Quality control method of spleen and stomach soothing pill

Abstract

The invention provides a quality control method of spleen and stomach soothing pills, which specifically comprises the following steps: respectively preparing a test solution and a reference medicinal material solution, and identifying by using a thin layer chromatography. The method overcomes the technical problem that the method in the prior art cannot meet the quality control of the spleen and stomach soothing pills, can simply and quickly complete the quality identification of the spleen and stomach soothing pills, and ensures the product quality and curative effect. The method disclosed by the invention is stable and good in reproducibility, and is applicable to conventional samples and medium-and-long-term reserved samples.

Description

Technical Field

[0001] The invention relates to a quality control method for a traditional Chinese medicine composition, in particular to a quality control method for a Piweishu pill. Background Art

[0002] Piweishu Pills are a traditional Chinese medicine combination preparation included in the 2020 edition of the Pharmacopoeia of the People's Republic of China. Its functions and indications are: soothing the liver and regulating qi, strengthening the spleen and harmonizing the stomach, and eliminating accumulation and digesting food; it is used to treat indigestion, loss of appetite, noisy stomach, abdominal distension and intestinal rumbling, nausea and vomiting, loose stools, distension and pain in the ribs, irritability, dizziness, fatigue, insomnia and nightmares; it is effective for patients with the above symptoms in chronic gastritis, chronic hepatitis, and early cirrhosis.

[0003] The prescription composition of Piweishu Pills is as follows: 50g of processed turtle shell, 50g of roasted astragalus, 50g of dried orange peel, 50g of immature bitter orange, 50g of white peony root, 50g of stir-fried white atractylodes with bran, 50g of vinegar-cooked cyperus, 50g of tsaoko, 50g of stir-fried black plum, 50g of chuanxiong, 50g of charred betel nut, 50g of magnolia bark. The above twelve Chinese medicines are crushed into fine powder, sieved, mixed, and 120-140g of refined honey is added to every 100g of powder to make large honey pills. The finished product of this product is large brown honey pills with a slight fragrance and a bitter and spicy taste.

[0004] The Chinese Pharmacopoeia clearly stipulates three identification items for this product, among which item (3) is: Take 2 pills of this product, cut them into pieces, take 12g, add 30ml of n-hexane, ultrasonically treat for 15min, filter, and concentrate the filtrate to about 2ml as the test solution. Take 0.5g of Atractylodes macrocephala control medicinal material, add 10ml of n-hexane, and prepare the control medicinal material solution in the same way. According to the thin layer chromatography method (General Rule 0502), take 10μl of each of the two newly prepared solutions and spot them on the same silica gel G thin layer plate, use petroleum ether (60-90℃)-ethyl acetate (10:0.2) as the developing solvent, develop, take out, dry, spray with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. In the chromatogram of the test product, spots of the same color appear at the corresponding positions of the chromatogram of the control medicinal material.

[0005] The inventors found in actual research work that, according to the above pharmacopoeia method, the test sample chromatogram failed to show spots at the corresponding positions of the control medicinal material chromatogram, and the quality of the product could not be effectively controlled. There is an urgent need to develop an analytical method that can effectively achieve quality control of Piwei Shu Wan in this field to ensure the quality of the product and the effectiveness of patient treatment. Summary of the invention

[0006] An object of one aspect of the present invention is to provide a quality control method for Piweishu Pills, comprising the following steps:

[0007] (1) Preparation of test solution: Take an appropriate amount of Piweishu pills, cut them into pieces, add an appropriate amount of water to dissolve them, remove the liquid, dry the residue, take the dried residue, add an appropriate amount of n-hexane, ultrasonically treat, filter, and concentrate the filtrate to obtain the test solution;

[0008] (2) Preparation of reference medicinal material solution: Take an appropriate amount of Atractylodes macrocephala reference medicinal material, add an appropriate amount of n-hexane, perform ultrasonic treatment, filter, and concentrate the filtrate to obtain the solution;

[0009] (3) Thin layer chromatography identification: Take appropriate amounts of the above two solutions and spot them on the same thin layer chromatography plate, develop them with an appropriate developer, let them dry, spray them with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. In the chromatogram of the test sample, spots of the same color should appear at the corresponding positions in the chromatogram of the control medicinal material.

