablets primarily rely on two approaches: first, they often use a single solvent to extract the sample and depend on simple developing systems and limited controls. This makes it difficult to comprehensively capture the characteristic components with varying polarities within the compound formula, resulting in insufficient information, weak specificity, and an inability to effectively distinguish genuine from counterfeit products; second, the developing systems used in these methods are relatively simple, leading to poor separation of complex components and issues such as spot overlap or tailing. These methods fail to guarantee robustness, specificity, precision, and reliability, making it impossible to provide reliable evidence for batch-to-batch consistency of formulation quality and stability of clinical efficacy, thus posing potential risks to quality control and clinical application. Summary of the Invention

[0004] To fill the gap in the quality standards for hair growth and degreasing tablets regarding thin-layer identification methods, the purpose of this invention is to provide a quality testing method for hair growth and degreasing tablets, thereby solving the technical problems that existing testing methods for hair growth and degreasing tablets cannot guarantee durability, specificity, precision, and reliability.

[0005] To achieve the above objectives, the present invention employs the following technical solution:

[0006] The first aspect of this invention discloses a method for quality testing of hair growth and degreasing tablets, comprising at least one of steps 1) to 4) for testing:

[0007] 1) Thin-layer chromatography identification of Angelica sinensis and Ligusticum chuanxiong

[0008] Preparation of the test solution: Take the fine powder of degreased hair growth tablets, add methanol, let stand, sonicate, filter, evaporate the filtrate to dryness, dissolve the residue in ethanol to obtain the test solution;

[0009] Preparation of negative control solution lacking Angelica sinensis and Ligusticum chuanxiong: negative samples lacking Angelica sinensis and Ligusticum chuanxiong were prepared according to the prescription and preparation method of the hair growth tablets, and negative control solution lacking Angelica sinensis and Ligusticum chuanxiong was prepared according to the preparation method of the test solution.

[0010] Preparation of Angelica sinensis reference medicinal material solution and Ligusticum chuanxiong reference medicinal material solution: Angelica sinensis reference medicinal material and Ligusticum chuanxiong reference medicinal material were taken respectively and prepared according to the preparation method of test sample solution.

[0011] The test solution, the negative control solution lacking Angelica sinensis and Ligusticum chuanxiong, the Angelica sinensis reference medicinal material solution, and the Ligusticum chuanxiong reference medicinal material solution were spotted onto the same silica gel thin-layer plate. The plate was developed using hexane-ethyl acetate-glacial acetic acid as the developing solvent. The plate was then removed, dried, and examined under ultraviolet light. In the chromatogram of the test sample, spots of the same color appeared at the corresponding positions as in the chromatogram of the reference medicinal materials.

[0012] 2) Thin-layer chromatography identification of peony bark

[0013] Preparation of the test solution: Take the fine powder of degreased hair growth tablets, add methanol, shake, filter, evaporate the filtrate to dryness, dissolve the residue in acetone to obtain the test solution;

[0014] Preparation of negative control solution lacking peony bark: Prepare negative sample lacking peony bark according to the prescription and preparation method of hair growth tablets, and prepare negative control solution lacking peony bark according to the preparation method of test solution;

[0015] Preparation of peony bark reference solution: Take peony bark reference material and prepare peony bark reference solution according to the preparation method of test solution;

[0016] Preparation of paeonol reference solution: Weigh paeonol reference standard, dissolve it in acetone to obtain paeonol reference solution;

[0017] The test sample solution, the negative control solution lacking peony bark, the peony bark reference medicinal material solution, and the paeonol reference solution were spotted onto the same silica gel thin-layer plate. Using hexane-ethyl acetate-glacial acetic acid as the developing solvent, vanillin-sulfuric acid ethanol solution was sprayed on the plate and heated until the spots were clearly visible. In the chromatogram of the test sample, spots of the same color appeared at the corresponding positions as those in the chromatograms of the reference standard and the reference medicinal material.

[0018] 3) Identification of Sophora flavescens medicinal materials

[0019] Preparation of the test solution: Take the fine powder of degreased hair growth tablets, add concentrated ammonia test solution and chloroform, sonicate in an ice bath, filter, evaporate the filtrate to dryness, dissolve the residue in chloroform to obtain the test solution;

[0020] Preparation of negative control solution lacking Sophora flavescens: Prepare negative sample lacking Sophora flavescens according to the prescription and preparation method of hair growth tablets, and prepare negative control solution lacking Sophora flavescens according to the preparation method of test solution;

[0021] Preparation of matrine reference solution: Weigh matrine reference standard, dissolve it in acetone to obtain matrine reference solution;

[0022] The test solution, the negative control solution lacking Sophora flavescens, and the matrine reference solution were spotted onto the same silica gel thin-layer plate. The plate was developed with chloroform-methanol. The plate was then removed, dried, sprayed with potassium bismuth iodide reagent, and examined under sunlight. In the chromatogram of the test sample, orange spots appeared at the same positions as those of the reference.

[0023] 4) Identification of processed Polygonum multiflorum medicinal material

[0024] Preparation of the test solution: Take the fine powder of degreased hair growth tablets, add ethanol, reflux, filter, and concentrate the filtrate to obtain the solution;

[0025] Preparation of negative control solution lacking processed Polygonum multiflorum: Prepare negative sample lacking processed Polygonum multiflorum according to the prescription and preparation method of hair growth tablets, and prepare negative control solution lacking processed Polygonum multiflorum according to the preparation method of test solution.

[0026] Preparation of prepared Polygonum multiflorum reference material solution: Take prepared Polygonum multiflorum reference material and prepare prepared Polygonum multiflorum reference material solution according to the preparation method of test sample solution;

[0027] Spot the test sample solution, the negative control solution lacking processed Polygonum multiflorum, and the reference medicinal material solution of processed Polygonum multiflorum onto the same silica gel thin-layer plate. Develop the plate using chloroform-methanol as the developing solvent, remove the plate, air dry it, and examine it under ultraviolet light. In the chromatogram of the test sample, fluorescent spots of the same color appear at the corresponding positions as in the chromatogram of the reference medicinal material.

[0028] Preferably, in step 1), the ratios of the amount of degreased hair growth powder, negative samples lacking Angelica sinensis and Ligusticum chuanxiong, Angelica sinensis reference material, and Ligusticum chuanxiong reference material to methanol are 5g:25mL, 5g:25mL, 1g:25mL, and 1g:25mL, respectively; the standing time is 30min, the ultrasonic treatment time is 10min, and the volume of ethanol used to dissolve the residue is 1mL.

[0029] Preferably, in step 1), the sample volume is 5 μL, and the thin-layer plate used is silica gel GF. 254 Thin-layer plate; the developing solvent is a mixed solution of n-hexane, ethyl acetate and glacial acetic acid in a volume ratio of 30:10:1.

[0030] Preferably, in step 2), the ratios of the amount of the degreased hair growth powder, the negative sample lacking peony bark, and the peony bark negative sample control material to methanol are 3g:20mL, 3g:20mL, and 1g:10mL, respectively; the ratio of the amount of paeonol reference standard to acetone is 5mg:10mL; and the shaking time is 10min.

