CN110954616A - Method for establishing bupleurum chinense fingerprint spectrum quality control system - Google Patents

Method for establishing bupleurum chinense fingerprint spectrum quality control system Download PDF

Info

Publication number
CN110954616A
CN110954616A CN201911271694.1A CN201911271694A CN110954616A CN 110954616 A CN110954616 A CN 110954616A CN 201911271694 A CN201911271694 A CN 201911271694A CN 110954616 A CN110954616 A CN 110954616A
Authority
CN
China
Prior art keywords
fingerprint
peak
bupleurum chinense
methanol
bupleurum
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201911271694.1A
Other languages
Chinese (zh)
Inventor
朱强
葛德助
李振
左成彬
马磊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Jiren Pharmaceutical Co ltd
Original Assignee
Anhui Jiren Pharmaceutical Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui Jiren Pharmaceutical Co ltd filed Critical Anhui Jiren Pharmaceutical Co ltd
Priority to CN201911271694.1A priority Critical patent/CN110954616A/en
Publication of CN110954616A publication Critical patent/CN110954616A/en
Withdrawn legal-status Critical Current

Links

Images

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/86—Signal analysis
    • G01N30/8624—Detection of slopes or peaks; baseline correction
    • G01N30/8631—Peaks
    • G01N30/8637—Peak shape

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention relates to the technical field of medicinal material quality control, in particular to a method for establishing a bupleurum chinense fingerprint spectrum quality control system, which comprises the following steps: preparing a reference substance solution; preparing a test solution: pulverizing bupleuri radix, sieving with 40 mesh sieve, collecting powder 1g, precisely weighing, adding 70% methanol 20mL, placing in round bottom flask, weighing, reflux extracting for 30 min, cooling to room temperature, weighing again, supplementing with 70% methanol, shaking, filtering, and collecting filtrate; compound determination; measuring a fingerprint spectrum; clustering analysis; establishing a fingerprint spectrum; assignment of chromatographic peaks. The established bupleurum chinense medicine fingerprint method is stable, reliable and good in reproducibility, and can provide a basis for quality evaluation of bupleurum chinense medicine.