[0010] In the preferred technical solution of the present invention, the volume weight ratio (V / W) of water to Piweishuwan in step (1) is 1-15:1, preferably 3-10:1, and more preferably 4-6:1.

[0011] In a preferred technical solution of the present invention, the method for removing the liquid in step (1) is selected from centrifugation or filtration.

[0012] In the preferred technical scheme of the present invention, the method for drying the medicinal residue in step (1) is high-temperature drying, the drying temperature is 30°C-100°C, preferably 50°C-80°C, more preferably 55°C-70°C, and the drying time is 1h-6h, preferably 2h-4h.

[0013] In the preferred technical solution of the present invention, the volume weight ratio (V / W) of n-hexane to the medicinal residue in step (1) is 2-20:1, preferably 2-10:1, and more preferably 2-5:1.

[0014] In the preferred technical solution of the present invention, the volume weight ratio (V / W) of n-hexane to the reference medicinal material in step (2) is 5-30:1, preferably 10-25:1, and more preferably 15-20:1.

[0015] In the preferred technical solution of the present invention, the time of ultrasonic treatment in step (1) and step (2) is 5 min-60 min, preferably 10 min-30 min, and more preferably 15 min-20 min, respectively.

[0016] In the preferred technical solution of the present invention, the aspirated amount of the two solutions in step (3) is 5 μl-25 μl, preferably 10 μl-20 μl.

[0017] In a preferred technical solution of the present invention, the thin layer chromatography plate in step (3) is selected from a silica gel thin layer chromatography plate, an alumina thin layer chromatography plate or a polyethylene thin layer chromatography plate.

[0018] In the preferred technical scheme of the present invention, the developing agent in step (3) is petroleum ether (60-90° C.)-ethyl acetate, preferably the ratio of petroleum ether:ethyl acetate is 1-100:1, preferably 30-70:1, and more preferably 40-60:1.

[0019] In the preferred technical scheme of the present invention, the prescription composition of the above-mentioned Piwei Shu Wan is: 50g of turtle shell (processed), 50g of roasted Astragalus, 50g of dried tangerine peel, 50g of Citrus aurantium, 50g of white peony root, 50g of stir-fried Atractylodes macrocephala with bran, 50g of Cyperus rotundus with vinegar, 50g of Tsaoko, 50g of black plum (fried), 50g of Ligusticum chuanxiong, 50g of charred Areca catechu, and 50g of Magnolia officinalis. The above twelve Chinese medicines are crushed into fine powder, sieved, and mixed. 120-140g of refined honey is added to every 100g of powder to make large honey pills.

[0020] Another object of the present invention is to provide an application of the above-mentioned quality control method in the quality control of Piweishu Pills.

[0021] Another object of the present invention is to provide the application of the above-mentioned quality control method in thin layer chromatography identification of Piweishu Pills.

[0022] Another object of the present invention is to provide a quality control method for Piweishu Pills, comprising the following steps:

[0023] (1) Preparation of the test solution: Take an appropriate amount of Piweishu Pills, chop them into pieces, add an appropriate amount of methanol and heat to reflux, cool, extract with an appropriate amount of n-hexane by shaking, combine the n-hexane extracts, evaporate the solvent, and dissolve the residue in a small amount of n-hexane to obtain the test solution;

[0024] (2) Preparation of reference medicinal material solution: Take an appropriate amount of Atractylodes macrocephala reference medicinal material, add an appropriate amount of n-hexane, perform ultrasonic treatment, filter, and concentrate the filtrate to obtain the solution;

[0025] (3) Thin layer chromatography identification: Take appropriate amounts of the two solutions mentioned above, spot them on the same thin layer chromatography plate, develop them with an appropriate developer, let them dry, spray them with vanillin sulfuric acid solution, and heat until the spots are clearly colored. In the chromatogram of the test sample, spots of the same color should appear at the corresponding positions in the chromatogram of the control medicinal material.