[0031] Preferably, in step 2), the sample volume is 10 μL; the thin-layer plate used is a silica gel G thin-layer plate; the developing solvent is a mixed solution of n-hexane, ethyl acetate and glacial acetic acid with a volume ratio of 4:1:0.1; the vanillin sulfuric acid ethanol concentration is 2% vanillin sulfuric acid ethanol solution, and the heating and color development temperature is 105℃.

[0032] Preferably, in step 3), the sample amount of the degreased hair growth tablet powder is 5g, the added volumes of concentrated ammonia solution and chloroform are 2mL and 25mL respectively, and the added volume of chloroform for the residue is 2mL; in the preparation of the negative control solution lacking Sophora flavescens, the sample amount of the negative sample lacking Sophora flavescens is 5g; in the preparation of the matrine reference solution, the ratio of matrine reference standard to acetone is 2mg:10mL; and the ice bath ultrasonic treatment time is 30min.

[0033] Preferably, in step 3), the sample volume is 3 μL; the thin-layer plate used is a silica gel G plate; and the developing solvent is a mixed solution of chloroform and methanol with a volume ratio of 5:0.8.

[0034] Preferably, in step 4), the ratios of the amount of the degreased hair growth powder, the negative sample lacking processed Polygonum multiflorum, and the controlled material of processed Polygonum multiflorum to ethanol are 5g:20mL, 5g:20mL, and 1g:20mL, respectively; the reflux time is 60min; and the filtrate is concentrated to 1mL.

[0035] Preferably, in step 4), the sample volume is 2 μL; the thin-layer plate used is a silica gel G plate; the plate is developed twice with chloroform-methanol as the developing solvent. In the first development, the volume ratio of chloroform to methanol in the developing solvent is 7:3, and the plate is developed to 3.5 cm; in the second development, the volume ratio of the developing solvent is 20:1, and the plate is developed to 7 cm.

[0036] Preferably, step 1) is performed under ultraviolet light at 365nm and 254nm; step 4) is performed under ultraviolet light at 365nm.

[0037] Compared with the prior art, the present invention has the following beneficial effects:

[0038] This invention provides a quality testing method for hair growth and degreasing tablets. It develops a comprehensive thin-layer chromatography (TLC) identification method for several key medicinal materials in the prescription (Angelica sinensis, Ligusticum chuanxiong, Paeonia suffruticosa, Sophora flavescens, and processed Polygonum multiflorum), particularly those containing raw powder and other major medicinal materials that constitute a significant portion of the prescription. The study focuses on the selection of TLC plates, optimization of the developing solvent, sample preparation, and spotting conditions to screen for the optimal sample preparation method and TLC identification conditions. The process design is reasonable, highly operable, fast, accurate, and cost-effective. Therefore, this method is simple to operate, low in cost, highly operable, and applicable to the quality control of multiple batches of samples, enabling TLC identification of various components (Angelica sinensis, Ligusticum chuanxiong, Paeonia suffruticosa, Sophora flavescens, and processed Polygonum multiflorum) in hair growth and degreasing tablets. Attached Figure Description

[0039] Figure 1 The image shows the thin-layer chromatography identification of Angelica sinensis and Ligusticum chuanxiong in Example 1; where 1 is the Angelica sinensis reference solution, 2 is the Ligusticum chuanxiong reference solution, 3 is the negative control solution lacking Angelica sinensis and Ligusticum chuanxiong, and 4-6 are the test sample solutions (230104, 230507, 230701).

[0040] Figure 2 The image shows a thin-layer chromatography (TLC) image obtained by optimizing the extraction solvent during the preparation of the test solution in Example 1 of this invention; wherein, 1 is the TLC result of the extraction solvent diethyl ether, 2 is the TLC result of the extraction solvent ethyl acetate, and 3 is the TLC result of the extraction solvent methanol.

[0041] Figure 3 The image shows a thin-layer identification diagram obtained by optimizing the developing solvent in the developing system conditions in Example 1 of this invention; wherein, A is cyclohexane-ethyl acetate (4:1), B is cyclohexane-ethyl acetate (9:1), C is n-hexane-ethyl acetate-glacial acetic acid (30:10:1), 1 is Angelica sinensis reference medicinal material solution, 2 is Ligusticum chuanxiong reference medicinal material solution, 3 is negative control solution lacking Angelica sinensis and Ligusticum chuanxiong, and 4 is test sample solution;

[0042] Figure 4 The image shows the thin-layer identification diagram of the optimal thin-layer plate obtained by the present invention under the optimized development system conditions in Example 1; wherein, 1 is the Angelica sinensis reference medicinal material solution, 2 is the Ligusticum chuanxiong reference medicinal material solution, 3 is the negative control solution lacking Angelica sinensis and Ligusticum chuanxiong, and 4 is the test sample solution.

[0043] Figure 5 In Example 1, during the durability test of this invention, silicone GF produced by Qingdao Ocean Chemical Co., Ltd. was used. 254The results of thin-layer chromatography identification are shown in the figure; where 1 is the Angelica sinensis reference solution, 2 is the Ligusticum chuanxiong reference solution, 3 is the negative control solution lacking Angelica sinensis and Ligusticum chuanxiong, and 4 is the test sample solution.

[0044] Figure 6 The thin-layer identification diagrams obtained in the durability test of the present invention in Example 1 under different temperature and humidity conditions are shown; wherein, the upper diagram is under the conditions of 26.5℃ and 41% RH, and the lower diagram is under the conditions of 5℃ and 70% RH; 1 is the Angelica sinensis reference medicinal material solution, 2 is the Ligusticum chuanxiong reference medicinal material solution, 3 is the negative control solution lacking Angelica sinensis and Ligusticum chuanxiong, and 4 is the test sample solution;

[0045] Figure 7 The image shows a thin-layer chromatography (TLC) diagram of the peony bark in Example 2. 1 is a paeonol reference solution, 2 is a peony bark reference solution, 3 is a negative control solution lacking peony bark, and 4-6 are the test solutions (230104, 230507, 230701).

[0046] Figure 8 The image shown is a thin-layer chromatography (TLC) identification diagram obtained by optimizing the extraction solvent during the preparation of the test sample solution in Example 2 of this invention; wherein, 1 is the paeonol reference solution, 2 is the TLC result of the extraction solvent methanol, 3 is the TLC result of the extraction solvent ethanol, 4 is the TLC result of the extraction solvent ethyl acetate, and 5 is the TLC result of the extraction solvent diethyl ether.

[0047] Figure 9 The image shown is the optimal thin-layer identification diagram obtained by testing thin-layer plates from different manufacturers and under different temperatures and humidity conditions in the durability test of the present invention in Example 2; wherein, 1 is paeonol reference solution, 2 is peony bark reference medicinal material solution, 3 is negative control solution lacking peony bark, and 4 is test sample solution;

[0048] Figure 10 The image shows a thin-layer chromatography (TLC) image of Sophora flavescens in Example 3; where 1 is a matrine reference solution, 2 is a negative control solution lacking Sophora flavescens, and 3-5 are test solutions (230104, 230507, 230701).