Description

Method for establishing bupleurum chinense fingerprint spectrum quality control system
Technical Field
The invention relates to the technical field of medicinal material quality control, in particular to a method for establishing a bupleurum chinense fingerprint spectrum quality control system.
Background
The product is prepared from dried root of Bupleurum chinense DC. of Umbelliferae, collected in spring and autumn, removed stem and leaf and sand, and dried to obtain Liaoning, Gansu, Hebei and Henan. In addition, it is also produced in Shaanxi, inner Mongolia and Shandong provinces. Bupleurum scorzonerifolium has the effects of dispelling heat, relieving depression of the liver-qi, and lifting yang-qi. Can be used for treating common cold, fever, alternating chills and fever, distending pain in chest and hypochondrium, menoxenia, uterine prolapse, and proctoptosis. Modern pharmacological studies prove that bupleurum chinense has the effects of resisting inflammation, protecting liver, relieving fever, relieving pain and the like. The main components of the extract are volatile oil and saikosaponin, and the secondary components comprise flavonoid, lignanoid and coumarin saikosaponin which is mainly saikosaponin A, B, C, D; also contains 3-O-acetyl saikosaponin A, 6-O-acetyl saikosaponin A, saikosaponin E, etc.
Referring to FIG. 10, Chinese pharmacopoeia (2015 edition) specifies saikosaponin a (C)42H68O13) And saikosaponin d (C)42H68O13) The total amount of (A) should not be less than 0.30%. However, the specified range is relatively wide, which brings great hidden troubles to the stable and uniform quality and clinical safety and effectiveness of the product, and the quality of the medicinal materials needs to be controlled more strictly.
Disclosure of Invention
The invention aims to solve the defect of unstable quality control of traditional Chinese medicine materials in the prior art, and provides a method for establishing a bupleurum chinense fingerprint quality control system.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method for establishing the bupleurum chinense fingerprint quality control system comprises the following steps:
step one control solution preparation
Accurately weighing 2.00mg of reference substances, respectively placing the reference substances into 10mL measuring bottles, adding a proper amount of 50% methanol for dissolving, and fixing the volume by 50% methanol to obtain reference substance storage liquid with the mass concentration of 200 mu g/mL, wherein the reference substance storage liquid is diluted by 10 times by 50% methanol before sample injection, and the reference substances are chlorogenic acid (111831-;
step two preparation of test solution
Pulverizing bupleuri radix, sieving with 40 mesh sieve, collecting powder 1g, precisely weighing, adding 70% methanol 20mL, placing in round bottom flask, weighing, reflux extracting for 30 min, cooling to room temperature, weighing again, supplementing with 70% methanol, shaking, filtering, and collecting filtrate;
step three compound assay
Detecting a reference solution and a test solution through an HPLC-TOF/MS positive and negative total ion current chromatogram, and carrying out comparative analysis to obtain a result;
step four, determining the fingerprint
Taking a plurality of batches of bupleurum chinense medicinal materials as labels respectively to be used as samples to carry out fingerprint study, importing AIA data files of the fingerprints of the medicinal materials into similarity software 2004A edition of traditional Chinese medicine chromatography fingerprint similarity evaluation system, taking the fingerprints of one batch of bupleurum chinense medicinal materials as reference spectrums, taking the average number vector synthesis of the plurality of samples as a common mode vector, setting the time width to be 0.10, after multi-point correction, determining a main chromatographic characteristic peak, selecting a peak with a large peak area and moderate and stable peak emergence time as a reference peak, calculating the peak area ratio of each chromatographic peak relative to the peak, and if a certain fingerprint has no peak at a certain relative retention time and the relative peak area is zero, still giving corresponding numbers to ensure that each chromatographic fingerprint has the same chromatographic peak number;
step five cluster analysis
Quantifying the peak area of each chromatographic peak in the total chromatographic peak to obtain an original data matrix, and performing cluster analysis on the original data matrix by using SPSS software, wherein the cluster analysis divides the bupleurum chinense sample into a first class and a second class;
step six fingerprint map establishment
Selecting chromatograms of multiple batches of medicinal materials belonging to class I from the clustering analysis results of multiple batches of bupleurum chinense medicinal materials to generate fingerprints and contrast fingerprints, and calculating similarity;
identification of seven chromatographic peaks
And identifying the main characteristic peak in the bupleurum chinense fingerprint by adopting a reference substance and a liquid chromatography-mass spectrometry combined method.
Preferably, in step three:
the chromatographic conditions are as follows: a chromatographic column: orca C185 μ 250 × 4.6 mm; detection wavelength: 210 nm; column temperature: 35 ℃, flow rate: 1 mL/min; mobile phase: a-acetonitrile, B-0.05% phosphoric acid; and (3) an elution mode: gradient elution is carried out for 0-10 min, 15-20% of A, 10-15 min, 20-25% of A, 15-40 min, 25-35% of A, 40-70 min and 35-60% of A; sample introduction amount: 20 mu L of the solution;
the mass spectrum conditions are as follows: the split ratio is set as 1:4, and TOF-MS experimental conditions are as follows: carrying out full scanning (ESI) on positive and negative ions respectively, wherein the scanning mass range is 50-1200 Da; the volume flow of the drying gas is 6L/min, the temperature of the drying gas is 180 ℃, the atomization air pressure is 0.8Bar, the capillary voltage is 4500V in a cation mode, the capillary voltage is 2600V in an anion mode, the fragmentation voltage is 200Vpp, and a sodium formate solution is selected as an internal standard for correction.
Preferably, in step seven:
comparison method:
