Fingerprint establishment method and quality control method of Naolingsu tablets

Abstract

The invention discloses a fingerprint establishment method and a quality control method of Naolingsu tablets, relates to the field of scientific research of traditional Chinese medicines, and solves the technical vacancy in the aspect of overall quality control of the Naolingsu tablets in the prior art. The method comprises the following steps: measuring 15 batches of test sample solutions of Naolingsu tablets through a high performance liquid chromatograph to obtain a fingerprint spectrum of the Naolingsu tablets, comparing the fingerprint spectrum with a control fingerprint spectrum, calculating the similarity through traditional Chinese medicine fingerprint spectrum similarity evaluation software, and if the similarity is not less than 0.9, determining that the quality of the Naolingsu tablets is qualified. Consistency of components and quality of all batches of products is ensured, and the technical vacancy of the existing Naolingsu tablets in the aspect of overall quality control is made up. According to the method, the quality of the Naolingsu tablets can be systematically and comprehensively evaluated, the scientificity and accuracy of quality control can be effectively improved, the analysis efficiency of the Naolingsu tablets is greatly improved, the analysis time and cost are reduced, and powerful support is provided for comprehensive and systematic quality control.

Description

Technical Field

[0001] The invention relates to the field of scientific research on traditional Chinese medicine, and in particular to a fingerprint establishment method and a quality control method for Naolingsu tablets. Background Art

[0002] Naolingsu Tablets is a traditional Chinese medicine compound preparation that has been on the market for many years. It is composed of 15 traditional Chinese medicines: Schisandra chinensis, Polygala tenuifolia (processed), Ziziphus jujuba seeds (fried), Poria cocos, Ginseng, Jujube, Epimedium, Deer Horn Glue, Deer Antler (dehaired), Tortoise Shell (processed), Lycium barbarum, Rehmannia glutinosa, Ophiopogon japonicus, Polygonatum sibiricum (steamed), Xanthium sibiricum (fried). At present, the current quality standards of Naolingsu Tablets are included in the 16th volume of the "Ministry of Health Drug Standards" Chinese Medicine Formula Preparations. The main contents include: 1. Properties: This product is a sugar-coated tablet. After removing the sugar coating, it is brown in color, bitter and slightly sour; 2. Identification: Ginseng, Poria cocos, and Polygonatum sibiricum are identified under a microscope; 3. Inspection: It should comply with the relevant provisions under the tablets. However, this standard cannot effectively reflect the quality of the drug. Although the single component of the preparation has been quantitatively tested in the existing literature, it is difficult to control the quality stability and consistency of clinical efficacy of the traditional Chinese medicine compound preparation by only determining the content of a single component of a certain medicinal material.

[0003] Traditional Chinese medicine compound preparations have complex chemical compositions, targets and mechanisms of action, so it is necessary to conduct overall quality control of their multiple active ingredients. At present, the main quality control methods for multiple components of traditional Chinese medicine are: multi-component quality control based on spectrum-effect correlation, multi-component quality control based on one-test-multiple-evaluation method, and multi-component quality control based on fingerprint spectrum. Among them, traditional Chinese medicine fingerprint spectrum is a comprehensive analytical method that can systematically, holistically and exclusively characterize the chemical components of traditional Chinese medicine, and reflect the overall quality status of traditional Chinese medicine as comprehensively as possible, which conforms to the characteristics of complex system quality control of traditional Chinese medicine. Common modern analytical techniques include infrared spectroscopy, ultraviolet spectroscopy, thin layer chromatography, high-performance liquid chromatography, gas chromatography, liquid chromatography-mass spectrometry, gas chromatography-mass spectrometry, immunoassay technology, electronic nose, electronic eye and other bionic technologies. Among them, high-performance liquid chromatography technology can simultaneously determine multiple components, has the characteristics of low detection limit and high sensitivity, and has been widely used in the quality research of traditional Chinese medicine. Summary of the invention