[0049] Figure 11 The image shown is a thin-layer identification diagram obtained by optimizing the preparation method during the preparation of the test solution in Example 3 of the present invention; wherein, 1 is matrine reference solution, 2 is test solution A, and 3 is test solution B;

[0050] Figure 12 This is a thin-layer identification image obtained by optimizing the type of thin-layer plate under the development system conditions in Example 3 of the present invention; from left to right, they are a silica gel G thin-layer plate, a silica gel G thin-layer plate prepared with 2% sodium hydroxide, and a GF thin-layer plate, respectively. 254 Thin-layer plates: 1 is matrine reference solution, 2 is negative control solution lacking matrine, and 3 is test solution;

[0051] Figure 13 The image shown is a thin-layer identification diagram obtained by optimizing the sample amount under the development system conditions in Example 3 of the present invention; wherein, 1 is the thin-layer result with a sample amount of 1 μL, 2 is the thin-layer result with a sample amount of 3 μL, 3 is the thin-layer result with a sample amount of 5 μL, and 4 is the thin-layer result with a sample amount of 7 μL.

[0052] Figure 14 The optimal thin-layer identification diagrams obtained in Example 3 of this invention during the durability test of thin-layer plates from different manufacturers and under different temperatures and humidity conditions are shown. In each diagram, 1 is the matrine reference solution, 2 is the negative control solution lacking matrine, and 3 is the test solution.

[0053] Figure 15 The image shows a thin-layer chromatography identification diagram of processed Polygonum multiflorum in Example 4; where 1 is the reference solution of Polygonum multiflorum, 2 is the negative control solution without processed Polygonum multiflorum, and 3-5 are the test solutions (230104, 230507, 230701).

[0054] Figure 16 The images shown are thin-layer identification diagrams obtained in Example 4 of this invention during the durability test of thin-layer plates from different manufacturers and under different temperatures and humidity conditions; in each diagram, 1 is the reference medicinal material solution of Polygonum multiflorum, 2 is the negative control solution without processed Polygonum multiflorum, and 3 is the test sample solution. Detailed Implementation

[0055] To enable those skilled in the art to understand the features and effects of the present invention, the following descriptions and definitions are only general descriptions of the terms and expressions mentioned in the specification and claims. Unless otherwise specified, all technical and scientific terms used herein have the ordinary meaning understood by those skilled in the art regarding the present invention, and in the event of any conflict, the definitions in this specification shall prevail.

[0056] The theories or mechanisms described and disclosed herein, whether right or wrong, should not in any way limit the scope of the invention, that is, the contents of the invention can be implemented without being limited by any particular theory or mechanism.

[0057] In this document, all features defined by numerical ranges or percentage ranges, such as numerical values, quantities, contents, and concentrations, are for the sake of brevity and convenience only. Accordingly, descriptions of numerical ranges or percentage ranges should be considered as covering and specifically disclosing all possible sub-ranges and individual numerical values ​​(including integers and fractions) within those ranges.

[0058] In this article, unless otherwise specified, “contains,” “includes,” “containing,” “has,” or similar terms cover the meanings of “composed of” and “mainly composed of,” for example, “A contains a” covers the meanings of “A contains a and others” and “A contains only a.”

[0059] For the sake of brevity, not all possible combinations of the technical features in each implementation scheme or embodiment are described herein. Therefore, as long as there is no contradiction in the combination of these technical features, the technical features in each implementation scheme or embodiment can be combined arbitrarily, and all possible combinations should be considered within the scope of this specification.

[0060] In this article, the hair growth and degreasing tablets are a non-exclusive product, with 21 approved manufacturers. The formula and manufacturing method of the hair growth and degreasing tablets are as follows:

[0061]

prescription

[0062]

Preparation

[0063] The hair growth and degreasing tablets used in this article are produced by Shanxi Renyuantang Pharmaceutical Co., Ltd. (National Drug Approval Number Z14020253). Its quality standard is included in Volume 10 of the "Drug Standards of the Ministry of Health: Traditional Chinese Medicine Compound Preparations" (WS3-B-2003-95).

[0064] This invention provides a quality testing method for degreasing hair growth tablets, comprising at least one of S1 to S4 for testing:

[0065] Thin-layer chromatography identification of S1, Angelica sinensis, and Ligusticum chuanxiong.

[0066] Preparation of the test solution: Take the fine powder of the degreased hair growth tablets and place it in an Erlenmeyer flask. Add an appropriate amount of methanol, seal tightly, let stand, sonicate, filter, evaporate the filtrate to dryness, and dissolve the residue in ethanol to obtain the test solution.

[0067] Preparation of negative control solution lacking Angelica sinensis and Ligusticum chuanxiong: According to the original prescription of the hair growth tablets, weigh 0.2 times the amount of medicinal materials lacking Angelica sinensis and Ligusticum chuanxiong, and prepare a negative sample lacking Angelica sinensis and Ligusticum chuanxiong according to the above preparation method; place the negative sample lacking Angelica sinensis and Ligusticum chuanxiong in an Erlenmeyer flask, add an appropriate amount of methanol, seal tightly, let stand, sonicate, filter, evaporate the filtrate to dryness, and dissolve the residue in ethanol to obtain the solution;

[0068] Preparation of Angelica sinensis reference material solution: Take Angelica sinensis reference material, grind it into fine powder, place it in an Erlenmeyer flask, add an appropriate amount of methanol, seal tightly, let stand, sonicate, filter, evaporate the filtrate to dryness, add ethanol to dissolve the residue to obtain Angelica sinensis reference material solution.

[0069] Preparation of Ligusticum chuanxiong reference material solution: Grind Ligusticum chuanxiong reference material into fine powder, place it in an Erlenmeyer flask, add an appropriate amount of methanol, seal tightly, let stand, sonicate, filter, evaporate the filtrate to dryness, dissolve the residue in ethanol to obtain Ligusticum chuanxiong reference material solution.

[0070] In the preparation of each solution, the ratios of methanol used for the degreased hair growth powder, the negative sample lacking Angelica sinensis and Ligusticum chuanxiong, the Angelica sinensis reference material, and the Ligusticum chuanxiong reference material were 5g:25mL, 5g:25mL, 1g:25mL, and 1g:25mL, respectively.

[0071] Thin-layer chromatography test: Take the above test solution, negative control solution lacking Angelica sinensis and Ligusticum chuanxiong, Angelica sinensis reference medicinal material solution and Ligusticum chuanxiong reference medicinal material solution, and spot them separately on the same silica gel thin-layer plate. Use n-hexane-ethyl acetate-glacial acetic acid as the developing solvent, develop, remove, air dry, and examine under ultraviolet light. In the chromatogram of the test sample, spots of the same color appear at the corresponding positions as in the chromatogram of the reference medicinal materials. The negative control does not have such spots.

[0072] The sample volume was 5 μL, and the thin-layer plate used was silica gel GF. 254 Thin-layer plate; the developing solvent is a mixed solution of n-hexane, ethyl acetate and glacial acetic acid in a volume ratio of 30:10:1; the inspection under ultraviolet light is performed under ultraviolet light at 365 nm and 254 nm respectively.

[0073] S2. Thin-layer chromatography identification of peony bark.

[0074] Preparation of the test solution: Take the fine powder of degreased hair growth tablets and place it in an Erlenmeyer flask. Add an appropriate amount of methanol, stopper tightly, shake, filter, evaporate the filtrate to dryness, and dissolve the residue in acetone to obtain the test solution.