[0026] In the preferred technical solution of the present invention, the volume weight ratio (V / W) of methanol to Piweishu pills in step (1) is 1-15:1, preferably 3-10:1, and more preferably 3-5:1.

[0027] In the preferred technical solution of the present invention, the heating reflux temperature in step (1) is 60°C-90°C, preferably 65°C-85°C, and more preferably 70°C-80°C.

[0028] In the preferred technical solution of the present invention, the heating reflux time in step (1) is 1 h-4 h, preferably 1 h-3 h, and more preferably 1.5 h-2.5 h.

[0029] In the preferred technical solution of the present invention, in step (1), the extraction is performed by shaking with n-hexane for 1-5 times, preferably 2-4 times, and the volume ratio (V / V) of the total amount of n-hexane used for extraction to methanol is 0.5-2:1.

[0030] In the preferred technical solution of the present invention, the volume weight ratio (V / W) of n-hexane to the reference medicinal material in step (2) is 5-30:1, preferably 10-25:1, and more preferably 15-20:1.

[0031] In the preferred technical solution of the present invention, the time of ultrasonic treatment in step (2) is 5 min-60 min, preferably 10 min-30 min, more preferably 15 min-20 min.

[0032] In the preferred technical solution of the present invention, the aspirated amount of the two solutions in step (3) is 5 μl-25 μl, preferably 10 μl-20 μl.

[0033] In a preferred technical solution of the present invention, the thin layer chromatography plate in step (3) is selected from a silica gel thin layer chromatography plate, an alumina thin layer chromatography plate or a polyethylene thin layer chromatography plate.

[0034] In the preferred technical scheme of the present invention, the developing agent in step (3) is petroleum ether (60-90° C.)-ethyl acetate, preferably the ratio of petroleum ether:ethyl acetate is 1-100:1, preferably 30-70:1, and more preferably 40-60:1.

[0035] In the preferred technical scheme of the present invention, the prescription composition of the above-mentioned Piwei Shu Wan is: 50g of turtle shell (processed), 50g of roasted Astragalus, 50g of dried tangerine peel, 50g of Citrus aurantium, 50g of white peony root, 50g of stir-fried Atractylodes macrocephala with bran, 50g of Cyperus rotundus with vinegar, 50g of Tsaoko, 50g of black plum (fried), 50g of Ligusticum chuanxiong, 50g of charred Areca catechu, and 50g of Magnolia officinalis. The above twelve Chinese medicines are crushed into fine powder, sieved, and mixed. 120-140g of refined honey is added to every 100g of powder to make large honey pills.

[0036] Another object of the present invention is to provide an application of the above-mentioned quality control method in the quality control of Piweishu Pills.

[0037] Another object of the present invention is to provide the application of the above-mentioned quality control method in thin layer chromatography identification of Piweishu Pills.

[0038] Unless otherwise specified, when the present invention relates to the percentage between liquids, the percentage is volume / volume percentage; when the present invention relates to the percentage between liquids and solids, the percentage is volume / weight percentage; when the present invention relates to the percentage between solids and liquids, the percentage is weight / volume percentage; the rest are weight / weight percentages.

[0039] Compared with the prior art, the present invention has the following beneficial effects: the present invention overcomes the technical difficulty that the method of the Chinese Pharmacopoeia cannot meet the quality control of Piweishu Pills for a long time, and the method of the present invention can simply and quickly complete the quality identification of Piweishu Pills, ensuring the product quality and efficacy. In addition, the method of the present invention is stable and reproducible, and is applicable to both conventional samples and medium- and long-term retained samples. DETAILED DESCRIPTION

[0040] To make the purpose, technical solution and advantages of the present invention more clear, the embodiments of the present invention will be described in detail below. It should be noted that the embodiments of the present invention and the features in the embodiments can be combined with each other arbitrarily without conflict.

