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CN-122017050-A - Quality detection method and application of moldavica dragonhead formula particles

CN122017050ACN 122017050 ACN122017050 ACN 122017050ACN-122017050-A

Abstract

The invention discloses a quality detection method and application of moldavica dragonhead formula particles. The quality detection method of the moldavica dragonhead formula particles comprises the following steps of carrying out gradient elution and separation on a to-be-detected solution of a to-be-detected sample solution 1 containing moldavica dragonhead formula particles through a high performance liquid chromatography, wherein a mobile phase A is methanol, a mobile phase B is a phosphoric acid aqueous solution, and the column temperature of a chromatographic column is 30-40 ℃. The method fills the blank of the quality standard research of the method in the prior art, and the constructed method can be used for rapidly and comprehensively controlling the quality of the moldavica dragonhead formula particles.

Inventors

  • YIN QIANG
  • CUI YUANFENG
  • CHEN JING
  • YIN HAILONG
  • MU DANDAN
  • SHI FENG
  • MA XIAOYAN
  • Du Mengge
  • LI CHAOJIE
  • JIN CAINA
  • SONG FEI

Assignees

  • 新疆维吾尔药业有限责任公司

Dates

Publication Date
20260512
Application Date
20241111

Claims (10)

  1. 1. A quality detection method of moldavica dragonhead formula particles is characterized by comprising the following steps of carrying out gradient elution and separation on a sample solution 1 containing moldavica dragonhead formula particles by a high performance liquid chromatography; in the high performance liquid chromatography, the mobile phase A is methanol, the mobile phase B is phosphoric acid aqueous solution, and the column temperature of the chromatographic column is 30-40 ℃.
  2. 2. The method for detecting the quality of moldavica dragonhead formula particles according to claim 1, wherein the method for detecting the quality of moldavica dragonhead formula particles satisfies one or more of the following conditions: (1) The moldavica dragonhead formula particles comprise tilianin and/or rosmarinic acid; (2) The preparation method of the sample solution 1 containing the moldavica dragonhead formula particles comprises the following steps of extracting and processing a mixed solution comprising the moldavica dragonhead formula particles and a solvent, and filtering to obtain a filtrate serving as the sample solution 1; (3) In the high performance liquid chromatography, preparing a reference substance solution 1 and a reference substance reference solution 1; (4) In the high performance liquid chromatography, the volume percentage of phosphoric acid in the phosphoric acid aqueous solution is 0.1% -0.5%, such as 0.2%, 0.3% or 0.4%; (5) In the high performance liquid chromatography, the column temperature of the chromatographic column is 32-38 ℃, such as 35 ℃; (6) In the high performance liquid chromatography, the flow rate of the mobile phase is 0.3-1.0mL/min, preferably 0.5-0.8mL/min, such as 0.6mL/min; (7) In the high performance liquid chromatography, the sample injection amount is 10-20. Mu.L, for example 15. Mu.L, and, (8) In the high performance liquid chromatography, the detection wavelength is 200-400nm, such as 328nm.
  3. 3. The method for detecting the quality of moldavica dragonhead formula particles according to claim 1, wherein in the high performance liquid chromatography, gradient elution is as follows: 、 、 Or alternatively Wherein, the percentages in the table are the volume percentages of each component in the total volume of the mobile phase A and the mobile phase B respectively.
  4. 4. The method for detecting the quality of moldavica dragonhead formula particles according to claim 2, wherein the method for detecting the quality of moldavica dragonhead formula particles satisfies one or more of the following conditions: (1) In the preparation method of the sample solution 1, the particle size of the moldavica dragonhead formula particles is that the moldavica dragonhead formula particles are sieved by a No. 6 sieve; (2) In the preparation method of the sample solution 1, the solvent is methanol and/or ethanol water solution, wherein the volume percentage of the ethanol in the ethanol water solution is preferably 40-80%, such as 70%; (3) In the preparation method of the test solution 1, the mass volume ratio of the moldavica dragonhead formula particles to the solvent is 0.6g (10-80) mL, preferably 0.6g (20-70) mL, for example 0.6g:40mL or 0.6g:50mL; (4) In the preparation method of the sample solution 1, the extraction treatment mode is ultrasonic treatment or reflux treatment, and, (5) In the method for producing the sample solution 1, the extraction treatment time is 0.2 to 2 hours, preferably 0.5 to 1.5 hours, for example 1 hour.