[0004] In order to solve the technical gap in the prior art in the overall quality control of Naolingsu tablets, the present invention proposes a fingerprint establishment method and a quality control method for Naolingsu tablets. The technical solution of the present invention is as follows:

[0005] A method for establishing a fingerprint spectrum of Naolingsu tablets comprises the following steps:

[0006] (1) Preparation of mixed reference solution: accurately weigh chlorogenic acid, icariin, epimedin C, and schisandrin A reference substances to prepare single reference substance stock solutions. Accurately pipette the single reference substance stock solutions separately, mix, and make up to volume to prepare a 100 μg / ml mixed reference substance solution.

[0007] (2) Preparation of test solution: Take Naolingsu tablets, remove the film coating, grind, mix, accurately weigh and place in a stoppered conical flask, add 70% methanol, weigh, ultrasonicate, cool, weigh again, make up the lost weight with 70% methanol, shake well, take the supernatant, filter, and obtain the Naolingsu tablet test solution;

[0008] (3) Preparation of single-herb reference substance solution: prepare single-herb extracts of epimedium, Xanthium sibiricum (fried), Lycium barbarum, Rehmannia root, Polygonatum sibiricum (steamed), Ophiopogon japonicus, Poria cocos, Tortoise shell (processed), Polygala tenuifolia (processed), jujube, antler glue, ginseng, pilose antler (dehaired), Schisandra chinensis, and Ziziphus jujuba seed (fried) according to the prescription process of Naolingsu tablets, and prepare single-herb reference substance solution according to the method of step (2);

[0009] (4) Preparation of negative control solution: According to the recipe of Naolingsu Tablets, samples lacking Epimedium, samples lacking Xanthium sibiricum (fried), samples lacking Lycium barbarum, samples lacking Rehmannia root, samples lacking Polygonatum sibiricum (steamed), samples lacking Ophiopogon japonicus, samples lacking Poria, samples lacking Tortoise Shell (processed), samples lacking Polygala tenuifolia (processed), samples lacking jujube, samples lacking antler glue, samples lacking ginseng, samples lacking pilose antler (dehaired), samples lacking Schisandra chinensis, and samples lacking Ziziphus jujuba seeds (fried) were prepared respectively, and negative control solution was prepared according to the method of step (2);

[0010] (5) Determination of the test solution: The test solution was aspirated and injected into a high performance liquid chromatograph for determination, and the chromatograms of 15 batches of Naolingsu tablets were obtained. The liquid chromatography conditions for fingerprint detection were as follows: the chromatographic column was a Symmetry Shield RP 18 chromatographic column (4.6×250 mm, 5 μm), the mobile phase A was acetonitrile, the mobile phase B was 0.05% phosphoric acid water, the flow rate was 1.0 mL / min, the detection wavelength was 260 nm, the column temperature was 30°C, and the injection volume was 10 μL;

[0011] (6) Establishment of fingerprint: The chromatograms of the test solutions of 15 batches of Naolingsu tablets were introduced into the similarity evaluation system of traditional Chinese medicine chromatographic fingerprint to determine their common fingerprint characteristic peaks, and the control fingerprints of 15 batches of Naolingsu tablets were established by software fitting. The common peaks were attributed by comparing with the chromatograms of the single-herb reference solution and the negative control solution;

[0012] Furthermore, in the preparation of the test solution in step (2), the power of the ultrasonic treatment is 500 W, the frequency of the ultrasonic treatment is 40 kHz, and the time of the ultrasonic treatment is 60 min;

[0013] Furthermore, in the preparation of the test solution in step (2), the filtration is performed by filtering through a 0.22 μm microporous filter membrane;

[0014] Further, in the determination of the test solution in step (5), the liquid chromatography conditions for fingerprint detection also include: the elution gradient is 0-5min 5%A, 5-30min 5-15%A, 30-52min15-20%A, 52-75min 20-25%A, 75-90min 25-28%A, 90-110min 28-36%A, 110-125min 36-40%A, 125-140min 40-100%A, 140-145min 100%A;

