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CN-121978228-A - Construction method of characteristic spectrum of Yunweiling or derivative product thereof

CN121978228ACN 121978228 ACN121978228 ACN 121978228ACN-121978228-A

Abstract

The invention belongs to the technical field of traditional Chinese medicine detection, and particularly relates to a method for constructing a characteristic spectrum of a Yunweiling or a derivative product thereof. The method for constructing the characteristic spectrum of the runwaline or the derivative thereof uses octadecylsilane chemically bonded silica as a filler, acetonitrile as a mobile phase A, one of an aqueous solution containing phosphoric acid, an aqueous solution containing formic acid and an aqueous solution containing glacial acetic acid as a mobile phase B, and obtains 9 common characteristic peaks through a specific gradient elution program, so that the effective separation of the common characteristic peaks is realized, the separation degree is good, the obtained characteristic spectrum has more characteristic peaks and better baseline separation, the positioning and qualitative analysis are easier, the precision, the stability and the repeatability are better, and the 1 characteristic component of the identified chlorogenic acid provides basis for the quality detection and the content measurement of the runwaline or the derivative thereof.

Inventors

  • ZHANG HUI
  • HUANG KAIWEI
  • SUN HAO
  • WEI JIABAO
  • WANG LIANG
  • HAN LING
  • TAN PEI
  • QIAN WEI
  • LI TAO

Assignees

  • 华润三九现代中药制药有限公司

Dates

Publication Date
20260505
Application Date
20251209

Claims (10)