  5. 5. The method for detecting the quality of moldavica dragonhead formula particles according to claim 2, wherein the method for detecting the quality of moldavica dragonhead formula particles satisfies one or more of the following conditions: (1) The reference substance solution 1 comprises a reference substance 1 and a solvent, wherein the reference substance 1 is cynarin and/or rosmarinic acid, the solvent is preferably methanol and/or ethanol water solution, and the ethanol water solution is preferably 40-80% by volume, such as 70%; Wherein, when the reference substance 1 comprises the thistle glycoside, the mass concentration of the thistle glycoside in the reference substance solution 1 is preferably 40-70 mug/mL, such as 60 mug/mL; When the reference substance 1 comprises rosmarinic acid, the mass concentration of rosmarinic acid in the reference substance solution 1 is preferably 100-130 μg/mL, for example 120 μg/mL; (2) The preparation method of the reference solution 1 comprises extracting the mixed solution of the reference solution 1 and solvent, filtering, and collecting filtrate as reference solution 1; Wherein, in the reference solution 1 of the reference medicinal material, the solvent is preferably methanol and/or ethanol water solution, and the volume percentage of the ethanol in the ethanol water solution is preferably 40-80%, such as 70%; Wherein the mass volume ratio of the control medicinal material 1 to the solvent is preferably 0.5g (10-30) mL, for example 0.5g:20mL; Wherein, the extraction treatment mode is preferably ultrasonic treatment or reflux treatment; Wherein the time of the extraction treatment is preferably 0.5 to 1.5 hours, for example 1 hour.
  6. 6. The quality detection method of moldavica dragonhead formula particles according to claim 1, wherein the fingerprint obtained after the sample solution 1 of moldavica dragonhead formula particles is subjected to gradient elution and separation by a high performance liquid chromatography method comprises 2 characteristic peaks, and the average relative retention time of each characteristic peak is as follows: peak 4 is rosmarinic acid with average relative retention time of 0.558 and RSD of 0.05%; Preferably, the fingerprint obtained by gradient elution and separation of the sample solution 1 of the moldavica dragonhead formula particle by a high performance liquid chromatography method comprises 9 characteristic peaks, wherein the peak of the field thrips is taken as a reference peak, and the average relative retention time of each characteristic peak is respectively as follows: the average relative retention time of peak 1 was 0.348, rsd was 0.02%; the average relative retention time of peak 2 was 0.383 and rsd was 0.03%; peak 3 has an average relative retention time of 0.498 and rsd of 0.03%; peak 4 is rosmarinic acid with average relative retention time of 0.558 and RSD of 0.05%; peak 5 had an average relative retention time of 0.619 and rsd of 0.04%; Peak 6 had an average relative retention time of 0.647 and rsd of 0.04%; Peak 7 has an average relative retention time of 0.739 and rsd of 0.04%; The average relative retention time of peak 9 was 1.017 and rsd was 0.02%.
  7. 7. The method for detecting the quality of moldavica dragonhead formula particles according to claim 1, wherein the method for detecting the quality of moldavica dragonhead formula particles satisfies (1) and/or (2) in the following steps: (1) Detecting the sample solution 2 containing the moldavica dragonhead formula particles by adopting a thin-layer chromatography; (2) And detecting the content of the cynara scolymus glucoside in the test solution 3 of the vanilla prescription granule by adopting a high performance liquid chromatography method.