[0015] Furthermore, in the determination of the test solution in step (5), in the fingerprint of Naolingsu tablets, No. 9 was used as the reference peak, and a total of 12 common peaks were screened out, and the relative retention time of each common peak was calculated, which were: 0.115min, 0.201min, 0.237min, 0.340min, 0.680min, 0.760min, 0.925min, 0.972min, 1.000min, 1.372min, 1.418min, 1.436min;

[0016] Furthermore, in the establishment of the fingerprint spectrum of step (6), in the fingerprint spectrum of Naolingsu tablets, by comparing with the reference substance, it was confirmed that peak 4 was chlorogenic acid, peak 8 was epimedin C, peak 9 was icariin, and peak 10 was schisandrae alcohol A; by comparing with the chromatograms of fifteen single-drug reference substance solutions and negative control sample solutions, 12 common peaks were attributed, among which peak 1 was derived from the medicinal materials polygonatum, wolfberry, rehmannia root, and epimedium, peak 2 was derived from the medicinal materials Xanthium sibiricum (fried), Schisandra chinensis, and epimedium, peak 3 was derived from the medicinal materials wolfberry and epimedium, peak 4 was derived from the medicinal materials Xanthium sibiricum (fried) and epimedium, peaks 5 and 6 were derived from the medicinal material polygala tenuifolia (processed), peaks 7, 8, 9, 11, and 12 were derived from the medicinal material epimedium, and peak 10 was derived from the medicinal materials polygala tenuifolia (processed) and Schisandra chinensis;

[0017] Furthermore, in the establishment of the fingerprint spectrum in step (6), the obtained data and spectrum are processed using the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System" (2012.130723 version) compiled by the Chinese Pharmacopoeia Committee to obtain a control fingerprint spectrum.

[0018] A fingerprint spectrum of Naolingsu tablets is obtained by the above-mentioned method for establishing the fingerprint spectrum of Naolingsu tablets.

[0019] A quality control method for Naolingsu tablets is disclosed. The fingerprint spectrum of the Naolingsu tablets is compared with a control fingerprint spectrum of the Naolingsu tablets. If the similarity is calculated by a traditional Chinese medicine fingerprint spectrum similarity evaluation software and is not less than 0.9, the quality of the Naolingsu tablets is considered to be qualified, thereby completing the overall quality control of the Naolingsu tablets.

[0020] Compared with the prior art, the present invention solves the technical gap in the prior art in the overall quality control of Naolingsu tablets, and the specific beneficial effects are:

[0021] 1. The present invention establishes the fingerprint of Naolingsu tablets based on high performance liquid chromatography technology, realizes the overall quality control of Naolingsu tablets, ensures the consistency of ingredients and quality of each batch of products, and makes up for the technical gap in the overall quality control of existing Naolingsu tablets. This method can not only systematically and comprehensively evaluate the quality of Naolingsu tablets, but also effectively improve the scientificity and accuracy of quality control. This greatly improves the analysis efficiency, reduces the analysis time and cost, and provides strong support for comprehensive and systematic quality control.

[0022] 2. The method of the present invention is simple and easy to operate, low in cost, and is suitable for the routine quality inspection of Chinese medicine preparations. Through the application of high performance liquid chromatography technology, not only the accuracy and sensitivity of the measurement are improved, but also the use of complex and expensive instruments and equipment or technology is avoided, the overall detection cost is reduced, and the operation process is simplified. At the same time, the difference between different batches can be effectively controlled, the consistency and stability of drug quality can be ensured, and people's demand for drug safety and effectiveness is met, and it is suitable for extensive promotion and application.

