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CN-121994977-A - Method for establishing HPLC fingerprint of Shuxin Jiangzhi tablet and fingerprint thereof

CN121994977ACN 121994977 ACN121994977 ACN 121994977ACN-121994977-A

Abstract

The invention discloses a method for establishing HPLC fingerprint of a Shuxin Jiangzhi tablet, wherein the method comprises the preparation of a reference substance and a sample solution, the determination of HPLC chromatographic conditions and the preparation of HPLC standard fingerprint. Meanwhile, the HPLC standard fingerprint of the Shuxin Jiangzhi tablet obtained by the method is disclosed, the fingerprint has 15 peaks, and 6 common peaks are identified by a reference substance. The method is simple and convenient, has good stability and reproducibility, the characteristic peaks of the obtained atlas are comprehensive, and the quality of the Shuxin Jiangzhi tablet can be comprehensively evaluated and controlled by comparing the common peaks of the standard fingerprint atlas, thereby being beneficial to accurately evaluating the inherent quality of the preparation and ensuring the safety and the effectiveness of clinical medication.

Inventors

  • CHEN HUANHUAN
  • ZHAO GUOQIANG
  • Li Haishuai
  • HAN XUE
  • WANG JIANYUN
  • LI YANING
  • WANG QI

Assignees

  • 河北国金药业有限责任公司

Dates

Publication Date
20260508
Application Date
20250329

Claims (10)

  1. 1. The method for establishing the HPLC fingerprint of the Shuxin Jiangzhi tablet is characterized by comprising the following steps: The preparation method of control and test solution comprises weighing sodium salvianic acid A, puerarin, polydatin, salvianolic acid B, emodin and tanshinone II A , and dissolving with methanol to obtain control solution; taking 10 pieces of Shuxin Jiangzhi tablets, removing film coatings, grinding, uniformly mixing, precisely weighing, adding 75% -100% methanol 20 ml, carrying out water bath reflux/ultrasonic extraction for 30: 30 min, cooling, filtering with a 0.45 mu m microporous filter membrane, and taking a subsequent filtrate to obtain the traditional Chinese medicine composition; Determining HPLC chromatographic conditions, namely taking octadecylsilane chemically bonded silica as a filler, acetonitrile as a mobile phase A,0.1% phosphoric acid solution as a mobile phase B, adopting gradient elution, detecting the wavelength of 230-367 nm, the flow rate of 1.0 ml/min, and the column temperature of 25 ℃; preparing fingerprint, namely carrying out sample injection analysis on the reference substance solution and the sample solution by adopting HPLC to obtain the HPLC fingerprint of the sample solution; And (3) introducing the HPLC fingerprint data of the sample solution into software of a traditional Chinese medicine chromatographic fingerprint similarity evaluation system 2012 edition recommended by the national formulary committee, taking the fingerprint of one of the sample solutions as a reference spectrum, and generating a standard fingerprint of the Shuxin Jiangzhi tablet by adopting an average method.
  2. 2. The method for establishing the test sample solution according to claim 1, wherein the test sample solution in step 1) is prepared by taking 10 tablets of Shuxin Jiangzhi tablets, removing film coatings, precisely weighing, grinding, uniformly mixing, taking about 0.72 g, precisely weighing, placing in a conical flask with a plug, precisely adding 75% methanol 20 ml, placing in a water bath kettle, heating and refluxing for 30 minutes, cooling, shaking, filtering with a microporous filter membrane with 0.45 μm, and taking subsequent filtrate to obtain the test sample solution.
  3. 3. The method according to claim 1, wherein the step 3) comprises taking the same batch of sample solution of the heart-soothing lipid-lowering tablet, continuously sampling for 6 times, and recording a chromatogram; taking the same batch of sample solutions of the heart-soothing lipid-lowering tablets, respectively sampling at 0,2,6,10,18 and 24 hours, and recording a chromatogram; meanwhile, 6 parts of sample solutions of the heart-soothing lipid-lowering tablet are prepared, sample injection is carried out respectively, and a chromatogram is recorded.
  4. 4. The method of claim 1, wherein the chromatographic Column in step 2) is WATERS SYMMETRY C Column chromatography.
  5. 5. The method according to claim 1, wherein the chromatographic column has a size of 4.6x250 mm,5 μm.
  6. 6. The method according to claim 1, wherein the detection wavelength in step 2) is 275nm.
  7. 7. The method according to claim 1, wherein the gradient elution conditions in step 2) are: Time (minutes) Mobile phase a (%) Mobile phase B (%) 0~10 3→6 97→94 10~15 6→10 94→90 15~20 10 90 20-55 10→20 90→80 55-75 20→35 80→65 75-100 35→40 65→60 100-110 40→55 60→45 110-120 55→80 45→20 120-121 80→3 20→97 121-130 3 97
  8. 8. The method according to claim 1, wherein the main components of the tablet comprise radix Salviae Miltiorrhizae, pollen Fagopyri Esculenti, fructus crataegi, rhizoma Polygoni Cuspidati, radix Puerariae, flos Carthami, bulbus Allii Macrostemonis, semen Persicae, caulis Spatholobi, lignum Dalbergiae Odoriferae, and radix Paeoniae Rubra, and in step 4), it is confirmed that the fingerprint of the tablet has 15 common peaks, and the relative retention time of the common peaks is 0.116,0.185,0.283,0.378,0.476,0.489,0.611,0.786,0.915,0.958,0.990,1.031,1.591,1.633.
  9. 9. The fingerprint of the heart-soothing lipid-lowering tablet of claims 1-8, wherein the fingerprint comprises 15 common peaks, and 6 common peaks of the 15 common peaks are identified as sodium salvianolate (peak No. 2), puerarin (peak No. 5), polydatin (peak No. 8), salvianolic acid B (peak No. 12), emodin (peak No. 14) and tanshinone II A (peak No. 15), respectively.
  10. 10. The method for detecting the quality of the heart-soothing lipid-lowering tablet is characterized by comprising the following steps of: preparing chromatographic peaks of a sample to be detected; Comparing the chromatographic peak of Yang to be detected with the fingerprint of the Shuxin Jiangzhi tablet in the patent claim 8, and if the similarity is more than 0.9, indicating that the quality of the sample to be detected is qualified.