preparing rutin, saikosaponin A, and saikosaponin D mixed reference solution, measuring by northern bupleurum fingerprint method, and comparing;
HPLC-Q-TOF method:
mass spectrum conditions: HPLC conditions as described before, split ratio was set at 1:4, TOF-MS experimental conditions: carrying out full scanning (ESI) on positive and negative ions respectively, wherein the scanning mass range is 50-1200 Da; the volume flow of the drying gas is 6L/min, the temperature of the drying gas is 180 ℃, the atomization air pressure is 0.8Bar, the capillary voltage is 4500V in a cation mode, the capillary voltage is 2600V in an anion mode, the fragmentation voltage is 200Vpp, and a sodium formate solution is selected as an internal standard for correction.
The establishing method of the bupleurum chinense fingerprint quality control system has the beneficial effects that: a quality evaluation method of the bupleurum chinense HPLC fingerprint is established, and a common mode of bupleurum chinense control fingerprint is established through a system clustering analysis and similarity evaluation system. The established bupleurum chinense fingerprint method is stable, reliable and good in reproducibility, can provide basis for quality evaluation of bupleurum chinense and reliable guarantee for quality control of wind dispelling and toxin removing capsules.
Drawings
FIG. 1 is an HPLC chromatogram of a precision test of the present invention;
FIG. 2 is an HPLC chromatogram of a stability test of the present invention;
FIG. 3 is an HPLC chromatogram of a repeatability test of the present invention;
FIG. 4 is HPLC fingerprint of 15 batches of bupleurum chinense medicinal material;
FIG. 5 is a graph of cluster analysis of Bupleurum chinense Puff;
FIG. 6 is HPLC fingerprint of Bupleurum chinense DC of the present invention;
FIG. 7 is a comparison fingerprint of the present invention;
FIG. 8 is a comparison chart of the bupleurum chinense medicinal material and the mixed contrast;
FIG. 9 is HPLC chromatogram and HPLC chromatogram of positive and negative total ion flow of bupleuri radix of the present invention;
FIG. 10 is a bar chart of determination of saikosaponin A, D content according to the method for determining the content of bupleurum chinense medicine in Chinese pharmacopoeia (2015 edition)
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1-9, a method for establishing a bupleurum chinense fingerprint quality control system comprises the following steps:
step one control solution preparation
Accurately weighing 2.00mg of reference substances, respectively placing the reference substances into 10mL measuring bottles, adding a proper amount of 50% methanol for dissolving, and fixing the volume by 50% methanol to obtain reference substance storage liquid with the mass concentration of 200 mu g/mL, wherein the reference substance storage liquid is diluted by 10 times by 50% methanol before sample injection, and the reference substances are chlorogenic acid (111831-;
step two preparation of test solution
Pulverizing bupleuri radix, sieving with 40 mesh sieve, collecting powder 1g, precisely weighing, adding 70% methanol 20mL, placing in round bottom flask, weighing, reflux extracting for 30 min, cooling to room temperature, weighing again, supplementing with 70% methanol, shaking, filtering, and collecting filtrate;
step three compound assay
Detecting a reference solution and a test solution through an HPLC-TOF/MS positive and negative total ion current chromatogram, and carrying out comparative analysis to obtain a result;
the chromatographic conditions are as follows: a chromatographic column: orca C185 μ 250 × 4.6 mm; detection wavelength: 210 nm; column temperature: 35 ℃, flow rate: 1 mL/min; mobile phase: a-acetonitrile, B-0.05% phosphoric acid; and (3) an elution mode: gradient elution is carried out for 0-10 min, 15-20% of A, 10-15 min, 20-25% of A, 15-40 min, 25-35% of A, 40-70 min and 35-60% of A; sample introduction amount: 20 mu L of the solution;
the mass spectrum conditions are as follows: the split ratio is set as 1:4, and TOF-MS experimental conditions are as follows: carrying out full scanning (ESI) on positive and negative ions respectively, wherein the scanning mass range is 50-1200 Da; the volume flow of the drying gas is 6L/min, the temperature of the drying gas is 180 ℃, the atomization air pressure is 0.8Bar, the capillary voltage is 4500V in a cation mode, the capillary voltage is 2600V in an anion mode, the fragmentation voltage is 200Vpp, and a sodium formate solution is selected as an internal standard for correction.
And (3) precision test:
preparing a bupleurum chinense test solution according to a sample preparation method, measuring under a determined chromatographic condition, continuously feeding samples for 6 times, measuring an HPLC chromatogram, and calculating the relative retention time and the relative peak area of each chromatogram peak by taking the retention time and the chromatogram peak area of the No. 7 peak as references. The HPLC chromatogram of the precision test is shown in figure 1, the precision test data is shown in tables 1 and 2, the relative retention time of each chromatogram peak and the RSD value of the relative peak area are both less than 5 percent, and the requirement of the fingerprint spectrum is met.
TABLE 1 precision test relative retention time data
Figure BDA0002314382390000071
TABLE 2 relative Peak area data for precision tests
Figure BDA0002314382390000081
Investigation of stability test
Taking a sample solution under the precision, sealing, placing at room temperature, detecting the fingerprint at time intervals of 0, 3, 6, 9, 12 and 24 hours, and calculating the relative retention time and the relative peak area of each chromatographic peak by taking the retention time and the chromatographic peak area of the No. 7 peak as references. The HPLC chromatogram of the stability test is shown in figure 2, and as can be seen from tables 3 and 4, the relative retention time of each chromatogram peak and the RSD value of the relative peak area are both less than 5%, which meet the requirements of the fingerprint. The test solution is stable within 24 h.
Table 3 stability test relative retention time data
Figure BDA0002314382390000091
TABLE 4 stability test relative peak area data
Figure BDA0002314382390000092
And (3) repeatability test:
