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CN-121978232-A - Detection method of characteristic spectrum of ginger and licorice decoction

CN121978232ACN 121978232 ACN121978232 ACN 121978232ACN-121978232-A

Abstract

The invention belongs to the field of traditional Chinese medicine detection, and particularly relates to a detection method of a characteristic spectrum of ginger and licorice decoction. The detection method specifically comprises the following steps of a, preparing a reference substance solution, b, preparing a sample solution, c, respectively sucking the reference substance solution and the sample solution, and injecting the reference substance solution and the sample solution into a liquid chromatograph for gradient elution. According to the invention, through the cooperation of specific sample solvents and chromatographic conditions, the chromatographic peak separation degree in the characteristic spectrum is high, the number of calibrated common peaks is large, the characteristic is strong, the chemical quality profile of the classical name ginger licorice decoction can be accurately, comprehensively and stably reflected, the quality control of the traditional preparation and the modern preparation of the ginger licorice decoction is realized, and the popularization and application values are provided.

Inventors

  • ZHOU HOUCHENG
  • ZHOU JINGWEI
  • WU QIN
  • LIN XIAOYAN
  • DENG YUE
  • HUANG YU
  • CHEN LONGHU
  • HU QING

Assignees

  • 四川新绿色药业科技发展有限公司

Dates

Publication Date
20260505
Application Date
20251219

Claims (10)

  1. 1. A detection method of a characteristic spectrum of ginger and licorice decoction is characterized by adopting HPLC detection, and specifically comprises the following steps: a. preparing reference solution by dissolving reference substance in methanol; b. Preparing test solution by extracting sample with methanol solution, filtering, and collecting filtrate; c. Respectively sucking the reference solution and the sample solution, and injecting into a liquid chromatograph under chromatographic conditions that a chromatographic column takes octadecylsilane chemically bonded silica as a filler, a mobile phase takes acetonitrile as a mobile phase A, 0.1% phosphoric acid solution as a mobile phase B, the flow rate is 0.9ml per minute, the column temperature is 25 ℃, and the gradient elution procedure is as follows: the reference substance comprises glycyrrhizin; the sample to be tested is a preparation of ginger and licorice soup; The ginger and licorice decoction consists of ginger, licorice, ginseng and jujube in a mass ratio of 65-70:50-58:40-45:30-38.
  2. 2. The method according to claim 1, wherein the reference substance further comprises isoliquiritigenin, liquiritigenin, apioside, monoammonium glycyrrhizinate and/or 6-gingerol.
  3. 3. The method according to claim 1, wherein the preparation of the ginger decoction comprises ginger decoction Shang Shangji, ginger decoction granule, ginger decoction Shang Fenji, ginger decoction Shang Wanji, ginger decoction Shang Pianji, and ginger decoction.
  4. 4. The method according to claim 1 or 3, wherein the ginger and licorice soup comprises ginger, licorice, ginseng and jujube in a mass ratio of 69:55.2:41.4:36.
  5. 5. The method according to claim 1, wherein the concentration of the reference solution in the step a) is 100-150. Mu.g per 1ml of the reference solution.
  6. 6. The detection method according to claim 1, wherein the mass volume ratio of the sample to be detected to the methanol solution in the step b) is 0.1-1 g/10 mL, and the extraction is ultrasonic extraction with power of 600w, frequency of 40kHz and time of 30min.
  7. 7. The method according to claim 1 or 6, wherein the concentration of the methanol solution is 70%.
  8. 8. The detection method according to claim 1, wherein in the step c), the chromatographic column is ZORBAX SB-Aq 4.6X150 mm 3.5 μm, the wavelength of the chromatographic condition is 230nm, the sample injection amount is 5. Mu.l, and the theoretical plate number is not less than 5000 calculated by glycyrrhizin.
  9. 9. The detection method according to claim 1, wherein the characteristic spectrum of the ginger decoction of licorice root is characterized in that 12 characteristic peaks are represented, the peak corresponding to the glycyrrhizin reference is S peak, the relative retention time of the remaining characteristic peaks and S peak is calculated to be within + -10% of a specified value, and the specified value is 1:0.346, 2:0.571, 3:0.781, 4:0.979, 6:1.118, 7:1.158, 8:1.187, 9:1.312, 10:1.455, 11:1.574, and 12:1.617.
  10. 10. The method according to claim 9, wherein the peak 7 is apigenin, the peak 8 is isoliquiritigenin, the peak 9 is glycyrrhizin, the peak 11 is monoammonium glycyrrhizinate, and the peak 12 is 6-gingerol.