[0041] Comparative Example 1 Identification of Piweishu Pills

[0042] The test was carried out according to the pharmacopoeia method: 2 pills of this product were cut into pieces, 12g was taken, 30ml of n-hexane was added, ultrasonic treatment was performed for 15min, and the filtrate was concentrated to about 2ml as the test solution. Another 0.5g of Atractylodes macrocephala control medicinal material was taken, 10ml of n-hexane was added, and the control medicinal material solution was prepared in the same way. According to the thin layer chromatography test, 10μl of each of the two newly prepared solutions was taken and spotted on the same silica gel G thin layer plate, and petroleum ether (60-90℃)-ethyl acetate (10:0.2) was used as the developing agent. The plate was developed, taken out, dried, sprayed with 5% vanillin sulfuric acid solution, and heated until the spots were clearly colored. The results showed that the control medicinal material chromatogram showed pink spots, and the test product chromatogram did not show color at the corresponding position of the control medicinal material chromatogram. This method could not achieve quality control.

[0043] Comparative Example 2 Identification of Piweishu Pills

[0044] Take 2 pills of this product, cut them into pieces, take 12g, add 60ml of n-hexane, ultrasonically treat for 15min, filter, and concentrate the filtrate to about 2ml as the test solution. Take another 0.5g of Atractylodes macrocephala control medicinal material, add 10ml of n-hexane, and prepare the control medicinal material solution in the same way. According to the thin layer chromatography test, take 10μl of each of the two newly prepared solutions, and spot them on the same silica gel G thin layer plate, use petroleum ether (60-90℃)-ethyl acetate (10:0.2) as the developing agent, develop, take out, dry, spray with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. The results show that the control medicinal material chromatogram shows pink spots, and the test product chromatogram does not show color at the corresponding position of the control medicinal material chromatogram. This method cannot achieve quality control.

[0045] Comparative Example 3 Identification of Piweishu Pills

[0046] Take 2 pills of this product, cut them into pieces, take 12g, add 60ml of n-hexane, ultrasonically treat for 45min, filter, and concentrate the filtrate to about 2ml as the test solution. Take another 0.5g of Atractylodes macrocephala control medicinal material, add 10ml of n-hexane, and prepare the control medicinal material solution in the same way. According to the thin layer chromatography test, take 10μl of each of the two newly prepared solutions, and spot them on the same silica gel G thin layer plate, use petroleum ether (60-90℃)-ethyl acetate (10:0.2) as the developing agent, develop, take out, dry, spray with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. The results show that the control medicinal material chromatogram shows pink spots, and the test product chromatogram does not show color at the corresponding position of the control medicinal material chromatogram. This method cannot achieve quality control.

[0047] Comparative Example 4 Identification of Piweishu Pills

[0048] Take 2 pills of this product, cut them into pieces, take 12g, add 30ml of methanol, ultrasonically treat for 15min, filter, and concentrate the filtrate to about 2ml as the test solution. Take another 0.5g of Atractylodes macrocephala control medicinal material, add 10ml of n-hexane, and prepare the control medicinal material solution in the same way. According to the thin layer chromatography test, take 10μl of each of the two newly prepared solutions, and spot them on the same silica gel G thin layer plate, use petroleum ether (60-90℃)-ethyl acetate (10:0.2) as the developing agent, develop, take out, dry, spray with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. The results show that the control medicinal material chromatogram shows pink spots, and the test product chromatogram only shows very weakly at the corresponding position of the control medicinal material chromatogram. This method cannot achieve quality control.

[0049] Comparative Example 5 Identification of Piweishu Pills

[0050] Take 2 pills of this product, cut them into pieces, take 12g, add 30ml of ethanol, ultrasonically treat for 15min, filter, and concentrate the filtrate to about 2ml as the test solution. Take another 0.5g of Atractylodes macrocephala control medicinal material, add 10ml of n-hexane, and prepare the control medicinal material solution in the same way. According to the thin layer chromatography test, take 10μl of each of the two newly prepared solutions, and spot them on the same silica gel G thin layer plate, use petroleum ether (60-90℃)-ethyl acetate (10:0.2) as the developing agent, develop, take out, dry, spray with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. The results show that the control medicinal material chromatogram shows pink spots, and the test product chromatogram does not show color at the corresponding position of the control medicinal material chromatogram. This method cannot achieve quality control.