[0075] Preparation of negative control solution lacking peony bark: According to the original prescription of the hair growth tablets, weigh 0.2 times the amount of medicinal material lacking peony bark, and prepare a negative sample lacking peony bark according to the above preparation method; place the negative sample lacking peony bark in an Erlenmeyer flask, add an appropriate amount of methanol, seal tightly, shake, filter, evaporate the filtrate to dryness, and dissolve the residue in acetone to obtain the solution;

[0076] Preparation of peony bark reference material solution: Place fine powder of peony bark reference material in an Erlenmeyer flask, add an appropriate amount of methanol, stopper tightly, shake, filter, evaporate the filtrate to dryness, dissolve the residue in acetone to obtain the solution;

[0077] Preparation of paeonol reference solution: Accurately weigh paeonol reference standard, add an appropriate amount of acetone to dissolve, and the solution is obtained.

[0078] In the preparation of each solution, the ratio of the amount of degreased hair growth powder, negative sample lacking peony bark, and peony bark reference material to methanol was 3g:20mL, 3g:20mL, and 1g:10mL, respectively, and the ratio of the amount of paeonol reference standard to acetone was 5mg:10mL.

[0079] Thin-layer chromatography test: Apply the above test solution, negative control solution lacking peony bark, peony bark reference material solution, and paeonol reference solution separately to the same silica gel thin-layer plate. Use n-hexane-ethyl acetate-glacial acetic acid as the developing solvent, spray with vanillin-sulfuric acid ethanol solution, and heat until the spots are clearly visible. In the chromatogram of the test sample, spots of the same color appear at the corresponding positions as in the chromatograms of the reference standard and the reference medicinal material. No such spots appear in the negative control.

[0080] The sample volume was 10 μL; the thin-layer plate used was a silica gel G thin-layer plate; the developing solvent was a mixed solution of n-hexane, ethyl acetate and glacial acetic acid with a volume ratio of 4:1:0.1; the vanillin sulfuric acid ethanol solution had a concentration of 2% vanillin sulfuric acid ethanol solution, and the heating temperature for color development was 105℃.

[0081] S3. Identification of Sophora flavescens medicinal materials

[0082] Preparation of the test solution: Take the fine powder of degreased hair growth tablets and place it in an Erlenmeyer flask. Add an appropriate amount of concentrated ammonia test solution and chloroform. Seal tightly and sonicate in an ice bath. Filter and evaporate the filtrate to dryness. Dissolve the residue in chloroform to obtain the test solution.

[0083] Preparation of negative control solution lacking Sophora flavescens: According to the original prescription of the hair growth tablets, weigh 0.2 times the amount of medicinal material lacking Sophora flavescens, and prepare a negative sample lacking Sophora flavescens according to the above preparation method; place the negative sample lacking Sophora flavescens in an Erlenmeyer flask, add an appropriate amount of concentrated ammonia test solution and chloroform, seal tightly, sonicate in an ice bath, filter, evaporate the filtrate to dryness, dissolve the residue in chloroform, and obtain the solution;

[0084] Preparation of matrine reference solution: Accurately weigh matrine reference standard, add an appropriate amount of acetone to dissolve it, the ratio of matrine reference standard to acetone is 2mg:10mL, and the solution is obtained.

[0085] Thin-layer chromatography test: Take the above test solution, negative control solution lacking Sophora flavescens, and matrine reference solution, and spot them separately on the same silica gel thin-layer plate. Use chloroform-methanol as the developing solvent, remove the plate, air dry it, spray it with potassium bismuth iodide test solution, and examine it under sunlight. In the chromatogram of the test sample, orange spots appear at the corresponding positions as those of the reference solution; while the negative control solution does not have such spots.

[0086] The sample volume was 3 μL; the thin-layer plate used was a silica gel G plate; and the developing solvent was a mixed solution of chloroform and methanol with a volume ratio of 5:0.8.

[0087] S4. Identification of processed Polygonum multiflorum (He Shou Wu) medicinal materials

[0088] Preparation of the test solution: Take the fine powder of the degreased hair growth tablets and place it in an Erlenmeyer flask. Add an appropriate amount of ethanol, reflux, filter, and concentrate the filtrate to obtain the test solution.

[0089] Negative control solution lacking processed Polygonum multiflorum: According to the original prescription of the hair growth tablets, weigh 0.2 times the amount of medicinal material lacking processed Polygonum multiflorum, and prepare a negative sample lacking processed Polygonum multiflorum according to the above preparation method; place the negative sample lacking processed Polygonum multiflorum in an Erlenmeyer flask, add an appropriate amount of ethanol, reflux, filter, and concentrate the filtrate to obtain the solution.

[0090] Preparation of Polygonum multiflorum reference material solution: Take fine powder of prepared Polygonum multiflorum reference material and place it in an Erlenmeyer flask, add an appropriate amount of ethanol, reflux, filter, concentrate the filtrate to obtain the solution;

[0091] In the preparation of each solution, the ratio of the amount of degreased hair growth powder, negative sample lacking processed Polygonum multiflorum, and control material of processed Polygonum multiflorum to ethanol was 5g:20mL, 5g:20mL, and 1g:20mL, respectively; the reflux time was 60min; and the filtrate was concentrated to 1mL.

[0092] Thin-layer chromatography test: Take the above test solution, the negative control solution without processed Polygonum multiflorum, and the prepared Polygonum multiflorum reference material solution, and spot them separately on the same silica gel thin-layer plate. Use chloroform-methanol as the developing solvent, develop, remove, air dry, and examine under ultraviolet light; in the chromatogram of the test sample, fluorescent spots of the same color appear at the corresponding positions as in the chromatogram of the reference material; while the negative control does not have such spots;

[0093] The sample volume was 2 μL; the thin-layer plate used was a silica gel G plate; the plate was developed twice with chloroform-methanol as the developing solvent. In the first development, the volume ratio of chloroform to methanol in the developing solvent was 7:3, and in the second development, the volume ratio of chloroform to methanol in the developing solvent was 20:1.

[0094] It should be noted that S1 to S4 in this method have no order.

[0095] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading this description, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

[0096] The following examples use instruments and equipment conventional in the art. Experimental methods in the following examples, unless otherwise specified, are generally performed under standard conditions or as recommended by the manufacturer. All raw materials used in the following examples are conventional commercially available products with specifications in the art, unless otherwise stated.

[0097] 1. Experimental apparatus

[0098] Table 1 Experimental Instruments

[0099] Instrument Name model Manufacturer Electronic balance CP213 Ohaus Instruments (Shanghai) Co., Ltd. Electronic balance BSA224S Sartorius Scientific Instruments (Beijing) Co., Ltd. CNC ultrasonic cleaner KQ-500DE Kunshan Ultrasonic Instruments Co., Ltd. Electric constant temperature water bath HH-S6A Beijing Kewei Yongxing Instrument Co., Ltd. High-efficiency multi-functional crusher TQ-500 Shanghai Tianqi Shengshi Technology Co., Ltd. Dark box ultraviolet analyzer ZF-1B Wuxi Jiuping Instrument Co., Ltd. Electric constant temperature drying oven DHG-9070A Shanghai Jinghong Experimental Equipment Co., Ltd. Vacuum drying oven DZF-6050 Shanghai Yiheng Scientific Instruments Co., Ltd. refrigerator BCD-452WDPF Qingdao Haier Co., Ltd. Smart dehumidifier ERS-860L Hangzhou Duole Information & Electric Appliance Co., Ltd. Rotary evaporator RE-5210A Shanghai Yarong Biochemical Instrument Factory Circulating water vacuum pump SHZ-III Shanghai Yarong Biochemical Instrument Factory Temperature-controlled electric heating mantle ZDHW-10000mL Beijing Zhongxing Weiye Century Instrument Co., Ltd.