  1. 1. The method for constructing the characteristic spectrum of the Yunweiling or the derivative thereof is characterized by comprising the steps of detecting by adopting a high performance liquid chromatography, wherein chromatographic conditions comprise: octadecylsilane chemically bonded silica is used as a filler, acetonitrile is used as a mobile phase A, taking one of an aqueous solution containing phosphoric acid, an aqueous solution containing formic acid and an aqueous solution containing glacial acetic acid as a mobile phase B, the gradient elution procedure included: 0-15 minutes, wherein the volume percentage of the mobile phase A is 5% -14%, and the volume percentage of the mobile phase B is 95% -86%; 15-25 minutes, wherein the volume percentage of the mobile phase A is 14% -20%, and the volume percentage of the mobile phase B is 86% -80%; 25-35 minutes, wherein the volume percentage of the mobile phase A is 20% -22%, and the volume percentage of the mobile phase B is 80% -78%; 35-45 minutes, the volume percentage of the mobile phase A is 22% -30%, and the volume percentage of the mobile phase B is 78% -70%.
  2. 2. The method of claim 1, wherein the chromatographic conditions comprise at least one of: (1) The detection wavelength is 325-329nm, preferably 327nm; (2) The flow rate is 0.20-0.30mL/min, preferably 0.2mL/min; (3) Column temperature is 20-30 ℃; (4) The sample injection amount is 1-5 mu L; (5) The mobile phase B is an aqueous solution containing phosphoric acid, preferably having a phosphoric acid concentration of 0.05-0.2% v/v, preferably having a phosphoric acid concentration of 0.1% v/v.
  3. 3. The construction method according to claim 1 or 2, further comprising the preparation of a test sample solution, comprising weighing the test sample, extracting with a solvent, separating solid from liquid, and obtaining the liquid as the test sample solution.
  4. 4. A method of constructing as claimed in claim 3 wherein the preparation of the test solution satisfies at least one of: A. The ratio of the mass of the test sample of the Yunweiling to the volume of the solvent is (0.2-1.0) (10-50), the unit of the mass of the test sample is g, and the unit of the volume of the solvent is mL; B. the extraction mode is ultrasonic extraction, heating reflux or oscillation extraction, preferably ultrasonic extraction; C. the extraction time is more than or equal to 20min; D. The solid-liquid separation is selected from filtration; E. the solvent is selected from one or more of methanol and water, preferably 50-100% v/v methanol water solution, preferably 70-90% v/v methanol water solution.
  5. 5. The method according to any one of claims 1 to 4, further comprising the steps of preparing a reference solution by adding a solvent to chlorogenic acid, and detecting the reference solution by high performance liquid chromatography in the method to obtain a reference map; Preferably, the concentration of chlorogenic acid reference substance in the chlorogenic acid reference substance solution is 10-40 mug/mL, preferably 10 mug/mL; Preferably, the solvent used in the preparation of the reference solution is selected from methanol or methanol aqueous solution with volume fraction not less than 50-100% v/v, more preferably, the solvent used in the preparation of the reference solution is selected from methanol aqueous solution with volume fraction not less than 80% v/v; Preferably, the construction method further comprises the steps of preparing a control medicinal material solution by adopting a runweiling control medicinal material, and detecting the control medicinal material solution according to the high performance liquid chromatography in the construction method to obtain a control medicinal material reference map.
  6. 6. The method of any one of claims 1-5, wherein the maverine or derivative thereof comprises one or more of maverine drug, maverine decoction pieces, or maverine formulations.
  7. 7. The construction method according to claim 6, wherein the Yunweiling preparation comprises at least one of Yunweiling decoction piece standard decoction and Yunweiling prescription granule, preferably the Yunweiling standard decoction comprises at least one of Yunweiling standard decoction concentrated extract, yunweiling standard decoction lyophilized powder and Yunweiling standard decoction water decoction.
  8. 8. The method for measuring the content of the active ingredients in the runweiling or the derivative thereof is characterized by comprising the following steps: taking a sample solution and a reference substance solution, and respectively adopting the high performance liquid chromatography detection in the method for constructing the characteristic spectrum of the Yunweiling or the derivative thereof in any one of claims 1-7; Wherein the reference substance comprises chlorogenic acid.
  9. 9. The quality detection method of the Yunweiling or the derivative products thereof is characterized by comprising the step of comparing the characteristic spectrum of the product to be detected with the characteristic spectrum of the Yunweiling or the derivative products thereof; the characteristic spectrum of the product to be detected is obtained by the construction method according to any one of claims 1 to 7; The characteristic spectrum of the yunweiling or the derivative thereof is selected from any one of the following (1) - (4): (1) The chlorogenic acid reference substance has 9 common characteristic peaks, wherein the peak corresponding to the chlorogenic acid reference substance reference peak is an S peak, the relative retention time of the peaks 2-9 and the S peak is within the range of +/-10% of a specified value, and the specified values of the peaks 2-9 are sequentially 1.102, 1.165, 2.821, 2.914, 3.110, 3.196, 3.501 and 5.052; (2) The chlorogenic acid reference peak has 9 common characteristic peaks, wherein 1 peak corresponds to the chlorogenic acid reference peak retention time, the peak corresponding to the chlorogenic acid reference peak is an S peak, the relative retention time of peaks 2-9 and the S peak is within the range of +/-10% of a specified value, and the specified values of peaks 2-9 are sequentially 1.102, 1.165, 2.821, 2.914, 3.110, 3.196, 3.501 and 5.052; (3) Using single-batch or multi-batch maverine and/or derivative products thereof as a sample according to the characteristic spectrum of Yun Weiling and/or preparation thereof obtained by the construction method of any one of claims 1-7; (4) The characteristic spectrum obtained by using a plurality of batches of runwaline and/or derivative products thereof as a test sample according to the construction method of any one of claims 1 to 7 is made into a control characteristic spectrum by means of average or median.
  10. 10. The method for detecting the quality of the yunweiling or its derivative products according to claim 9, wherein peak 1 (S) corresponds to chlorogenic acid.