[0051] Comparative Example 6 Identification of Piweishu Pills

[0052] Take 2 pills of this product, cut them into pieces, take 12g, grind them with diatomaceous earth (12g), add 30ml of n-hexane, ultrasonically treat for 15min, filter, and concentrate the filtrate to about 2ml as the test solution. Take another 0.5g of Atractylodes macrocephala control medicinal material, add 10ml of n-hexane, and prepare the control medicinal material solution in the same way. According to the thin layer chromatography test, take 10μl of each of the two newly prepared solutions, and spot them on the same silica gel G thin layer plate, use petroleum ether (60-90℃)-ethyl acetate (10:0.2) as the developing agent, develop, take out, dry, spray with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. The results show that the control medicinal material chromatogram shows pink spots, and the test product chromatogram shows blue-purple spots at the corresponding position of the control medicinal material chromatogram. This method cannot achieve quality control.

[0053] Example 1 Identification of Piweishu Pills

[0054] Take 2 pills of this product, cut them into pieces, take 12g, add 60ml of water to dissolve, centrifuge to remove the liquid, take the residue and put it in a drying oven at 65℃ for 3 hours to dry, take the residue and add 30ml of n-hexane, ultrasonically treat for 15min, filter, and concentrate the filtrate to about 2ml as the test solution. Take another 0.5g of Atractylodes macrocephala control medicinal material, add 10ml of n-hexane, and prepare the control medicinal material solution in the same way. According to the thin layer chromatography test, take 10μl of each of the two newly prepared solutions, and spot them on the same silica gel G thin layer plate, use petroleum ether (60~90℃)-ethyl acetate (10:0.2) as the developing agent, develop, take out, dry, spray with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. The results show that in the chromatogram of the test product, spots of the same color appear at the corresponding position of the chromatogram of the control medicinal material. This method can be used for quality control.

[0055] Identification of Embodiment 2 Piweishu Pills

[0056] Take 2 pills of this product, cut them into pieces, take 12g, add 40ml of methanol, heat and reflux for 2 hours (temperature 75-80℃), cool, extract with n-hexane shaking 3 times (15ml, 15ml, 10ml), combine the n-hexane extracts, recover the solvent and evaporate to dryness, add 2ml of n-hexane to dissolve the residue, and use it as the test solution. Take another 0.5g of Atractylodes macrocephala control medicinal material, add 20ml of n-hexane, and prepare the control medicinal material solution in the same way. According to the thin layer chromatography test, take 10μl of each of the two newly prepared solutions, spot them on the same silica gel G thin layer plate, use petroleum ether (60~90℃)-ethyl acetate (10∶0.2) as the developing solvent, develop, take out, dry, spray with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. The results show that the test solution shows spots of the same color at the corresponding position of the reference solution. This method can be used for quality control.

[0057] Example 3 Identification of Piweishu Pills

[0058] Take 2 long-term samples of Piweishu Pills (batch number: 20061007), cut them into pieces, take 12g, add 60ml of water to dissolve, centrifuge to remove the liquid, take the residue and put it into a drying oven at 65℃ for 3 hours to dry, take the residue and add 30ml of n-hexane, ultrasonically treat for 15min, filter, and concentrate the filtrate to about 2ml as the test solution. Take another 0.5g of Atractylodes macrocephala control medicinal material, add 10ml of n-hexane, and prepare the control medicinal material solution in the same way. According to the thin layer chromatography test, take 10μl of each of the two newly prepared solutions, and spot them on the same silica gel G thin layer plate, use petroleum ether (60~90℃)-ethyl acetate (10:0.2) as the developing agent, develop, take out, dry, spray with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. The results show that the test solution shows spots of the same color at the corresponding positions of the reference solution.