[0023] 3. The present invention not only has significant advantages in the quality control of Naolingsu tablets, but also provides strong technical support for the secondary development of traditional Chinese medicine and the development of new drugs. By establishing a quality control system based on fingerprints, it can provide reference for the construction of quality standards for other traditional Chinese medicine preparations, promote technological progress in the field of traditional Chinese medicine, and promote the development and industrialization of new drugs. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 The fingerprint and reference spectrum of Naolingsu tablets (R);

[0025] Figure 2 Flow chart of the fingerprint establishment method and quality control method for Naolingsu tablets. DETAILED DESCRIPTION

[0026] In order to make the technical solution of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the specification of the present invention. It should be noted that the following embodiments are only used to better understand the technical solution of the present invention and should not be understood as a limitation to the present invention.

[0027] Experimental Materials:

[0028] 1260 InfinityⅡ liquid chromatograph (Agilent Technologies, USA); Milli-Q ultrapure water system (Millipore, USA); electronic balance (Sartorius Scientific Instruments (Beijing) Co., Ltd., BCE124I-1CCN); SQP electronic balance (Sartorius Scientific Instruments (Beijing) Co., Ltd.); KQ-500DE CNC ultrasonic cleaner (Kunshan Ultrasonic Instrument Co., Ltd.);

[0029] Epimedium, Xanthium sibiricum (fried), Lycium barbarum, Rehmannia root, Polygonatum sibiricum (steamed), Ophiopogon japonicus, Poria cocos, Tortoise shell (processed), Polygala tenuifolia (processed), Jujube, Deer antler glue, Ginseng, Ziziphus jujuba seed (fried), Deer antler (dehaired), Naolingsu tablets (Changchun People's Pharmaceutical Group Co., Ltd.);

[0030] Chlorogenic acid, icariin, epimedin C, schisandrin A, schisandrin B, schisandrin ester A, schisandrin ester B, schisandrin A, schisandrin B (standard products, Shanghai Fusion Pharmaceutical Technology Development Co., Ltd.).

[0031] Example:

[0032] (1) Preparation of mixed reference solution: Accurately weigh appropriate amounts of chlorogenic acid, icariin, epimedin C, and schisandrin A reference substances to prepare 1 mg / mL single reference substance stock solutions. Pipette 100 μL of each single reference substance stock solution, mix, and dilute to 1 mL to prepare a 100 μg / mL mixed reference solution.

[0033] (2) Preparation of the test solution: Take 10 tablets of Naolingsu, remove the film coating, grind them into powder, mix them, weigh 2.0 g, accurately weigh them and place them in a 50 mL stoppered conical flask, add 25 mL of 70% methanol and weigh them. Ultrasonicate (power 500 W, frequency 40 kHz) for 60 min, cool them, weigh them again, make up the lost weight with 70% methanol, shake them well, take the supernatant, and filter them through a 0.22 μm microporous filter membrane to obtain the test solution.

[0034] (3) Preparation of single-herb reference solution: Prepare single-herb extracts of epimedium, Xanthium sibiricum (fried), Lycium barbarum, Rehmannia root, Polygonatum sibiricum (steamed), Ophiopogon japonicus, Poria cocos, Tortoise shell (processed), Polygala tenuifolia (processed), jujube, antler glue, ginseng, pilose antler (dehaired), Schisandra chinensis, and Ziziphus jujuba seed (fried) according to the prescription process of Naolingsu tablets, and prepare the single-herb reference solution according to step (2).

[0035] (4) Preparation of negative control solution: According to the prescription process of Naolingsu Tablets, prepare samples lacking Epimedium, lacking Xanthium sibiricum (fried), lacking Lycium barbarum, lacking Rehmannia root, lacking Polygonatum sibiricum (steamed), lacking Ophiopogon japonicus, lacking Poria, lacking Tortoise Shell (processed), lacking Polygala tenuifolia (processed), lacking jujube, lacking antler glue, lacking ginseng, lacking pilose antler (dehaired), lacking Schisandra chinensis, and lacking Ziziphus jujuba seed (fried), and prepare negative control solution according to the method of step (2).