Description

Detection method of characteristic spectrum of ginger and licorice decoction Technical Field The invention belongs to the field of traditional Chinese medicine detection, and particularly relates to a detection method of a characteristic spectrum of ginger and licorice decoction. Background Ginger and licorice decoction is from Tang, sunshiji Fang (great many important prescriptions), and is recorded in the original text as "treating consumptive lung disease, cough, saliva and foam, dry throat and thirst". The traditional Chinese medicine composition is applied to lung fibrosis or lung atelectasis diseases caused by lung cancer or lung injury diseases such as emphysema, bronchitis and the like in the later period. The research and development technical difficulty of modern preparation of ginger and licorice decoction is in the ancient and modern preparation equivalence evaluation system. Because the raw materials, the processing and extracting processes of the raw materials and the preparation process of the modern preparation of the classical prescription have influence on the quality of the final product, and the quality of the final product is difficult to reflect by the simple qualitative identification of index components, in order to ensure the safety, the effectiveness, the stability and the controllability of the classical prescription and the preparation thereof, the whole chemical spectrum which reflects the composition of the classical prescription more stably and comprehensively is required to be used as an effective means for controlling and evaluating the preparation of the classical prescription and the preparation of the classical prescription. However, at present, no method for performing quality control evaluation on the traditional preparation of the ginger decoction of liquorice and performing overall quality control on the modern preparation of the ginger decoction of liquorice is available. Disclosure of Invention In order to solve the problems, the invention provides a detection method of a characteristic spectrum of ginger and licorice decoction, which adopts HPLC detection and specifically comprises the following steps: a. preparing reference solution by dissolving reference substance in methanol; b. Preparing test solution by extracting sample with methanol solution, filtering, and collecting filtrate; c. Respectively sucking the reference solution and the sample solution, and injecting into a liquid chromatograph under chromatographic conditions that a chromatographic column takes octadecylsilane chemically bonded silica as a filler, a mobile phase takes acetonitrile as a mobile phase A, 0.1% phosphoric acid solution as a mobile phase B, the flow rate is 0.9ml per minute, the column temperature is 25 ℃, and the gradient elution procedure is as follows: the reference substance comprises glycyrrhizin; the sample to be tested is a preparation of ginger and licorice soup; The ginger and licorice decoction consists of ginger, licorice, ginseng and jujube in a mass ratio of 65-70:50-58:40-45:30-38. Further, the reference substance further comprises isoliquiritigenin, glycyrrhizin, apiose isoliquiritigenin, monoammonium glycyrrhizinate and/or 6-gingerol. Further, the preparation of the ginger decoction comprises ginger decoction Shang Shangji, ginger decoction granules, ginger decoction Shang Fenji, ginger decoction Shang Wanji, ginger decoction Shang Pianji and a ginger decoction substance standard; further, the ginger and licorice decoction consists of ginger, licorice, ginseng and jujube in a mass ratio of 69:55.2:41.4:36. Further, the concentration of the reference substance solution in the step a) is 100-150 mug of the reference substance per 1 ml. Further, the mass volume ratio of the sample to be detected to the methanol solution in the step b) is 0.1-1 g/10 mL, the extraction is ultrasonic extraction, the power is 600w, the frequency is 40kHz, and the time is 30min. Still further, the concentration of the methanol solution was 70%. Further, in the step c), the chromatographic column is ZORBAX SB-Aq 4.6X150 mm 3.5 μm, the wavelength of the chromatographic condition is 230nm, the sample injection amount is 5 μl, and the theoretical plate number is not less than 5000 calculated by glycyrrhizin. Further, the characteristic spectrum of the ginger and licorice decoction should show 12 characteristic peaks, the peak corresponding to the glycyrrhizin reference substance is an S peak, the relative retention time of the other characteristic peaks and the S peak is calculated, the relative retention time is within +/-10% of a specified value, and the specified value is 1:0.346, 2:0.571, 3:0.781, 4:0.979, 6:1.118, 7:1.158, 8:1.187, 9:1.312, 10:1.455, 11:1.574 and 12:1.617; The peak 7 is apigenin, the peak 8 is isoliquiritigenin, the peak 9 is glycyrrhizin, the peak 11 is monoammonium glycyrrhizinate, and the peak 12 is 6-gingerol. According to the detection method of the characteristic spect