  8. 8. The method for detecting the quality of the moldavica dragonhead formula particles according to claim 7, wherein the method for detecting the quality of the moldavica dragonhead formula particles satisfies one or more of the following conditions, (1) In the step (1), the preparation method of the sample solution 2 containing the moldavica dragonhead formula particles comprises the following steps of carrying out ultrasonic treatment, filtering and drying on the moldavica dragonhead formula particle solution to obtain residues, wherein the solution of the residues is the sample solution 2; In the step (1), the solvent 2-1 is preferably methanol and/or ethanol water solution, and the volume percentage of the ethanol in the ethanol water solution is preferably 40% -80%, such as 70%; Wherein in the step (1), the mass-volume ratio of the moldavica dragonhead formula particles to the solvent 2-1 in the moldavica dragonhead formula particle solution is preferably 5g (40-60) mL, such as 5g:50mL; wherein in step (1), the time of the ultrasonic treatment is preferably 5 to 30min, for example, 10min; Wherein in the step (1), the type of the solvent 2-2 in the solution of the residue is preferably consistent with the type of the solvent 2-1, and the volume ratio of the solvent 2-1 to the solvent 2-2 is preferably (4-6): 1, for example, 5:1; (2) In the step (1), the preparation of a reference substance solution 2 and a reference medicinal material reference solution 2 is also carried out; in the step (1), the reference substance solution 2 preferably comprises a reference substance 2 and a solvent, wherein the reference substance 2 is preferably thrips in the field, the solvent is preferably methanol and/or ethanol water solution, and the volume percentage of the ethanol in the ethanol water solution is preferably 40% -80%, for example 70%; Wherein, in the step (1), when the reference substance 2 comprises the thistle glycoside, the mass concentration of the thistle glycoside in the reference substance solution 2 is preferably 0.1-0.3mg/mL, such as 0.2mg/mL; In the step (1), the preparation method of the reference solution 2 for the reference medicinal material preferably comprises the following steps of carrying out ultrasonic treatment, filtering and drying on a solution containing the reference medicinal material 2 and a solvent 2-3 to obtain residues, wherein the solution of the residues and the solvent 2-4 is the reference solution 2 for the reference medicinal material; in the step (1), the solvent 2-3 is preferably methanol and/or ethanol water solution in the solution containing the reference medicinal material 2 and the solvent 2-3, wherein the volume percentage of the ethanol in the ethanol water solution is preferably 40% -80%, for example 70%; wherein in the step (1), the mass-volume ratio of the control medicinal material 2 to the solvent 2-3 in the solution containing the control medicinal material 2 and the solvent 2-3 is preferably 1g (40-60) mL, for example, 1g:50mL; wherein in step (1), the time of the ultrasonic treatment is preferably 5 to 30min, for example, 10min; Wherein in the step (1), the type of the solvent 2-4 is preferably consistent with the type of the solvent 2-3 in the solution of the residue and the solvent 2-4, and the volume ratio of the solvent 2-3 to the solvent 2-4 is preferably (4-6): 1, for example, 5:1; (3) In the step (1), the thin layer chromatography comprises the steps of respectively dispensing the sample solution 2, the reference solution 2 for reference medicinal materials and the reference solution 2 for reference medicinal materials on the same silica gel thin layer plate, spreading, taking out, airing, and inspecting under ultraviolet lamp; Wherein in the step (1), the sample application amounts of the sample solution 2, the reference solution 2 for reference medicinal material and the reference solution 2 for reference medicinal material in the thin layer chromatography are each independently preferably 1 to 10. Mu.L, more preferably 2 to 5. Mu.L, for example 3 or 4. Mu.L; wherein in step (1), the wavelength of the test in the thin layer chromatography is preferably at the ultraviolet wavelength, for example, 254nm or 365 nm; wherein in the step (1), in the thin layer chromatography, a 5% aluminum trichloride ethanol solution is preferably sprayed during the detection; Wherein in