[0100] 2. Experimental reagents

[0101] Table 2 Experimental Drugs and Reagents

[0102]

[0103]

[0104] Example 1: Identification of Angelica sinensis and Ligusticum chuanxiong in the degreasing and hair growth tablets

[0105] I. Identification Methods

[0106] 1. Preparation of test solution: Take 5g of fine powder from three batches of hair growth tablets (batch numbers: 230104, 230507, 230701) produced by Shanxi Renyuantang Pharmaceutical Co., Ltd., place them in an Erlenmeyer flask, add 25mL of methanol, seal tightly, let stand for 30min, sonicate for 10min, filter, evaporate the filtrate to dryness, and dissolve the residue in 1mL of ethanol to obtain the test solution;

[0107] 2. Preparation of negative control solution lacking Angelica sinensis and Ligusticum chuanxiong: According to the original prescription of the hair growth tablets, weigh 0.2 times the amount of medicinal materials lacking Angelica sinensis and Ligusticum chuanxiong, and prepare a negative sample lacking Angelica sinensis and Ligusticum chuanxiong according to the above preparation method; place 5g of negative sample lacking Angelica sinensis and Ligusticum chuanxiong in an Erlenmeyer flask, add 25mL of methanol, seal tightly, let stand, sonicate, filter, evaporate the filtrate to dryness, dissolve the residue in ethanol to obtain the negative control solution lacking Angelica sinensis and Ligusticum chuanxiong;

[0108] 3. Preparation of Angelica sinensis reference material solution: Take 1g of Angelica sinensis reference material, grind it into fine powder, place it in an Erlenmeyer flask, add 25mL of methanol, seal tightly, let stand for 30min, sonicate for 10min, filter, evaporate the filtrate to dryness, add 1mL of ethanol to dissolve the residue to obtain Angelica sinensis reference material solution.

[0109] 4. Preparation of Ligusticum chuanxiong reference material solution: Take 1g of Ligusticum chuanxiong reference material, grind it into fine powder, place it in an Erlenmeyer flask, add 25mL of methanol, seal tightly, let stand for 30min, sonicate for 10min, filter, evaporate the filtrate to dryness, add 1mL of ethanol to dissolve the residue to obtain Ligusticum chuanxiong reference material solution.

[0110] 5. Thin-layer chromatography test: Take 5 μL of each of the above four solutions and spot them on the same silica gel GF plate. 254 On the thin-layer plate, hexane-ethyl acetate-glacial acetic acid (30:10:1) was used as the developing solvent. The plate was then removed, dried, and examined under ultraviolet light at 365 nm and 254 nm, respectively.

[0111] The results are as follows Figure 1 As shown, in the chromatograms of the three batches of test samples, spots of the same color were displayed at the corresponding positions as in the chromatogram of the reference medicinal material, and there was no interference from the negative control.

[0112] II. Examination under different conditions

[0113] 1. Investigation of solvent extraction in the preparation method of the test sample

[0114] Take 5g of the fine powder of the degreasing hair growth tablets and place them in conical flasks. Use ether, ethyl acetate and methanol as extraction solvents respectively for the investigation. Add 25mL of each solvent, seal tightly, let stand for 30min, sonicate for 10min, filter, evaporate the filtrate to dryness, add 1mL of ethanol to dissolve the residue to obtain the test solution.

[0115] According to the thin-layer chromatography method (General Rule 0502), take 5 μL of the test solution and spot it on the same silica gel G thin-layer plate. Use cyclohexane-ethyl acetate (4:1) as the developing solvent, develop, remove, air dry, and examine under ultraviolet light at 365 nm.

[0116] The results are as follows Figure 2 As shown, the extraction effect of the test sample solution is the best when methanol is used as the extraction solvent. Therefore, methanol was selected as the extraction solvent for this experiment.

[0117] 2. Investigation of the developing solvent

[0118] According to the thin-layer chromatography method (General Rule 0502), 5 μL each of the following four solutions were applied to the same silica gel G thin-layer plate: Angelica sinensis reference solution, Ligusticum chuanxiong reference solution, negative control solution lacking Angelica sinensis and Ligusticum chuanxiong, and test solution. The plate was developed using A-cyclohexane-ethyl acetate (4:1), B-cyclohexane-ethyl acetate (9:1), and C-n-hexane-ethyl acetate-glacial acetic acid (30:10:1), respectively. The plate was then removed, dried, and examined under ultraviolet light at 365 nm.

[0119] The results are as follows Figure 3As shown, when the developing solvent is hexane-ethyl acetate-glacial acetic acid (30:10:1), the main spot of the test sample solution is clearly visible and has the best separation at the corresponding position of the spot of the reference drug. Therefore, hexane-ethyl acetate-glacial acetic acid (30:10:1) is selected as the optimal developing solvent.

[0120] 3. Examination of thin-layer plates

[0121] According to the thin-layer chromatography method (General Rule 0502), 5 μL each of the above-mentioned Angelica sinensis reference solution, Ligusticum chuanxiong reference solution, negative control solution lacking Angelica sinensis and Ligusticum chuanxiong, and test sample solution were spotted onto silica gel GF. 254 Thin-layer plates and silica gel G thin-layer plates were developed using hexane-ethyl acetate-glacial acetic acid (30:10:1) as the developing solvent. After development, the plates were removed, dried, and examined under ultraviolet light at 365 nm and 254 nm, respectively.

[0122] The results are as follows Figure 4 As shown, compared to the silicone G plate, the silicone GF plate... 254 The spots are clearer on thin-layer plates, so silicone GF was chosen. 254 The thin-layer plate used in this experiment was the silica gel GF. 254 Thin-layer plate.

[0123] III. Durability Test

[0124] 1. Investigation of thin-layer boards from different manufacturers

[0125] The above-mentioned Angelica sinensis reference solution, Ligusticum chuanxiong reference solution, negative control solution lacking Angelica sinensis and Ligusticum chuanxiong, and test sample solution were tested to investigate the effects of different manufacturers' (Yantai Donghai Thin Plate Co., Ltd. and Qingdao Haiyang Chemical Co., Ltd.) silica gel GF 254 Durability of thin-layer boards.

[0126] The results showed that characteristic spots could be detected using thin-layer plates from different manufacturers, and the test results were stable; however, the thin-layer plates from Qingdao Ocean Chemical Co., Ltd. performed better. Figure 5 ).

[0127] 2. Investigation under different temperatures and humidity levels

[0128] The effects of temperature and humidity on the experimental results were investigated in laboratory (26.5℃, 41% RH) and refrigerator (5℃, 70% RH) environments for the above-mentioned Angelica sinensis reference solution, Ligusticum chuanxiong reference solution, negative control solution lacking Angelica sinensis and Ligusticum chuanxiong, and test solution.

