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CN-117741031-B - Construction method, detection method and application of strong Ma De Tu Alite preparation fingerprint

CN117741031BCN 117741031 BCN117741031 BCN 117741031BCN-117741031-B

Abstract

The invention discloses a method for constructing a fingerprint of a powerful Ma De Tu Ala special agent, a detection method and application thereof. The construction method comprises the steps of detecting a sample solution by utilizing high performance liquid chromatography, generating a fingerprint according to a detection result, wherein the sample solution is a solution containing the powerful Ma De-Tu-Ala preparation, a chromatographic column is a YMC-Triart C 18 column in the high performance liquid chromatography, the column temperature is 26-40 ℃, the flow rate is 1.05-1.5mL/min, a mobile phase A is acetonitrile, and a mobile phase B is a phosphoric acid aqueous solution with the volume concentration of 0.06% -0.2%. The fingerprint spectrum is established aiming at the powerful Ma De Tu Ala preparation, the quality condition of the powerful Ma De Tu Ala preparation can be evaluated from the whole angle, the unilateral quality control of single components is avoided, and the guarantee is provided for the safe use of the powerful Ma De Tu Ala preparation.

Inventors

  • YIN QIANG
  • Du Mengge
  • LI CHAOJIE
  • SONG FEI
  • WEI WEI
  • YIN HAILONG
  • MENG WENQUAN
  • MU DANDAN
  • DONG YUWEI
  • CHEN CHANGCHUN
  • TIAN FANG
  • ZHOU QIN

Assignees

  • 新疆维吾尔药业有限责任公司

Dates

Publication Date
20260512
Application Date
20231208
Priority Date
20231114

Claims (11)

  1. 1. The method for constructing the fingerprint of the powerful Ma De Tu Alite preparation is characterized by comprising the following steps of: s1, preparing a sample solution, wherein the sample solution is a solution containing the powerful Ma De Tu Ala preparation, and an extraction solvent used for preparing the sample solution is 75% methanol water solution; S2, preparing a mixed reference substance solution, wherein the mixed reference substance solution comprises gallic acid, corilagin, cinnamaldehyde, 6-gingerol, ellagic acid and piperine, and the dissolution solvent in the preparation of the mixed reference substance solution is 75% methanol water solution; S3, detecting the sample solution and the mixed reference substance solution according to the following high performance liquid chromatography respectively; The chromatographic conditions comprise octadecylsilane chemically bonded silica as filler, acetonitrile as mobile phase A, 0.1% phosphoric acid aqueous solution as mobile phase B, gradient elution according to the following table, detection wavelength of 280nm, flow rate of 1.2mL min -1 , column temperature of 30deg.C, YMC-Triart C 18 column of 4.6mm×150mm,5 μm, and high performance liquid chromatograph of Thermo Scientific UlitiMate 3000 type; time min Mobile phase A% Mobile phase B% 0~6 4 96 6~9 4~12 96~88 9~15 12~13 88~87 15~24 13~19 87~81 24~51 19~65 81~35 51~56 65~4 35~96 56~60 4 96 The percentages in the table are the volume percentages of each component in the total volume of mobile phase A and mobile phase B, respectively; and determining the attribution of each peak in the sample solution according to the retention time of each substance in the mixed reference substance solution, and generating a fingerprint according to the detection result of the sample solution.
  2. 2. The method for constructing the fingerprint of the powerful Ma De Tu Alite preparation according to claim 1, which is characterized in that, In the high performance liquid chromatography, the sample injection volume is 5-20 mu L.
  3. 3. The method for constructing a fingerprint of a powerful madaiyate preparation according to claim 2, wherein the sample injection volume in the high performance liquid chromatography is 10 μl.
  4. 4. The method for constructing the fingerprint of the powerful Ma De Tu Alite preparation according to claim 1, which is characterized in that, In the sample solution, the mass volume ratio of the powerful Ma De-Tu-Ala preparation to the extraction solvent is 1g (40-60) mL; And/or the sample solution is prepared by mixing the powerful Ma De-Tu-Alite preparation with the extraction solvent, performing ultrasonic treatment, cooling, and filtering.
  5. 5. The method for constructing a fingerprint of a powerful madaisub preparation according to claim 4, wherein the mass-to-volume ratio of the powerful madaisub preparation to the extraction solvent in the sample solution is 1g:45mL or 1g:50mL.
  6. 6. The method for constructing the fingerprint of the powerful Madeli-African preparation as claimed in claim 1, wherein in the mixed reference solution, the concentration of gallic acid is 30-40 mug/mL, the concentration of corilagin is 30-35 mug/mL, the concentration of cinnamaldehyde is 3-5 mug/mL, the concentration of 6-gingerol is 20-30 mug/mL, the concentration of piperine is 90-100 mug/mL, and the concentration of ellagic acid is 5-10 mug/mL.
  7. 7. The method for constructing the fingerprint of the powerful Madeli-African preparation as claimed in claim 6, wherein in the mixed reference solution, the concentration of gallic acid is 37 mug/mL, the concentration of corilagin is 31 or 31.05 mug/mL, the concentration of cinnamaldehyde is 4 or 4.12 mug/mL, the concentration of 6-gingerol is 25.9 or 26 mug/mL, the concentration of piperine is 97 or 97.10 mug/mL, and the concentration of ellagic acid is 7 or 7.3 mug/mL.
  8. 8. The method for constructing the fingerprint of the powerful madillidium preparation according to claim 1, wherein the fingerprint obtained by the method for constructing the fingerprint of the powerful madillidium preparation comprises 6 common peaks, peak 11 is taken as a reference peak, and the relative retention time of the common peaks is respectively as follows: peak 1 is gallic acid, relative retention time is 0.123-0.124, rsd is 0.25%; Peak 2 is corilagin, relative retention time is 0.392, RSD is 0.00%; Peak 6 is ellagic acid with a relative retention time of 0.592 and RSD of 0.00%; Peak 9 is cinnamaldehyde, the relative retention time is 0.811, and the RSD is 0.00%; Peak 10 is 6-gingerol, relative retention time is 0.946, RSD is 0.00%; peak 11 is piperine with a relative retention time of 1.00 and RSD of 0.00%.
  9. 9. The method for constructing the fingerprint of the powerful madillidium preparation according to claim 8, which is characterized in that the fingerprint obtained by the method for constructing the fingerprint of the powerful madillidium preparation further comprises the following 5 common peaks, wherein peak 11 is taken as a reference peak, and the relative retention time of the common peaks is respectively: the relative retention time of peak 3 was 0.439 and rsd was 0.00%; peak 4 has a relative retention time of 0.458-0.459 and rsd of 0.09%; the relative retention time of peak 5 was 0.572-0.573 and rsd was 0.08%; the relative retention time of peak 7 was 0.731 and rsd was 0.00%; the relative retention time of peak 8 was 0.764 and rsd was 0.00%.
  10. 10. A method for detecting the quality of a powerful madillidium preparation, which is characterized in that the method comprises generating a fingerprint of a sample to be detected according to the method for constructing the powerful madillidium preparation fingerprint as claimed in any one of claims 1 to 9.
  11. 11. A quality control method of a powerful madaiia preparation, characterized in that a fingerprint obtained by the construction method of the powerful madaiia preparation fingerprint as claimed in any one of claims 1-9 is used as a standard fingerprint in quality control of the powerful madaiia preparation.