the step (1), the silica gel thin layer plate is preferably H plate, GF254 or G plate, such as G plate; wherein in the step (1), the developing agent used in the thin layer chromatography is preferably an aqueous solution of ethyl acetate and formic acid or an aqueous solution of ethyl acetate, formic acid and toluene; When the developing agent used is an aqueous solution of ethyl acetate and formic acid, the volume ratio of ethyl acetate, formic acid and water is preferably (6-10): 1 (5-7), e.g. 8:0.5:3; When the developing agent used is an aqueous solution of ethyl acetate, toluene and formic acid, the volume ratio of ethyl acetate, toluene, formic acid and water is preferably (14-17): (0.5-2.5): 1 (0.5-0.7), for example 16:2:1:0.6 or 16:0.6:1:0.6; wherein in step (1), the temperature of the development in the thin layer chromatography is preferably 10-40 ℃, such as 25 ℃; Wherein in step (1), the humidity of the development in the thin layer chromatography is preferably 10% -90%, for example 40%.
  9. 9. The method for detecting the quality of moldavica dragonhead formula particles according to claim 7, wherein the method for detecting the quality of moldavica dragonhead formula particles satisfies one or more of the following conditions: (1) In the step (2), the preparation method of the sample solution 3 containing the moldavica dragonhead formula particles comprises the following steps of extracting and treating the moldavica dragonhead formula particle solution, and filtering to obtain filtrate serving as the sample solution 3; Wherein in the step (2), the solvent 3-1 is preferably methanol, ethanol aqueous solution or methanol aqueous solution, wherein in the ethanol aqueous solution, the volume percentage of the ethanol is preferably 40% -80%, such as 70%, and the volume percentage of the methanol is preferably 40% -80%, such as 70%; wherein in the step (2), the mass-volume ratio of the moldavica dragonhead formula particles to the solvent 3-1 is preferably 0.3g (20-110) mL, more preferably 0.3g (25-100) mL, such as 0.3g:50mL or 0.3g:80mL; in the step (2), the extraction treatment is preferably ultrasonic treatment or reflux treatment; wherein in the step (2), the time of the extraction treatment is preferably 10 to 30min, for example, 20min; (2) In the step (2), a reference substance solution 3 and a reference medicinal material reference solution 3 are also prepared; In the step (2), the reference substance solution 3 preferably comprises a general reference substance 3 and a solvent 3-2, wherein the reference substance 3 is preferably thrips in the field, the solvent 3-2 is preferably methanol, an ethanol aqueous solution or a methanol aqueous solution, the volume percentage of the ethanol in the ethanol aqueous solution is preferably 40% -80%, for example 70%, and the volume percentage of the methanol in the methanol aqueous solution is preferably 40% -80%, for example 70%; When the reference substance 3 is thistle glycoside, the mass concentration of thistle glycoside in the reference substance solution 3 is preferably 20-30 mug/mL, such as 26 mug/mL; (3) In the step (2), in the high performance liquid chromatography, the mobile phase A is acetonitrile; (4) In the step (2), the mobile phase B is phosphoric acid aqueous solution, and the volume percentage of phosphoric acid in the phosphoric acid aqueous solution is preferably 0.1% -0.5%, such as 0.2%, 0.3% or 0.4%; (5) In the step (2), the volume ratio of the mobile phase A to the mobile phase B in the high performance liquid chromatography is (20-25): (75-80), such as 22:78, 23:77, 25:75 or 20:80; (6) In the step (2), the detection wavelength in the high performance liquid chromatography is 200-400nm, for example 333nm; (7) In the step (2), in the high performance liquid chromatography, the column temperature of the chromatographic column is 25-40 ℃, such as 30 ℃; (8) In the step (2), the flow rate of the mobile phase in the high performance liquid chromatography is 0.5-2mL/min, for example 1.0mL/min, and, (9) In the step (2), the sample injection amount in the high performance liquid chromatography is 10-20 μl, for example 15 μl.
  10. 10. Use of a quality detection method of moldavica dragonhead formula particles as defined in any one of claims 1-9 for evaluating and/or controlling the quality thereof.