[0129] The results are as follows Figure 6As shown, under different temperature and humidity conditions, there was no significant change in the main spot of the control solution and the main spot of the test solution, and the Rf value varied in the range of 0.4 to 0.8, which meets the system adaptability requirements, indicating that this identification method has good robustness.

[0130] Example 2: Identification of Moutan Cortex in Hair Growth and Fat Removal Tablets

[0131] I. Identification Methods

[0132] 1. Preparation of test solution: Take 3g of fine powder from three batches of hair growth tablets (batch numbers: 230104, 230507, 230701) produced by Shanxi Renyuantang Pharmaceutical Co., Ltd., place them in an Erlenmeyer flask, add 20mL of methanol, stopper tightly, shake for 10min, filter, evaporate the filtrate to dryness, and dissolve the residue in 2mL of acetone to obtain the test solution.

[0133] 2. Preparation of negative control solution lacking peony bark: According to the original prescription of the hair growth tablets, weigh 0.2 times the amount of medicinal material lacking peony bark, and prepare a negative sample lacking peony bark according to the above preparation method; place 3g of negative sample lacking peony bark in an Erlenmeyer flask, add 20mL of methanol, seal tightly, shake, filter, evaporate the filtrate to dryness, dissolve the residue in acetone to obtain the negative sample solution lacking peony bark;

[0134] 3. Preparation of peony bark reference material solution: Take 1g of peony bark reference material, grind it into fine powder, place it in an Erlenmeyer flask, add 20mL of methanol, seal tightly, shake for 10min, filter, evaporate the filtrate to dryness, add 2mL of acetone to dissolve the residue to obtain peony bark reference material solution.

[0135] 4. Preparation of paeonol reference standard: Accurately weigh 2 mg of paeonol reference standard, add an appropriate amount of acetone to dilute to 1 mL in a volumetric flask, and the solution is ready.

[0136] 5. Thin-layer chromatography test: Take 10 μL each of the prepared paeonol reference solution, peony bark reference material solution, negative control solution lacking peony bark, and test sample solution, and spot them separately on the same silica gel G thin-layer plate. Use n-hexane-ethyl acetate-glacial acetic acid (4:1:0.1) as the developing solvent, develop, remove, air dry, spray with 2% vanillin sulfuric acid ethanol solution, and heat at 105℃ until the spots are clearly visible.

[0137] The results are as follows Figure 7 As shown, in the chromatograms of the three batches of test samples, spots of the same color were displayed at the corresponding positions as in the chromatograms of the reference standard and the reference medicinal material, and there was no interference from the negative control.

[0138] II. Investigation of the preparation method of the test sample

[0139] Investigation of extraction solvents: 3g of the degreased hair growth tablets fine powder was placed in an Erlenmeyer flask, and methanol, ethanol and ethyl acetate were used as extraction solvents respectively. 20mL of each solvent was added, the flask was sealed, shaken for 10min, filtered, the filtrate was evaporated to dryness, and 2mL of acetone was added to the residue to dissolve it, which yielded the product.

[0140] According to the thin-layer chromatography method (General Rule 0502), 10 μL of the above solution and paeonol reference solution were respectively spotted onto the same silica gel G thin-layer plate. The plate was developed using n-hexane-ethyl acetate-glacial acetic acid (4:1:0.1) as the developing solvent. The plate was then removed, dried, sprayed with 2% vanillin sulfuric acid ethanol solution, and heated at 105℃ until the spots were clearly visible.

[0141] The results are as follows Figure 8 As shown, when methanol is used as the extraction solvent, the test sample chromatogram shows spots of the same color at the corresponding positions as the reference sample. Therefore, methanol was selected as the extraction solvent for this test.

[0142] III. Durability Test

[0143] The four solutions prepared above—the test solution, the reference solution, the negative control solution lacking peony bark, and the peony bark reference medicinal material solution—were used to investigate the effects of silica gel G thin-layer plates from different manufacturers (Qingdao Hailang Desiccant Co., Ltd. and Qingdao Haiyang Chemical Plant Co., Ltd.) and different temperatures and humidity levels (laboratory environment (25.6℃, 41% RH) and refrigerator environment (5℃, 71% RH)) on the test results.

[0144] The results are as follows Figure 9 As shown in the left figure, the characteristic spots were detected by the thin-layer plate of Qingdao Hailang Desiccant Co., Ltd., and the test results were stable. In the middle and right figures, under different temperature and humidity conditions, the Rf values ​​of the corresponding spots of the test sample chromatogram, the reference standard and the reference medicinal material solution varied in the range of 0.4 to 0.8, which met the system adaptability requirements, indicating that this identification method has good robustness.

[0145] Example 3: Identification of Sophora flavescens in Hair Growth and Fat Removal Tablets

[0146] I. Identification Methods

[0147] 1. Preparation of test solution: Take 5g of powder from three batches of hair growth tablets (batch numbers: 230104, 230507, 230701) produced by Shanxi Renyuantang Pharmaceutical Co., Ltd., add 2mL of concentrated ammonia solution and 25mL of chloroform, seal tightly, sonicate in an ice bath for 30min, filter, evaporate the filtrate to dryness, and dissolve the residue in 2mL of chloroform to obtain the test solution.

[0148] 2. Preparation of negative control solution lacking Sophora flavescens: According to the original prescription of the hair growth tablets, weigh 0.2 times the amount of medicinal material lacking Sophora flavescens. Prepare a negative sample lacking Sophora flavescens according to the above method. Place 5g of negative sample lacking Sophora flavescens in an Erlenmeyer flask, add 2mL of concentrated ammonia solution and 25mL of chloroform, seal tightly, sonicate in an ice bath for 30min, filter, evaporate the filtrate to dryness, add 2mL of chloroform to dissolve the residue, and obtain a negative control solution lacking Sophora flavescens.

[0149] 3. Preparation of matrine reference solution: Take 2 mg of matrine reference standard and add acetone to dilute to 10 mL in a volumetric flask to obtain matrine reference solution;

[0150] 4. Thin-layer chromatography test: Take 3 μL of each of the three solutions, namely matrine reference solution, negative control solution lacking matrine and test solution, and spot them on silica gel G thin-layer plate. Use chloroform-methanol (5:0.8) as the developing solvent. After the plate is dried, spray it with potassium bismuth iodide test solution and examine it under sunlight.

[0151] The results are as follows Figure 10 As shown, in the chromatograms of the three batches of test samples, the same orange spots were observed at the corresponding positions as in the chromatograms of the reference standard and the reference medicinal material, while the negative control showed no spots.

[0152] II. Investigation of the preparation method of the test sample

[0153] Investigation of preparation methods: Preparation method A: Take 5g of fine powder from degreasing hair growth tablets, add 2mL of concentrated ammonia solution and 25mL of chloroform, seal tightly, sonicate in an ice bath for 30min, filter, evaporate the filtrate to dryness, dissolve the residue in 2mL of chloroform, and use as test solution A. Preparation method B: Take 5g of fine powder from degreasing hair growth tablets, add 25mL of ethanol, heat under reflux for 1h, filter, concentrate the filtrate to 2mL to dissolve, and use as test solution B.

[0154] According to the thin-layer chromatography method (General Rule 0502), the above solution and matrine reference solution were spotted onto silica gel G thin-layer plates treated with 2% sodium hydroxide solution. The plates were developed using chloroform-methanol (5:0.8) as the developing solvent. After the plates were dried, they were sprayed with potassium bismuth iodide test solution and examined under sunlight.