preparing 6 parts of test solution according to the determined preparation method of the test solution, measuring under the determined chromatographic conditions, recording a chromatogram, and calculating the relative retention time and the relative peak area of each chromatogram peak by taking the retention time and the chromatographic peak area of the No. 7 peak as references. The HPLC chromatogram of the repeatability test is shown in figure 3, the repeatability test results are shown in tables 5 and 6, the relative retention time of each chromatogram peak and the RSD value of the relative peak area are both less than 5 percent, and the requirement of the fingerprint spectrum is met.
TABLE 5 repeatability test relative retention time data
Figure BDA0002314382390000101
TABLE 6 relative peak area data for repeatability tests
Figure BDA0002314382390000111
Step four, determining the fingerprint
Taking 15 batches of bupleurum chinense medicinal materials as samples to carry out fingerprint study, importing AIA data files of fingerprints of the 15 batches of medicinal materials into similarity software 2004A edition of traditional Chinese medicine chromatography fingerprint similarity evaluation system, taking the fingerprint of bupleurum chinense medicinal material No. C5 in the table 15 as a reference, taking multi-sample average number vector synthesis as a common mode vector, setting the time width as 0.10, and determining 8 main chromatographic characteristic peaks after multi-point correction. Selecting a No. 7 peak with large peak area and moderate and stable peak-off time as a reference peak, and calculating the peak area ratio of each spectral peak relative to the peak area. If a certain fingerprint has no peak at a certain relative retention time and the relative peak area is zero, corresponding numbers are still given to ensure that all the spectral fingerprints have the same chromatographic peak number. The data are shown in Table 7, and the overlay is shown in FIG. 4;
TABLE 715 batch northern bupleurum root finger-print data
Figure BDA0002314382390000121
Step five cluster analysis
And (3) quantifying the peak area of each chromatographic peak in the total chromatographic peak to obtain a 15x 8-order original data matrix, and performing clustering analysis on the original data matrix by using SPSS software. Clustering analysis divides 15 bupleurum chinense samples into 2 categories, and the intrinsic quality of bupleurum chinense can be judged to have difference. The taxonomic clustering pedigree is shown in FIG. 5. 15 samples are divided into two types, wherein the samples with the sample numbers of 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13 and 15 belong to the class I, and the samples with the sample number of 14 belong to the class II;
step six fingerprint map establishment
Selecting 10 batches of medicinal materials belonging to class I from the 15 batches of bupleurum chinense medicinal materials according to the clustering analysis result to generate a fingerprint and a comparison fingerprint, and calculating the similarity according to a result table 8, and shown in figures 6 and 7;
TABLE 810 batch of similarity evaluation results of Bupleurum chinense
Figure BDA0002314382390000131
As can be seen from the similarity evaluation result, the similarity between each batch of bupleurum chinense and the reference fingerprint is 0.994-0.929, and the technical requirements of the fingerprint are met.
The 15 batches of samples were matched with the control fingerprint by using the 2004 version B calculation software of the evaluation system of chromatographic fingerprint similarity of traditional Chinese medicine, and the similarity evaluation was carried out, the results are shown in Table 9. The result shows that the similarity between each batch of bupleurum chinense medicinal material and the reference fingerprint is 0.994-0.880, which shows that the medicinal materials in each batch have better consistency, and the method can be used for comprehensively evaluating the overall quality of bupleurum chinense medicinal material.
TABLE 9 similarity evaluation of 15 batches of Bupleurum chinense
Figure BDA0002314382390000141
The similarity evaluation result of the research shows that the HPLC chromatograms of the bupleurum chinense medicinal materials are very similar, but the clustering analysis shows that the bupleurum chinense of different batches has certain difference in the content of the main components, and the bupleurum chinense can be divided into two categories according to the difference.
Identification of seven chromatographic peaks
Identifying main characteristic peaks in the bupleurum chinense fingerprint by adopting a reference substance and a liquid chromatography-mass spectrometry combination method;
comparison method:
preparing rutin, saikosaponin A, and saikosaponin D mixed reference solution, measuring by northern bupleurum fingerprint method, and comparing; see fig. 8
HPLC-Q-TOF method:
mass spectrum conditions: HPLC conditions as described before, split ratio was set at 1:4, TOF-MS experimental conditions: carrying out full scanning (ESI) on positive and negative ions respectively, wherein the scanning mass range is 50-1200 Da; the volume flow of the drying gas is 6L/min, the temperature of the drying gas is 180 ℃, the atomization air pressure is 0.8Bar, the capillary voltage is 4500V in a cation mode, the capillary voltage is 2600V in an anion mode, the fragmentation voltage is 200Vpp, and a sodium formate solution is selected as an internal standard for correction.
And identifying the main characteristic peak in the bupleurum chinense fingerprint by adopting a reference substance and a liquid chromatography-mass spectrometry combined method. The 8 main characteristic peaks in the fingerprint are as follows: chlorogenic acid, rutin, rhamnoside, isochlorogenic acid A, isochlorogenic acid B, saikosaponin A, and saikosaponin D. The results are shown in Table 10, FIGS. 8 and 9.
TABLE 10 fingerprint chromatogram peak assignment results
Figure BDA0002314382390000161
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any technical solutions, concepts and designs obtained by equivalent substitutions or changes of the technical solutions and the inventive concepts of the present invention by those skilled in the art within the technical scope of the present invention shall be covered by the scope of the present invention.