[0059] Example 4 Identification of Piweishu Pills

[0060] Take 2 long-term preserved Piweishu pills (batch number: 20070904), cut into pieces, take 12g, add 40ml methanol, heat and reflux for 2 hours (temperature 75-80℃), cool, shake and extract with n-hexane 3 times (15ml, 15ml, 10ml), combine the n-hexane extracts, recover the solvent and evaporate to dryness, add 2ml n-hexane to dissolve the residue, and use it as the test solution. Take 0.5g of Atractylodes macrocephala control medicinal material, add 20ml n-hexane, and prepare the control medicinal material solution in the same way. According to the thin layer chromatography test, take 10μl of each of the two newly prepared solutions, spot them on the same silica gel G thin layer plate, use petroleum ether (60~90℃)-ethyl acetate (10:0.2) as the developing solvent, develop, take out, dry, spray with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. The results show that the test solution shows spots of the same color at the corresponding positions of the reference solution.

[0061] Although the embodiments disclosed in the present invention are as above, the contents described are only embodiments adopted to facilitate understanding of the present invention and are not intended to limit the present invention. Any technician in the field to which the present invention belongs can make any modifications and changes in the form and details of implementation without departing from the spirit and scope disclosed in the present invention, but the patent protection scope of the present invention shall still be subject to the scope defined in the attached claims.

Claims

1. A quality control method for Piweishu pills, comprising the following steps: (1) Preparation of the test solution: Take an appropriate amount of Piweishu Pills, cut them into pieces, add an appropriate amount of water to dissolve them, remove the liquid, dry the residue, take the dried residue, add an appropriate amount of n-hexane, ultrasonically treat, filter, and concentrate the filtrate to obtain the test solution; (2) Preparation of reference medicinal material solution: Take an appropriate amount of Atractylodes macrocephala reference medicinal material, add an appropriate amount of n-hexane, perform ultrasonic treatment, filter, and concentrate the filtrate to obtain the solution; (3) Thin layer chromatography identification: Take appropriate amounts of the above two solutions and spot them on the same thin layer chromatography plate, develop them with an appropriate developer, let them dry, spray them with 5% vanillin sulfuric acid solution, and heat until the spots are clearly colored. In the chromatogram of the test sample, spots of the same color should appear at the corresponding positions in the chromatogram of the control medicinal material.

2. The quality control method according to claim 1, wherein the volume weight ratio (V / W) of water to Piwei Shu Wan in step (1) is 1-15:1, preferably 3-10:1, and more preferably 4-6:1; the method for removing the liquid in step (1) is selected from centrifugation or filtration; the method for drying the medicinal residue in step (1) is high temperature drying, the drying temperature is 30°C-100°C, preferably 50°C-80°C, and more preferably 55°C-70°C; the drying time is 1h-6h, and preferably 2h-4h; the volume weight ratio (V / W) of n-hexane to the medicinal residue in step (1) is 2-20:1, preferably 2-10:1, and more preferably 2-5:1; the volume weight ratio (V / W) of n-hexane to the control medicinal material in step (2) is 2-30:1, preferably 2-10:1, and more preferably 2-5:1; The ratio of W to W) is 5-30:1, preferably 10-25:1, and more preferably 15-20:

1. The time of ultrasonic treatment in step (1) and step (2) is 5 min-60 min, preferably 10 min-30 min, and more preferably 15 min-20 min. The amount of the two solutions absorbed in step (3) is 5 μl-25 μl, preferably 10 μl-20 μl. The thin layer chromatography plate in step (3) is selected from silica gel thin layer chromatography plate, alumina thin layer chromatography plate or polyethylene thin layer chromatography plate. The developing solvent in step (3) is petroleum ether (60-90° C.)-ethyl acetate, and preferably the ratio of petroleum ether:ethyl acetate is 1-100:1, preferably 30-70:1, and more preferably 40-60:

1.