[0155] The results are as follows Figure 11 As shown, in the chromatogram of the test sample, the same orange spots are displayed at the corresponding positions as in the chromatogram of the reference sample. However, the spots of test sample solution A are more clearly visible. Therefore, method 1 is selected as the preparation method of the test sample in this experiment.

[0156] III. Examining the System Conditions

[0157] 1. Investigation of Thin-Layer Plate Types

[0158] According to the thin-layer chromatography method (General Rule 0502), the reference solution, the negative control solution lacking Sophora flavescens, and the test solution from the identification method in Example 3 (I) were spotted onto silica gel G thin-layer plates produced by Qingdao Marine Chemical Plant, silica gel G thin-layer plates prepared with 2% sodium hydroxide, and GF thin-layer plates, respectively. 254 On the thin-layer plate, chloroform-methanol (5:0.8) was used as the developing solvent. The plate was then removed, dried, sprayed with potassium bismuth iodide solution, and examined under sunlight.

[0159] The results are as follows Figure 12 As shown, the main chromatographic spot on the silica gel G thin-layer plate has good separation and is clearly visible, so the silica gel G thin-layer plate was selected for this experiment.

[0160] 2. Investigation of sample size

[0161] According to the thin-layer chromatography method (General Rule 0502), 1 μL, 3 μL, 5 μL and 7 μL of the test sample A solution under the identification method of Example 3 (I) were respectively spotted onto the same silica gel G thin-layer plate. The plate was developed with chloroform-methanol (5:0.8) as the developing solvent, removed, dried, sprayed with potassium bismuth iodide test solution, and examined under sunlight.

[0162] The results are as follows Figure 13 As shown, the spots of all four sample sizes are clearly visible in the chromatogram of the test sample, and the final sample size was determined to be 3 μL.

[0163] IV. Durability Test

[0164] The corresponding test solution, reference solution and negative control solution were prepared according to the preparation method of the solution under the identification method in Example 3 (I). The effects of silica gel G thin-layer plates from different manufacturers (Qingdao Hailang Desiccant Co., Ltd. and Qingdao Haiyang Chemical Plant Co., Ltd.) and different temperatures and humidity (laboratory environment (26℃, 43% RH) and refrigerator environment (5℃, 71% RH)) on the test results were investigated.

[0165] The results are as follows Figure 14 As shown in the left figure, the characteristic spots of the thin-layer plate from Qingdao Hailang Desiccant Co., Ltd. are clearly visible, indicating good specificity and stable test results. In the middle and right figures, under different temperature and humidity conditions, the Rf values ​​of the corresponding spots of the test sample and the reference sample vary in the range of 0.4 to 0.8, which meets the system adaptability requirements, indicating that this identification method has good robustness.

[0166] Example 4: Identification of Processed Polygonum multiflorum Medicinal Material

[0167] I. Identification Methods

[0168] 1. Preparation of test solution: Take 5g of fine powder from three batches of hair growth tablets (batch numbers: 230104, 230507, 230701) produced by Shanxi Renyuantang Pharmaceutical Co., Ltd., add 20mL of ethanol and reflux for 1h, filter, and concentrate the filtrate to 5mL to obtain the test solution.

[0169] 2. Preparation of negative control solution lacking processed Polygonum multiflorum: According to the original prescription of the hair growth tablets, weigh 0.2 times the amount of medicinal material lacking processed Polygonum multiflorum, and prepare a negative sample lacking processed Polygonum multiflorum according to the above preparation method; place 5g of negative sample lacking processed Polygonum multiflorum in an Erlenmeyer flask, add 20mL of ethanol, reflux, filter, concentrate the filtrate to obtain negative control solution lacking processed Polygonum multiflorum;

[0170] 3. Preparation of prepared Polygonum multiflorum reference material solution: Take 1g of prepared Polygonum multiflorum reference material, add 20mL of ethanol and reflux for 1h, filter, concentrate the filtrate to 5mL to obtain prepared Polygonum multiflorum reference material solution;

[0171] 4. Thin-layer chromatography test: Take 2 μL of each of the above three solutions: Polygonum multiflorum reference material solution, negative control solution without processed Polygonum multiflorum, and test sample solution, and spot them separately on the same silica gel G thin-layer plate. First, use chloroform-methanol (7:3) as the first developing solvent and develop to about 3.5 cm. Remove and air dry. Then, use chloroform-methanol (20:1) as the developing solvent and develop to about 7 cm. Remove, air dry, and examine under a UV lamp at 365 nm.

[0172] The results are as follows Figure 15 As shown, in the chromatograms of the three batches of test samples, fluorescent spots of the same color were displayed at the corresponding positions as in the chromatogram of the reference medicinal material, and there was no interference from the negative control.

[0173] II. Durability Test

[0174] The corresponding test solution, control herbal solution, and negative sample solution for Polygonum multiflorum were prepared according to the preparation method of the solution under the identification method in Example 4 (I). The effects of silica gel G thin-layer plates from different manufacturers (Qingdao Hailang Desiccant Co., Ltd. and Qingdao Haiyang Chemical Plant Co., Ltd.) and different temperatures and humidity (laboratory environment (26℃, 47% RH) and refrigerator environment (5℃, 68% RH)) on the test results were investigated.

[0175] The results are as follows Figure 16 As shown in the left figure, the characteristic spots were detected by the thin-layer plate of Qingdao Hailang Desiccant Co., Ltd., and the test results were stable. In the middle and right figures, under different temperature and humidity conditions, the Rf values ​​of the corresponding spots of the test sample chromatogram and the control solution varied in the range of 0.4 to 0.8, which met the system adaptability requirements, indicating that this identification method has good robustness.

[0176] In summary, the thin-layer chromatography method used in this invention can quickly and accurately identify the various medicinal materials in the hair growth and degreasing tablets, with a high accuracy rate. This is beneficial for the quality control of the hair growth and degreasing tablets and has important application value in ensuring quality and clinical efficacy.

[0177] The above content is only for illustrating the technical concept of the present invention and should not be construed as limiting the scope of protection of the present invention. Any modifications made to the technical solution based on the technical concept proposed in this invention shall fall within the scope of protection of the claims of this invention.