Claims (3)

1. A method for establishing a bupleurum chinense fingerprint quality control system is characterized by comprising the following steps:
step one control solution preparation
Accurately weighing 2.00mg of reference substances, respectively placing the reference substances into 10mL measuring bottles, adding a proper amount of 50% methanol for dissolving, and fixing the volume by 50% methanol to obtain reference substance storage liquid with the mass concentration of 200 mu g/mL, wherein the reference substance storage liquid is diluted by 10 times by 50% methanol before sample injection, and the reference substances are chlorogenic acid (111831-;
step two preparation of test solution
Pulverizing bupleuri radix, sieving with 40 mesh sieve, collecting powder 1g, precisely weighing, adding 70% methanol 20mL, placing in round bottom flask, weighing, reflux extracting for 30 min, cooling to room temperature, weighing again, supplementing with 70% methanol, shaking, filtering, and collecting filtrate;
step three compound assay
Detecting a reference solution and a test solution through an HPLC-TOF/MS positive and negative total ion current chromatogram, and carrying out comparative analysis to obtain a result;
step four, determining the fingerprint
Taking labels of multiple batches of bupleurum chinense medicinal materials as samples to perform fingerprint study, importing AIA data files of the fingerprints of the multiple batches of medicinal materials into similarity software 2004A edition of Chinese medicine chromatogram fingerprint similarity evaluation system, taking the fingerprints of one batch of bupleurum chinense medicinal materials as reference spectrums, taking the average number vector synthesis of the multiple samples as a common mode vector, setting the time width to be 0.10, determining a main chromatogram characteristic peak after multi-point correction, selecting a peak with a large peak area and moderate and stable peak emergence time as a reference peak, calculating the peak area ratio of each chromatogram peak relative to the peak, and if a certain fingerprint has no peak at a certain relative retention time and the relative peak area is zero, still giving corresponding numbers to ensure that the fingerprints of all the colors have the same chromatogram peak number;
step five cluster analysis
Quantifying the peak area of each chromatographic peak in the total chromatographic peak to obtain an original data matrix, and performing cluster analysis on the original data matrix by using SPSS software, wherein the cluster analysis divides the bupleurum chinense sample into a first class and a second class;
step six fingerprint map establishment
Selecting chromatograms of multiple batches of medicinal materials belonging to class I from the clustering analysis results of multiple batches of bupleurum chinense medicinal materials to generate fingerprints and contrast fingerprints, and calculating similarity;
identification of seven chromatographic peaks
And identifying the main characteristic peak in the bupleurum chinense fingerprint by adopting a reference substance and a liquid chromatography-mass spectrometry combined method.
2. The method for establishing the bupleurum chinense fingerprint quality control system according to claim 1, which is characterized in that the method comprises the following steps:
the chromatographic conditions are as follows: a chromatographic column: orca C185 μ 250 × 4.6 mm; detection wavelength: 210 nm; column temperature: 35 ℃, flow rate: 1 mL/min; mobile phase: a-acetonitrile, B-0.05% phosphoric acid; and (3) an elution mode: gradient elution is carried out for 0-10 min, 15-20% of A, 10-15 min, 20-25% of A, 15-40 min, 25-35% of A, 40-70 min and 35-60% of A; sample introduction amount: 20 mu L of the solution;
the mass spectrum conditions are as follows: the split ratio is set as 1:4, and TOF-MS experimental conditions are as follows: carrying out full scanning (ESI) on positive and negative ions respectively, wherein the scanning mass range is 50-1200 Da; the volume flow of the drying gas is 6L/min, the temperature of the drying gas is 180 ℃, the atomization air pressure is 0.8Bar, the capillary voltage is 4500V in a cation mode, the capillary voltage is 2600V in an anion mode, the fragmentation voltage is 200Vpp, and a sodium formate solution is selected as an internal standard for correction.
3. The method for establishing the bupleurum chinense fingerprint quality control system according to claim 2, wherein in the seventh step:
comparison method:
preparing rutin, saikosaponin A, and saikosaponin D mixed reference solution, measuring by northern bupleurum fingerprint method, and comparing;
HPLC-Q-TOF method:
mass spectrum conditions: HPLC conditions as described before, split ratio was set at 1:4, TOF-MS experimental conditions: carrying out full scanning (ESI) on positive and negative ions respectively, wherein the scanning mass range is 50-1200 Da; the volume flow of the drying gas is 6L/min, the temperature of the drying gas is 180 ℃, the atomization air pressure is 0.8Bar, the capillary voltage is 4500V in a cation mode, the capillary voltage is 2600V in an anion mode, the fragmentation voltage is 200Vpp, and a sodium formate solution is selected as an internal standard for correction.
CN201911271694.1A 2019-12-12 2019-12-12 Method for establishing bupleurum chinense fingerprint spectrum quality control system Withdrawn CN110954616A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911271694.1A CN110954616A (en) 2019-12-12 2019-12-12 Method for establishing bupleurum chinense fingerprint spectrum quality control system