[0036] (5) Determination of the test solution: The test solution was aspirated and injected into a high performance liquid chromatograph for determination to obtain a chromatogram of the Naolingsu tablets. The liquid chromatography conditions for fingerprint detection were as follows: the chromatographic column was a Symmetry Shield RP 18 chromatographic column (4.6×250 mm, 5 μm), the mobile phase A was acetonitrile, the mobile phase B was 0.05% phosphoric acid water, the flow rate was 1.0 mL / min, the detection wavelength was 260 nm, the column temperature was 30°C, the injection volume was 10 μL, and the elution gradient was 0-5 min 5% A, 5-30 min 5-15% A, 30-52 min 15-20% A, 52-75 min 20-25% A, 75-90 min 25-28% A, 90-110 min 28-36% A, 110-125 min 36-40% A, 125-140 min 40-100%A, 140-145min 100%A.

[0037] (6) Establishment of fingerprint: Prepare 15 batches of test solution according to step (2), measure according to the liquid chromatography conditions of step (5), record the chromatogram (CDF format), import the original data into the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System" (2012.130723 version), perform common peak matching by multi-point correction method, obtain the fingerprint of Naolingsu tablets, take S9 as the reference spectrum, and use the median method to generate the reference fingerprint of 15 batches of Naolingsu tablets. Figure 1 This is the fingerprint and reference spectrum of Naolingsu tablets (R).

[0038] The fingerprint spectrum used peak 9 as the reference peak, and a total of 12 common peaks were screened out. By comparing with the reference substance, it was confirmed that peak 4 was chlorogenic acid, peak 8 was epimedin C, peak 9 was icariin, and peak 10 was schisandrae alcohol A.

[0039] By comparing the chromatograms with those of fifteen single-drug reference solutions and negative control sample solutions, 12 common peaks were assigned, among which peak 1 originated from the medicinal materials Polygonatum sibiricum, Lycium barbarum, Rehmannia root, and Epimedium, peak 2 originated from the medicinal materials Xanthium sibiricum (fried), Schisandra chinensis, and Epimedium, peak 3 originated from the medicinal materials Lycium barbarum and Epimedium, peak 4 originated from the medicinal materials Xanthium sibiricum (fried) and Epimedium, peaks 5 and 6 originated from the medicinal material Polygala tenuifolia (processed), peaks 7, 8, 9, 11, and 12 originated from the medicinal material Epimedium, and peak 10 originated from the medicinal materials Polygala tenuifolia (processed) and Schisandra chinensis.

[0040] Methodological investigation:

[0041] (1) Precision investigation: Prepare the test solution according to the method of step (2) in 1.2, repeat the test solution for 6 times, record the retention time and peak area of ​​each chromatographic peak, and calculate the RSD of its relative retention time and relative peak area. The precision RSD of the relative retention time of the 12 common peaks were 0.33%, 0.44%, 0.36%, 0.24%, 0.09%, 0.09%, 0.01%, 0.01%, 0.00%, 0.02%, 0.02%, 0.02%, all less than 1%; the precision RSD of the relative peak area were 1.62%, 2.33%, 1.38%, 2.03%, 2.71%, 1.51%, 2.72%, 0.73%, 0.00%, 2.68%, 1.20%, 1.48%, all less than 3%, indicating that the precision of the instrument is good.

[0042] (2) Repeatability study: Six samples of the test solution were prepared in parallel according to the method of step (2) in 1.2, and the samples were measured. The retention time and peak area of ​​each chromatographic peak were recorded, and the RSD of the relative retention time and relative peak area was calculated. The RSD of the repeatability of the relative retention time of the 12 common peaks was 0.14%, 0.06%, 0.28%, 0.03%, 0.01%, 0.01%, 0.01%, 0.02%, 0.00%, 0.02%, 0.02%, and 0.02%, respectively, all less than 1%; the RSD of the repeatability of the relative peak area was 1.83%, 1.23%, 2.68%, 1.58%, 2.85%, 0.88%, 2.38%, 1.00%, 0.00%, 1.41%, 0.70%, and 1.63%, respectively, all less than 3%, indicating that the method has good repeatability.