Description

Quality detection method and application of moldavica dragonhead formula particles Technical Field The invention relates to the technical field of medicine quality control, in particular to a detection method and application for comprehensively controlling the quality of moldavica dragonhead formula particles. Background The moldavica dragonhead medicinal material is the dry overground part of moldavica dragonhead (Dracocephalum moldavica L.) of Labiatae, is cut in the full bloom stage in summer, is removed with impurities, is dried in the sun, is cultivated in Xinjiang all places at present, has the property II-level dry heat, and has the main functions of tonifying heart, protecting brain, protecting liver, invigorating stomach, enhancing sensory power, supplementing protective power, filling intelligence and activating brain occlusion. Can be used for treating palpitation, heart pain, dizziness, slow reaction, hypoesthesia, weak mind, stomach deficiency, liver weakness, and physical weakness. Modern medicines have three characteristics of stability, uniformity, safety and effectiveness, and for Chinese patent medicines, various means are needed for detection, so that the reliability and stability of detection results are ensured. The traditional Chinese medicine formula particles are single traditional Chinese medicine products prepared by adopting modern scientific technology and imitating the traditional Chinese medicine decoction, and the traditional Chinese medicine decoction pieces are refined by the processes of leaching, concentrating, drying and the like, so that the traditional Chinese medicine decoction pieces maintain the property, taste and efficacy of the traditional Chinese medicine decoction pieces, have stable quality, are applied to the preparation of clinical prescriptions of the traditional Chinese medicine, adapt to the needs of dialectical treatment and prescription change, and have the advantages of no need of decoction, convenient administration, quick absorption, accurate dosage, safety, cleanness, convenient carrying and the like. Compared with the traditional medicinal materials, the morphological characteristics of the formula particles are obviously changed, and the authenticity and quality of the product cannot be obtained by naked eye observation. Therefore, it is necessary to establish a quality evaluation system of the traditional Chinese medicine formula particles so as to comprehensively reflect the inherent quality of the formula particles. Regarding the quality control means of the moldavica dragonhead medicinal material, the property, the cross section, the powder microscopic identification, the thin layer chromatography and the content measurement method are adopted in the published revised draft of the national formulary committee. At present, no manufacturer produces the moldavica dragonhead formula particles in the market, and the quality standard of the moldavica dragonhead formula particles is not disclosed in the prior patent literature data. The earlier application patent CN202211559765.X of the company discloses a preparation method of the moldavica dragonhead formula particle, but a systematic quality detection method is not formed for the moldavica dragonhead formula particle, and the conventional medicinal material quality detection means are only adopted to detect the formula particle, so that the whole internal quality of the moldavica dragonhead formula particle cannot be reflected, and the quality control requirement of the traditional Chinese medicine formula particle cannot be met. Disclosure of Invention The invention aims to overcome the defect that a quality detection method of a moldavica dragonhead formula particle is lacked in the prior art, and provides a quality detection method and application of the moldavica dragonhead formula particle. The method fills the blank of the quality standard research of the method in the prior art, and the constructed method can be used for rapidly and comprehensively controlling the quality of the moldavica dragonhead formula particles. The invention adopts the following technical proposal to solve the technical problems. The invention provides a quality detection method of moldavica dragonhead formula particles, which comprises the following steps of carrying out gradient elution and separation on a solution to be detected of a sample solution 1 containing moldavica dragonhead formula particles by a high performance liquid chromatography; in the high performance liquid chromatography, the mobile phase A is methanol, the mobile phase B is phosphoric acid aqueous solution, and the column temperature of the chromatographic column is 30-40 ℃. In the invention, the moldavica dragonhead formula particles preferably comprise tilianin and/or rosmarinic acid. In the invention, the preparation method of the sample solution 1 containing the moldavica dragonhead formula particles preferably comprises the following steps