Description

Construction method, detection method and application of strong Ma De Tu Alite preparation fingerprint Technical Field The invention relates to the technical field of traditional Chinese medicine detection, in particular to a construction method, a detection method and application of a strong Ma De Tu Alite preparation fingerprint. Background The traditional Chinese medicine has complex components, the traditional Chinese medicine compound preparation prepared from a plurality of medicinal materials has more complex components, and the traditional Chinese medicine fingerprint can embody the whole quality of the traditional Chinese medicine and the compound preparation, thereby having important effect in the aspect of quality control. The high performance liquid fingerprint method has the characteristics of high sensitivity and strong selectivity, and can evaluate the similarity of traditional Chinese medicines and compound preparations. The quality of the traditional Chinese medicine preparation is comprehensively evaluated through a traditional Chinese medicine chromatographic fingerprint similarity evaluation system (2012 edition) which is put forward by the national formulary Committee. The powerful Made Tuli Ayite honey paste is a vitamin preparation commonly used in hospitals, is loaded in the Xinjiang Uygur autonomous region Uygur medical institution preparation standard (standard number: MZJ-W-0133-2013), is composed of 14 medicinal materials such as dried ginger, black pepper, long pepper, cinnamon and the like, has the effects of strengthening the body, relieving pain, tonifying brain and nourishing brain, and is used for treating hemiplegia, joint bone pain, dementia, heavy tongue, waist soreness and other diseases. However, the existing standard test items for the powerful Ma De Tu Alite preparation are few, only have characters, identification and inspection items, the quality of the medicine cannot be accurately and comprehensively controlled, and reports on the related research of the fingerprint of the powerful Ma De Tu Alite preparation are not yet relevant. Therefore, the establishment of the fingerprint spectrum of the powerful Ma De Tu Alite preparation is needed to perfect the quality standard of the preparation, so that the overall quality of the preparation can be evaluated systematically and comprehensively. Disclosure of Invention The invention aims to overcome the defect that the strong Ma De Tu Lai Ala preparation fingerprint is lacking in the prior art, and provides a method for constructing the strong Ma De Tu Ala preparation fingerprint, a detection method and application thereof. The detection method can simply, rapidly and accurately evaluate the quality of the powerful Ma De Tu Alite preparation, and provides scientific basis for establishing the quality standard of the powerful Ma De Tu Alite preparation from the whole angle. The invention establishes the fingerprint for the powerful Ma De Tu Ala preparation, can comprehensively and accurately reflect the quality of the powerful Ma De Tu Ala preparation, provides theoretical basis and data reference for quality control and standard promotion, can evaluate the quality condition of the powerful Ma De Tu Ala preparation from the whole angle, avoids the unilateral quality control of a single component, and provides guarantee for the safe use of the powerful Ma De Tu Ala preparation. The invention solves the technical problems through the following technical proposal. The invention provides a method for constructing a strong Ma De Tu Alite preparation fingerprint, which comprises the following steps of detecting a sample solution by using high performance liquid chromatography, and generating a fingerprint from a detection result; The sample solution is a solution containing the powerful Ma De Tu Alite preparation; In the high performance liquid chromatography, a chromatographic column is a YMC-Triart C 18 column, the column temperature is 26-40 ℃, the flow rate is 1.05-1.5mL/min, a mobile phase A is acetonitrile, and a mobile phase B is phosphoric acid aqueous solution with the volume concentration of 0.06% -0.2%. In the present invention, the solvent in the sample solution may be methanol or an aqueous methanol solution, preferably an aqueous methanol solution. The volume percent of methanol in the aqueous methanol solution is preferably 60% to 80%, such as 70% or 75%. In the present invention, the mass volume of the powerful Madelbrueck preparation and the solvent in the test solution is preferably 1g (40-60) mL, for example 1g:45mL or 1g:50mL. In the invention, the sample solution can be prepared by a method conventional in the art, preferably by mixing the powerful Ma De-Gei Alite preparation with a solvent, performing ultrasonic treatment, cooling and filtering. Wherein the conditions of the sonication may be conventional in the art. The power of the sonication may be 200-300W, for example 250W. The frequency of the sonicat