[0043] (3) Stability study: Prepare the test solution according to the method in step (2) of 1.2, and measure it at 0 h, 4 h, 8 h, 12 h, 16 h, and 24 h, respectively. Record the retention time and peak area of ​​each chromatographic peak, and calculate the RSD of the relative retention time and relative peak area. The stability RSDs of the relative retention times of the 12 common peaks were 0.16%, 0.21%, 0.08%, 0.11%, 0.04%, 0.04%, 0.02%, 0.00%, 0.00%, 0.02%, 0.01%, and 0.02%, respectively, all less than 1%; the stability RSDs of the relative peak areas were 2.22%, 2.78%, 2.28%, 2.18%, 2.41%, 2.31%, 1.97%, 2.10%, 0.00%, 2.40%, 2.26%, and 2.49%, respectively, all less than 3%, indicating that the test solution had good stability within 24 hours.

[0044] Similarity evaluation:

[0045] The similarity evaluation of the fingerprints of 15 batches of Naolingsu tablets and the control fingerprints is shown in Table 1. The similarity of the liquid chromatograms of the 15 batches is greater than 0.9, indicating that the sample has good homogeneity and stable quality. Figure 2 Flow chart of the fingerprint establishment method and quality control method for Naolingsu tablets.

[0046] Table 1

[0047]

[0048]

[0049] In summary, the present invention establishes the fingerprint of Naolingsu tablets based on high performance liquid chromatography technology, ensures the consistency of ingredients and quality of each batch of products, and makes up for the technical gap in the overall quality control of existing Naolingsu tablets. This method can not only systematically and comprehensively evaluate the quality of Naolingsu tablets, but also effectively improve the scientificity and accuracy of quality control. This greatly improves the analysis efficiency of Naolingsu tablets, reduces analysis time and cost, and provides strong support for comprehensive and systematic quality control.

[0050] It is to be understood that the present invention is described by some embodiments, and it is known to those skilled in the art that various changes or equivalent substitutions may be made to these features and embodiments without departing from the spirit and scope of the present invention. In addition, under the teachings of the present invention, these features and embodiments may be modified to adapt to specific circumstances and materials without departing from the spirit and scope of the present invention. Therefore, the present invention is not limited by the specific embodiments disclosed herein, and all embodiments falling within the scope of the claims of this application are within the scope of protection of the present invention.