3. According to the quality control method according to any one of claims 1-2, the prescription composition of the Piwei Shu Wan is: 50g of processed turtle shell, 50g of roasted astragalus, 50g of dried tangerine peel, 50g of immature bitter orange, 50g of white peony root, 50g of stir-fried Atractylodes macrocephala with bran, 50g of vinegar-cooked Cyperus rotundus, 50g of Tsaoko, 50g of stir-fried black plum, 50g of Chuanxiong, 50g of charred Areca catechu, and 50g of Magnolia officinalis. The above twelve Chinese medicines are crushed into fine powder, sieved, and mixed. 120-140g of refined honey is added to every 100g of powder to make large honey pills.

4. Use of the quality control method according to any one of claims 1 to 3 in the quality control of Piweishu Pills.

5. Use of the quality control method according to any one of claims 1 to 3 in thin layer chromatography identification of Piweishu Pills.

6. A quality control method for Piweishu pills, comprising the following steps: (1) Preparation of the test solution: Take an appropriate amount of Piweishu Pills, chop them into pieces, add an appropriate amount of methanol and heat to reflux, cool, extract with an appropriate amount of n-hexane by shaking, combine the n-hexane extracts, evaporate the solvent, and dissolve the residue in a small amount of n-hexane to obtain the test solution; (2) Preparation of reference medicinal material solution: Take an appropriate amount of Atractylodes macrocephala reference medicinal material, add an appropriate amount of n-hexane, perform ultrasonic treatment, filter, and concentrate the filtrate to obtain the solution; (3) Thin layer chromatography identification: Take appropriate amounts of the two solutions mentioned above, spot them on the same thin layer chromatography plate, develop them with an appropriate developer, let them dry, spray them with vanillin sulfuric acid solution, and heat until the spots are clearly colored. In the chromatogram of the test sample, spots of the same color should appear at the corresponding positions in the chromatogram of the control medicinal material.

7. The quality control method according to claim 6, wherein the volume weight ratio (V / W) of methanol to Piweishu Pills in step (1) is 1-15:1, preferably 3-10:1, and more preferably 3-5:1; the heating reflux temperature in step (1) is 60°C-90°C, preferably 65°C-85°C, and more preferably 70°C-80°C; the heating reflux time in step (1) is 1h-4h, preferably 1h-3h, and more preferably 1.5h-2.5h; in step (1), the extraction is performed by shaking with n-hexane for 1-5 times, preferably 2-4 times; the volume ratio (V / V) of the total amount of n-hexane used for extraction to methanol is 0.5-2:1; and the volume weight ratio of n-hexane to the control medicinal material in step (2) is 0.5-1:

1. V / W) is 5-30:1, preferably 10-25:1, and more preferably 15-20:

1. The time of ultrasonic treatment in step (2) is 5min-60min, preferably 10min-30min, and more preferably 15min-20min. The amount of the two solutions absorbed in step (3) is 5μl-25μl, preferably 10μl-20μl. The thin layer chromatography plate in step (3) is selected from silica gel thin layer chromatography plate, alumina thin layer chromatography plate or polyethylene thin layer chromatography plate. The developing solvent in step (3) is petroleum ether (60-90°C)-ethyl acetate, and preferably the ratio of petroleum ether:ethyl acetate is 1-100:1, preferably 30-70:1, and more preferably 40-60:

1.

8. According to the quality control method according to any one of claims 6-7, the prescription composition of the Piwei Shu Wan is: 50g of processed turtle shell, 50g of roasted astragalus, 50g of dried tangerine peel, 50g of immature bitter orange, 50g of white peony root, 50g of stir-fried Atractylodes macrocephala with bran, 50g of vinegar-cooked Cyperus rotundus, 50g of Tsaoko, 50g of stir-fried black plum, 50g of Chuanxiong, 50g of charred Areca catechu, and 50g of Magnolia officinalis. The above twelve Chinese medicines are crushed into fine powder, sieved, and mixed. 120-140g of refined honey is added to every 100g of powder to make large honey pills.

9. Use of the quality control method according to any one of claims 6 to 8 in the quality control of Piweishu Pills.

10. Use of the quality control method according to any one of claims 6 to 8 in thin layer chromatography identification of Piweishu Pills.