Description

Construction method of characteristic spectrum of Yunweiling or derivative product thereof Technical Field The invention belongs to the technical field of traditional Chinese medicine detection, and particularly relates to a method for constructing a characteristic spectrum of a Yunweiling or a derivative product thereof. Background Yun Weiling is dried root and rhizome of Inulae flos (Inula nervosa wall. Ex. DC) belonging to Inulae genus of Compositae. At present, the quality report of the Yunweiling mainly refers to the content measurement of volatile oil components, and no related literature adopts other technical means such as characteristic patterns, thin layers and the like to establish a quality control method. How to improve the quality detection efficiency of the Yunweiling or the derivative products thereof and effectively control the quality of finished products is needed to be solved. Disclosure of Invention Therefore, the first object of the invention is to provide a method for constructing a characteristic spectrum of the Yunweiling or the derivative products thereof, which establishes the characteristic spectrum of the variety according to the characteristics of the Yunweiling or the derivative products thereof, has a plurality of characteristic peaks and high separation degree, has obvious characteristics and good precision, stability and repeatability, and can carry out overall quality control on the Yunweiling or the derivative products thereof. For this purpose, the invention provides the following technical scheme. The invention provides a method for constructing a characteristic spectrum of a Yunweiling or a derivative thereof, which comprises the steps of adopting a high performance liquid chromatography for detection, wherein chromatographic conditions comprise: octadecylsilane chemically bonded silica is used as a filler, acetonitrile is used as a mobile phase A, taking one of an aqueous solution containing phosphoric acid, an aqueous solution containing formic acid and an aqueous solution containing glacial acetic acid as a mobile phase B, the gradient elution procedure included: 0-15 minutes, wherein the volume percentage of the mobile phase A is 5% -14%, and the volume percentage of the mobile phase B is 95% -86%; 15-25 minutes, wherein the volume percentage of the mobile phase A is 14% -20%, and the volume percentage of the mobile phase B is 86% -80%; 25-35 minutes, wherein the volume percentage of the mobile phase A is 20% -22%, and the volume percentage of the mobile phase B is 80% -78%; 35-45 minutes, the volume percentage of the mobile phase A is 22% -30%, and the volume percentage of the mobile phase B is 78% -70%. In an alternative embodiment, the chromatographic conditions include at least one of: (1) The detection wavelength is 325-329nm, preferably 327nm; (2) The flow rate is 0.20-0.30mL/min, preferably 0.2mL/min; (3) Column temperature is 20-30 ℃; (4) The sample injection amount is 1-5 mu L; (5) The mobile phase B is an aqueous solution containing phosphoric acid, preferably having a phosphoric acid concentration of 0.05-0.2% v/v, preferably having a phosphoric acid concentration of 0.1% v/v. In an alternative embodiment, the method further comprises the steps of weighing the sample, adding a solvent for extraction, and performing solid-liquid separation to obtain a liquid, namely the sample solution. In an alternative embodiment, the preparation of the test solution satisfies at least one of the following: A. The ratio of the mass of the test sample of the Yunweiling to the volume of the solvent is (0.2-1.0) (10-50), the unit of the mass of the test sample is g, and the unit of the volume of the solvent is mL; B. the extraction mode is ultrasonic extraction, heating reflux or oscillation extraction, preferably ultrasonic extraction; C. the extraction time is more than or equal to 20min; D. The solid-liquid separation is selected from filtration; E. the solvent is selected from one or more of methanol and water, preferably 50-100% v/v methanol water solution, preferably 70-90% v/v methanol water solution. In an alternative embodiment, the construction method further comprises a step of preparing a reference substance solution by adding a solvent to chlorogenic acid, and a step of detecting the reference substance solution according to high performance liquid chromatography in the construction method to obtain a reference substance reference map; Preferably, the concentration of chlorogenic acid reference substance in the chlorogenic acid reference substance solution is 10-40 mug/mL, preferably 10 mug/mL; Preferably, the solvent used in the preparation of the reference solution is selected from methanol or methanol aqueous solution with volume fraction not less than 50-100% v/v, more preferably, the solvent used in the preparation of the reference solution is selected from methanol aqueous solution with volume fraction not less than 80% v/v; Preferably, the construction