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CN-121994986-A - Identification method of qingning powder target component

CN121994986ACN 121994986 ACN121994986 ACN 121994986ACN-121994986-A

Abstract

The invention discloses an identification method of a qingning powder target component, which comprises the following steps of firstly, from a microscopic identification level, ensuring that a finished product contains three medicinal materials such as honey mulberry bark, wine fried red poria cocos, fried semen lepidii and the like, secondly, taking 1-2g of the product, adding an extraction solvent, selecting a corresponding extraction method, filtering, evaporating filtrate, adding 1-2ml of a dissolving agent into residues to dissolve the residues to serve as a sample solution, taking a reference medicinal material, preparing the reference medicinal material solution by using the same method as the second step, sucking 1-5ul of the sample solution and 1-5ul of the reference medicinal material solution according to a thin layer chromatography test, and respectively spotting the sample solution and the reference medicinal material solution on the same stationary phase.

Inventors

  • ZHAO KUN
  • YIN JIAJUN
  • SU JIE
  • YANG JUAN

Assignees

  • 河南省新四方制药有限公司

Dates

Publication Date
20260508
Application Date
20260129

Claims (9)

  1. 1. The identification method of the qingning powder target component is characterized by comprising the following steps of; Step one, ensuring that the finished product contains three medicinal materials of honey mulberry bark, red poria fried with wine, fried pepperweed seed and the like from the microscopic identification level; Step two, 1 to 2g of the product is taken, a corresponding extraction method is selected, the product is filtered, the filtrate is evaporated to dryness, 1 to 2ml of a dissolving agent is added into residues to be dissolved to serve as a sample solution, a reference medicinal material is taken, the reference medicinal material solution is prepared by adopting a method similar to the step two, 1 to 5ul of the sample solution and 1 to 5ul of the reference medicinal material solution are respectively spotted on the same stationary phase according to a thin layer chromatography test, then a corresponding developing agent is selected, developed, taken out and dried, a positioning reagent is sprayed, the product is heated to 105 ℃ until the color of spots is clear, and then the product is inspected according to a corresponding detection mode, and main spots with the same color are displayed on the positions corresponding to the reference medicinal material chromatogram in the sample chromatogram.
  2. 2. The method for identifying the target components of qingning powder according to claim 1, wherein 1G of the product is taken, 25ml of methanol is added, ultrasonic treatment is carried out for 30 minutes, filtration is carried out, filtrate is evaporated to dryness, 2ml of methanol is added to residues to be dissolved to be used as a sample solution, 1G of white mulberry root-bark reference medicinal material is taken, the reference medicinal material solution is prepared by the same method, the thin layer chromatography test is carried out, 4ul of each of the two solutions is absorbed, the two solutions are respectively spotted on the same silica gel G thin layer plate, petroleum ether (60-90 ℃) and toluene-chloroform (2:1:2) are used as developing agents, the developing agent is taken out, the solution is dried, 5% vanillin sulfuric acid solution is sprayed, 105 ℃ is heated to have clear color development of spots, and main spots with the same color are displayed on the positions corresponding to the reference medicinal material chromatogram in the sample chromatogram.
  3. 3. The method for identifying the target components of qingning powder according to claim 1, wherein 1g of the product is taken, 20ml of 70% methanol is added, heating reflux is carried out for 1 hour, filtering is carried out, filtrate is evaporated to dryness, 2ml of methanol is added into residues to dissolve the residues to be used as a sample solution, a quercetin-3-O-B-D-glucose-7-O-beta-D-gentiobioside reference substance is additionally taken, 70% methanol is added to prepare a solution with 90 mu g of each 1ml of the solution to be used as a reference substance solution, 1 mu l of each of the two solutions is absorbed according to a thin layer chromatography test, the two solutions are respectively sprayed on the same polyamide film, ethyl acetate-methanol-water (7:4:1) is used as a developing agent, the developing solution is taken out, airing is carried out, a 2% aluminum trichloride ethanol solution is sprayed, the same hot air is heated to have the same fluorescent spots, and the heating temperature range during heating reflux is 80-100 ℃.
  4. 4. The method for identifying the target components of qingning powder according to claim 1, wherein 1G of the product is taken, 50ml of diethyl ether is added, ultrasonic treatment is carried out for 10 minutes, filtration is carried out, filtrate is evaporated to dryness, 1ml of methanol is added into residues to be dissolved, 1G of poria cocos reference medicine is taken, the reference medicine solution is prepared by the same method, 4ul of the reference medicine solution and 3 ul of the reference medicine solution are absorbed by the thin layer chromatography test, the sample solution and the reference medicine solution are respectively spotted on the same silica gel G thin layer plate, toluene-ethyl acetate-formic acid (20:5:0.5) are taken as developing agents, the developing agent is taken out, dried in the air, a 2% vanillin sulfuric acid solution-ethanol (4:1) mixed solution is sprayed, and spots are heated at 105' C until the color of the spots are clear, and spots with the same color are displayed at the positions corresponding to the chromatogram of the reference medicine.
  5. 5. The method for identifying a target component of qingning powder as claimed in claim 1, wherein the stationary phase can be a silica gel GF1sa thin layer plate and a silica gel G thin layer plate prepared by using a 1% sodium hydroxide solution.
  6. 6. The method for identifying a target component of qingning powder as claimed in claim 1, wherein the developing agent is selected from toluene-ethyl acetate-formic acid (20:5:0.5), ethyl acetate-methanol-formic acid-water (18:2:15:1) and chloroform-methanol-water (13:7:2) under-layer solutions.
  7. 7. The method for identifying a target component of qingning powder as claimed in claim 1, wherein the detection mode is selected from ultraviolet light (254 nm) detection and sunlight and ultraviolet 365nm detection.
  8. 8. The method for identifying the target components of qingning powder according to claim 1, wherein the product is prepared by mixing and crushing 222.42g of white mulberry root-bark, 222.42g of wine-fried red poria cocos, 110.32g of fried licorice root, 222.42g of fried palmate and 222.42g of fried plantain seed into the most fine powder, sieving, uniformly mixing, carrying out high-temperature instantaneous sterilization, wherein the sterilization temperature is 160-180 ℃, the sterilization time is 7-10 s, sieving, and uniformly mixing.
  9. 9. The method for identifying a target component of qingning powder according to claim 1, wherein the product is light brown to brown powder, has slight fragrance, and has slightly bitter and slightly sweet taste.