Description

Method for establishing HPLC fingerprint of Shuxin Jiangzhi tablet and fingerprint thereof Technical Field The invention belongs to the field of analysis of traditional Chinese medicine preparations, and discloses a method for establishing an HPLC fingerprint of a Shuxin Jiangzhi tablet. Background A heart-soothing and lipid-lowering tablet is a medicine for treating diseases such as qi and blood turbid phlegm obstruction, chest pain, palpitation and insomnia, epigastric fullness and hypodynamia and the like. The Chinese medicinal composition adopts the red sage root and the hawthorn which activate blood circulation to remove blood stasis and remove stagnation to reduce blood lipid as monarch drugs, adopts peach kernels, safflower, red paeony root, giant knotweed rhizome and suberect spatholobus stem which remove blood stasis to reduce blood lipid to remove meridian obstruction to relieve pain as ministerial drugs, and adopts allium macrostemon, rosewood heart wood, kudzuvine root and wheat-flour which serve as adjuvant drugs to regulate qi, relieve chest pain, activate yang to remove turbidity and reduce blood lipid, and the above drugs are combined together to play the roles of activating blood circulation to remove blood stasis, activating yang to remove turbidity and activating qi to relieve pain. The active ingredients of the Chinese medicinal composition comprise, by weight, 183g of red sage root, 31.4g of buckwheat pollen, 171.4g of haw, 34.3g of giant knotweed, 34.3g of kudzuvine root, 34.3g of safflower, 34.3g of allium macrostemon, 11.4g of peach kernel, 34.3g of suberect spatholobus stem, 17g of rosewood and 34.3g of red paeony root. The Shuxin Jiangzhi tablet is a Chinese medicinal compound preparation, and the Chinese medicinal preparation contains a plurality of Chinese medicaments and has complex chemical components, and the chemical components generate an overall treatment effect, so that the Chinese medicinal preparation can play an important index of medicinal effect, and effective quality control is an important basis for ensuring the clinical curative effect. The quality control of the Shuxin Jiangzhi tablet refers to the fourteenth book WS3-B-2799-97 of the standard Chinese medicine formulation of the medicine of the Ministry of health, and the detection content is mainly the identification of physicochemical and ultraviolet spectrophotometry, but because the composition of the Shuxin Jiangzhi tablet is more, the detection and identification are difficult to be completely lack and reflect the whole quality of the preparation. Therefore, in order to ensure and stabilize the quality of the product, comprehensive researches on quality detection and control methods thereof are required. The HPLC fingerprint research of the Shuxin Jiangzhi tablet can identify 6 common peaks, and the method for establishing the fingerprint of the Shuxin Jiangzhi tablet is provided, so that the integrity and complexity of chemical components of the Shuxin Jiangzhi tablet are effectively reflected, the quality of the preparation is comprehensively evaluated and controlled, and the safety and effectiveness of clinical medication are further ensured. Disclosure of Invention The invention aims to provide a method for establishing a finger print of a heart-soothing lipid-lowering tablet. Specifically, the method prepares the Shuxin Jiangzhi tablet into a sample solution, and performs HPLC separation detection to obtain the standard fingerprint of the Shuxin Jiangzhi tablet, so as to realize all-round multi-aspect detection, perfect the quality detection system, and have good stability and durability, thereby providing reliable basis for the true and false identification and the internal quality of the Shuxin Jiangzhi tablet, and ensuring clinical curative effect. The invention relates to a method for establishing an HPLC fingerprint of a Shuxin Jiangzhi tablet, which is characterized by comprising the following steps: 1) The preparation method of control and test solution comprises weighing sodium salvianic acid A, puerarin, polydatin, salvianolic acid B, emodin and tanshinone II A, and dissolving with methanol to obtain control solution; 2) Taking 10 pieces of Shuxin Jiangzhi tablet, removing film coat, grinding, mixing well, precisely weighing, adding 75% methanol 20ml, refluxing in water bath for 30min, cooling, filtering with 0.45 μm microporous membrane, and collecting subsequent filtrate. Determining HPLC chromatographic conditions by taking octadecylsilane chemically bonded silica as filler, acetonitrile as mobile phase A,0.1% phosphoric acid solution as mobile phase B, gradient eluting, and detecting wavelength of 275nm at flow rate of 1.0ml/min at column temperature of 25deg.C; 3) Preparing fingerprint, namely carrying out sample injection analysis on the reference substance solution and the sample solution by adopting HPLC to obtain the HPLC fingerprint of the sample solution; 4) And (3) introducing the H