Claims

1. A quality testing method for degreasing and hair growth tablets, characterized in that, The detection is carried out by at least one of steps 1) to 4): 1) Thin-layer identification of angelica and ligusticum medicinal materials Preparation of test solution: Take the fine powder of Zhisu Shengfa Tablets, add methanol, and then perform ultrasonic treatment after standing. Filter, evaporate the filtrate, and dissolve the residue in ethanol to obtain the test solution; Preparation of negative control solution without angelica and ligusticum: Prepare a negative sample without angelica and ligusticum according to the prescription and preparation method of Zhisu Shengfa Tablets, and prepare the negative control solution without angelica and ligusticum according to the preparation method of test solution; Preparation of angelica and ligusticum control medicinal material solutions: Take angelica and ligusticum control medicinal materials, respectively, and prepare the angelica and ligusticum control medicinal material solutions according to the preparation method of test solution; Take the test solution, the negative control solution without angelica and ligusticum, the angelica control medicinal material solution, and the ligusticum control medicinal material solution, respectively, and apply them to the same silica gel thin-layer plate. Use n-hexane-ethyl acetate-glacial acetic acid as the developing agent, develop, take out, air dry, and observe under ultraviolet light. In the test chromatogram, the same color spots appear at the positions corresponding to the control medicinal material chromatogram; 2) Thin-layer identification of cortex moutan medicinal materials Preparation of test solution: Take the fine powder of Zhisu Shengfa Tablets, add methanol, and then perform ultrasonic treatment after standing. Filter, evaporate the filtrate, and dissolve the residue in ethanol to obtain the test solution; Preparation of negative control solution without cortex moutan: Prepare a negative sample without cortex moutan according to the prescription and preparation method of Zhisu Shengfa Tablets, and prepare the negative control solution without cortex moutan according to the preparation method of test solution; Preparation of cortex moutan control medicinal material solution: Take cortex moutan control medicinal material, and prepare the cortex moutan control medicinal material solution according to the preparation method of test solution; Preparation of paeonol control solution: Take the paeonol control, add acetone to dissolve, and obtain the paeonol control solution; Take the test solution, the negative control solution without cortex moutan, the cortex moutan control medicinal material solution, and the paeonol control solution, respectively, and apply them to the same silica gel thin-layer plate. Use n-hexane-ethyl acetate-glacial acetic acid as the developing agent, spray with vanillin sulfuric acid ethanol solution, and heat until the spots develop clearly. In the test chromatogram, the same color spots appear at the positions corresponding to the control solution and the control medicinal material chromatogram; 3) Identification of medicinal materials of radix sophorae flavescentis Preparation of test solution: Take the fine powder of Zhisu Shengfa Tablets, add concentrated ammonia solution and chloroform, perform ultrasonic treatment in an ice bath, filter, evaporate the filtrate, and dissolve the residue in chloroform to obtain the test solution; Preparation of negative control solution without radix sophorae flavescentis: Prepare a negative sample without radix sophorae flavescentis according to the prescription and preparation method of Zhisu Shengfa Tablets, and prepare the negative control solution without radix sophorae flavescentis according to the preparation method of test solution; Preparation of sophoramine control solution: Take the sophoramine control, add acetone to dissolve, and obtain the sophoramine control solution; Take the test solution, the negative control solution without radix sophorae flavescentis, and the sophoramine control solution, respectively, and apply them to the same silica gel thin-layer plate. Use chloroform-methanol as the developing agent, take out, air dry, spray with bismuth potassium iodide solution, and observe under daylight. In the test chromatogram, the same orange spots appear at the positions corresponding to the control solution; 4) Identification of medicinal materials of radix polygoni multiflori Preparation of test solution: Take the fine powder of Zhisu Shengfa Tablets, add ethanol, perform reflux, filter, and concentrate the filtrate to obtain the test solution; Preparation of negative control solution without Radix Polygoni Multiflori: the negative sample without Radix Polygoni Multiflori was prepared according to the prescription and preparation method of Zhi Zhi Shengfa Tablets, and the negative control solution without Radix Polygoni Multiflori was prepared according to the preparation method of test solution; Preparation of Radix Polygoni Multiflori control solution: Radix Polygoni Multiflori was taken as the control solution according to the preparation method of test solution; The test solution, the negative control solution without Radix Polygoni Multiflori and the Radix Polygoni Multiflori control solution were taken and spotted on the same silica gel thin layer plate, chloroform-methanol was used as the developing agent, and then the plate was taken out, dried and observed under ultraviolet light; the same fluorescent spots were observed in the test solution and the control solution.

2. The method for detecting the quality of the anti-hair loss tablet according to claim 1, wherein, In step 1), the use amount ratio of Zhi Zhi Shengfa Tablets fine powder, the negative sample without Angelica sinensis and Ligusticum chuanxiong, Angelica sinensis control solution and Ligusticum chuanxiong control solution to methanol was 5g:25mL, 5g:25mL, 1g:25mL and 1g:25mL respectively; the standing time was 30min, the ultrasonic treatment time was 10min, and the volume of ethanol used to dissolve the residue was 1mL.

3. The method for quality detection of the anti-hair loss tablet according to claim 1, characterized in that, In step 1), the spotting volume was 5 μL and the thin layer plates used were silica gel GF 254 Thin layer plates; developing solvent was a mixture of n-hexane, ethyl acetate and glacial acetic acid in the ratio 30:10:1 by volume.

4. The method for detecting the quality of the anti-hair loss tablet according to claim 1, wherein, In step 2), the use amount ratio of Zhi Zhi Shengfa Tablets fine powder, the negative sample without Radix Moutan and Radix Moutan control solution to methanol was 3g:20mL, 3g:20mL and 1g:10mL respectively, the use amount ratio of paeonol control to acetone was 5mg:10mL, and the oscillation time was 10min.

5. The method for quality detection of the anti-hair loss tablet according to claim 1, characterized in that, In step 2), the spotting amount was 10μL; the thin layer plate used was silica gel G thin layer plate; the developing agent was a mixed solution of n-hexane, ethyl acetate and glacial acetic acid with a volume ratio of 4:1:0.1; the concentration of vanillin sulfuric acid ethanol was 2% vanillin sulfuric acid ethanol solution, and the temperature for color development was 105℃.

6. The method for detecting the quality of the anti-hair loss tablet according to claim 1, wherein, In step 3), the sampling amount of Zhi Zhi Shengfa Tablets fine powder was 5g, the added volumes of concentrated ammonia solution and chloroform were 2mL and 25mL respectively, and the volume of chloroform added to the residue was 2mL; in the preparation of the negative control solution without Radix Sophorae Flavescentis, the sampling amount of the negative sample without Radix Sophorae Flavescentis was 5g; in the preparation of the Radix Sophorae Flavescentis control solution, the use amount ratio of Radix Sophorae Flavescentis control to acetone was 2mg:10mL; the ice bath ultrasonic treatment time was 30min.

7. The method for detecting the quality of the anti-hair loss tablet according to claim 1, wherein, In step 3), the spotting amount was 3μL; the thin layer plate used was silica gel G thin layer plate; the developing agent was a mixed solution of chloroform and methanol with a volume ratio of 5:0.

8.

8. The method for detecting the quality of the anti-hair loss tablet according to claim 1, wherein, In step 4), the use amount ratio of Zhi Zhi Shengfa Tablets fine powder, the negative sample without Radix Polygoni Multiflori and Radix Polygoni Multiflori control to ethanol was 5g:20mL, 5g:20mL and 1g:20mL respectively; the reflux time was 60min; the filtrate was concentrated to 1mL.

9. The method for quality detection of the anti-hair loss tablet according to claim 1, characterized in that, In step 4), the spotting amount was 2μL; the thin layer plate used was silica gel G thin layer plate; the developing agent was chloroform-methanol, and the volume ratio of chloroform to methanol was 7:3 in the first developing, and the developing distance was 3.5cm; the volume ratio of chloroform to methanol was 20:1 in the second developing, and the developing distance was 7cm.

10. The method for quality detection of the anti-hair loss tablet according to claim 1, characterized in that, In step 1), the observation was carried out under 365nm and 254nm ultraviolet light; in step 4), the observation was carried out under 365nm ultraviolet light.

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