Description

Identification method of qingning powder target component Technical Field The invention relates to the technical field of medicine identification, in particular to a method for identifying target components of qingning powder. Background The Qingning powder is a Chinese medicinal compound preparation (different documents describe the composition, common components contain rhubarb, baikal skullcap root, bitter orange, magnolia bark, dried orange peel and the like), the identification of the target components of the Qingning powder is to confirm the existence and content of characteristic components in the compound by modern analysis technology, thereby guaranteeing the authenticity, purity and curative effect stability of the preparation, in the prior art, the patent of the authorized publication number CN 113010613A discloses a multi-dimensional intelligent identification system and method for checking foods and medicines, comprising a terminal system, a communication system and a cloud computing service system, wherein the terminal system mainly comprises a high-definition camera and an infrared spectrometer, and is used for scanning images of biological characteristics of the checked foods and medicines and the spectrum of the components, and detecting the components in the foods or medicines by the communication system and the cloud computing service system, but the infrared spectrometer obtains a vibration absorption spectrum of molecular chemical bonds and functional groups, and for complex mixtures (such as Chinese medicines and compound foods), the spectrum is superposition of signals of all the components, thus the identification effect can be influenced, and the infrared signal strength is related to the content of the components, if the characteristic components are very low in content (such as 1 percent, the main component is submerged out, the main component is completely) and the identification signal of the starch is completely lost. Disclosure of Invention The invention aims to overcome the existing defects, provides a method for identifying the target components of qingning powder, carries out identification by adopting a thin layer chromatography without complex data processing, can directly visually compare spots of a sample and a reference substance in the same position and the same color/fluorescence, can visually and specifically confirm the existence of one or more characteristic components, realizes the physical separation of the components in the identification process, avoids the interference of mixture signal superposition in the spectrometry, can clearly distinguish different components in complex samples, and can effectively solve the problems in the background technology. In order to achieve the aim, the invention provides the following technical scheme that the identification method of the qingning powder target component comprises the following steps of; Step one, ensuring that the finished product contains three medicinal materials of honey mulberry bark, red poria fried with wine, fried pepperweed seed and the like from the microscopic identification level; Step two, 1-2g of the sample is taken, a corresponding extraction method is selected, filtration is carried out, filtrate is evaporated, 1-2ml of dissolving agent is added into residues to be dissolved to serve as a sample solution, a control medicinal material is taken, the control medicinal material solution is prepared by a method which is the same as that of the step two, 1-5ul of the sample solution and 1-5ul of the control medicinal material solution are respectively spotted on the same stationary phase according to a thin layer chromatography test, then the corresponding developing agent is selected, developed, taken out and dried, sprayed with a positioning reagent, heated to 105 ℃ until the color of spots is clear, and then the spots are inspected according to a corresponding detection mode, main spots with the same color are displayed on the positions corresponding to the control medicinal material chromatogram in the sample chromatogram, identification is carried out through the thin layer chromatography, complex data processing is not needed, the existence of certain characteristic components or the spots with the same color or the same fluorescent color can be directly visually compared with the sample at the same positions, physical separation of the components is realized in the identification process, and different groups of the mixed signal superimposed spectrum can be clearly distinguished in a complex manner. Further, 1G of the product is taken, 25ml of methanol is added, ultrasonic treatment is carried out for 30 minutes, filtration is carried out, filtrate is evaporated, 2ml of methanol is added to residues for dissolution to be used as a sample solution, 1G of white mulberry root bark reference medicine is taken, the same method is adopted to prepare reference medicine solutions, the two solutions ar