Claims

1. A method for establishing a fingerprint of Naolingsu tablets, characterized in that: The following steps are involved: (1) Preparation of mixed reference solution: accurately weigh chlorogenic acid, icariin, epimedin C, and schisandrin A reference substances to prepare single reference substance stock solutions. Accurately pipette the single reference substance stock solutions separately, mix, and make up to volume to prepare a 100 μg / ml mixed reference substance solution. (2) Preparation of test solution: Take Naolingsu tablets, remove the film coating, grind, mix, accurately weigh and place in a stoppered conical flask, add 70% methanol, weigh, ultrasonicate, cool, weigh again, make up the lost weight with 70% methanol, shake well, take the supernatant, filter, and obtain the Naolingsu tablet test solution; (3) Preparation of single-herb reference substance solution: prepare single-herb extracts of epimedium, Xanthium sibiricum, Lycium barbarum, Rehmannia root, Polygonatum sibiricum, Ophiopogon japonicus, Poria cocos, Carapax tortoise shell, Polygala tenuifolia, jujube, antler glue, ginseng, pilose antler, Schisandra chinensis, and Ziziphus jujuba seed according to the prescription process of Naolingsu tablets, and prepare single-herb reference substance solution according to the method of step (2); (4) Preparation of negative control solution: According to the prescription process of Naolingsu Tablets, prepare samples lacking Epimedium, lacking Xanthium sibiricum, lacking Lycium barbarum, lacking Rehmannia glutinosa, lacking Polygonatum sibiricum, lacking Ophiopogon japonicus, lacking Poria, lacking Carapax tortoise shell, lacking Polygala tenuifolia, lacking jujube, lacking antler glue, lacking ginseng, lacking pilose antler, lacking Schisandra chinensis, and lacking Ziziphus jujuba seed, and prepare negative control solution according to the method of step (2); (5) Determination of the test solution: The test solution was aspirated and injected into a high performance liquid chromatograph for determination, and the chromatograms of 15 batches of Naolingsu tablets were obtained. The liquid chromatography conditions for fingerprint detection were as follows: the chromatographic column was a Symmetry Shield RP 18 chromatographic column (4.6×250 mm, 5 μm), the mobile phase A was acetonitrile, the mobile phase B was 0.05% phosphoric acid water, the flow rate was 1.0 mL / min, the detection wavelength was 260 nm, the column temperature was 30°C, and the injection volume was 10 μL; (6) Establishment of fingerprint: The chromatograms of 15 batches of Naolingsu tablets were imported into the Chinese medicine chromatographic fingerprint similarity evaluation system to determine their common fingerprint characteristic peaks. The control fingerprints of 15 batches of Naolingsu tablets were established by software fitting. The common peaks were attributed by comparing with the chromatograms of single-herb reference solution and negative control solution.

2. The method for establishing the fingerprint of Naolingsu tablets according to claim 1, characterized in that: The power of the ultrasonic treatment in the preparation of the test solution in step (2) is 500W.

3. The method for establishing the fingerprint of Naolingsu tablets according to claim 1, characterized in that: The frequency of ultrasonic treatment in the preparation of the test solution in step (2) is 40 kHz.

4. The method for establishing the fingerprint of Naolingsu tablets according to claim 1, characterized in that: The ultrasonic treatment time in the preparation of the test solution in step (2) is 60 minutes.

5. The method for establishing the fingerprint of Naolingsu tablets according to claim 1, characterized in that: The filtration is performed by filtering through a 0.22 μm microporous membrane.

6. The method for establishing the fingerprint of Naolingsu tablets according to claim 1, characterized in that: In the determination of the test solution in step (5), the liquid chromatography conditions for fingerprint detection also include: an elution gradient of 0-5min 5% A, 5-30min 5-15% A, 30-52min 15-20% A, 52-75min 20-25% A, 75-90min 25-28% A, 90-110min28-36% A, 110-125min 36-40% A, 125-140min40-100% A, 140-145min 100% A.

7. The method for establishing the fingerprint of Naolingsu tablets according to claim 1, characterized in that: In the determination of the test solution in the step (5), in the fingerprint of Naolingsu tablets, taking No. 9 as the reference peak, a total of 12 common peaks were screened out, and the relative retention time of each common peak was calculated, which were: 0.115min, 0.201min, 0.237min, 0.340min, 0.680min, 0.760min, 0.925min, 0.972min, 1.000min, 1.372min, 1.418min, and 1.436min, respectively.

8. A fingerprint spectrum of Naolingsu tablets, characterized in that: Obtained by the fingerprint establishment method of the Naolingsu tablets described in any one of claims 1-7.

9. A quality control method for Naolingsu tablets, characterized in that: The fingerprint of the Naolingsu tablets obtained by the fingerprint establishment method of any one of claims 1 to 7 or the Naolingsu tablets described in claim 8 is compared with the control fingerprint of the Naolingsu tablets. If the similarity is calculated by the traditional Chinese medicine fingerprint similarity evaluation software and is not less than 0.9, the quality of the Naolingsu tablets is considered to be qualified, and the overall quality control of the Naolingsu tablets is completed.

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