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911271694.1A CN110954616A (en) 2019-12-12 2019-12-12 Method for establishing bupleurum chinense fingerprint spectrum quality control system

Publications (1)

Publication Number Publication Date
CN110954616A true CN110954616A (en) 2020-04-03

Family

ID=69981061

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911271694.1A Withdrawn CN110954616A (en) 2019-12-12 2019-12-12 Method for establishing bupleurum chinense fingerprint spectrum quality control system

Country Status (1)

Country Link
CN (1) CN110954616A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113514576A (en) * 2021-04-29 2021-10-19 北京振东光明药物研究院有限公司 Establishing method of fingerprint of bupleurum medicinal material, extract and single preparation
CN113917009A (en) * 2021-09-13 2022-01-11 山西大学 Construction method and application of bupleurum chinense non-saponin component HPLC fingerprint
CN114166980A (en) * 2021-12-28 2022-03-11 山西振东泰盛制药有限公司 Method for constructing lignan fingerprint in ginkgo leaf medicinal material, extract and single preparation thereof
CN115586279A (en) * 2022-10-25 2023-01-10 四川新绿色药业科技发展有限公司 Detection method of Bupleurum falcatum or preparation thereof and construction method of fingerprint spectrum thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113514576A (en) * 2021-04-29 2021-10-19 北京振东光明药物研究院有限公司 Establishing method of fingerprint of bupleurum medicinal material, extract and single preparation
CN113917009A (en) * 2021-09-13 2022-01-11 山西大学 Construction method and application of bupleurum chinense non-saponin component HPLC fingerprint
CN113917009B (en) * 2021-09-13 2024-03-12 山西大学 Construction method and application of HPLC fingerprint of non-saponin component of radix bupleuri
CN114166980A (en) * 2021-12-28 2022-03-11 山西振东泰盛制药有限公司 Method for constructing lignan fingerprint in ginkgo leaf medicinal material, extract and single preparation thereof
CN115586279A (en) * 2022-10-25 2023-01-10 四川新绿色药业科技发展有限公司 Detection method of Bupleurum falcatum or preparation thereof and construction method of fingerprint spectrum thereof
CN115586279B (en) * 2022-10-25 2023-12-22 四川新绿色药业科技发展有限公司 Detection method of bupleurum chinense or preparation thereof and construction method of fingerprint of bupleurum chinense or preparation thereof

Similar Documents

Publication Publication Date Title
CN110954616A (en) Method for establishing bupleurum chinense fingerprint spectrum quality control system
Qian et al. Metabolic fingerprinting of Angelica sinensis during growth using UPLC-TOFMS and chemometrics data analysis
Zhang et al. Quality evaluation of S emen C assiae (Cassia obtusifolia L.) by using ultra‐high performance liquid chromatography coupled with mass spectrometry
Kim et al. Chemical fingerprinting of Codonopsis pilosula and simultaneous analysis of its major components by HPLC–UV
Cho Application of proteomics in Chinese medicine research
CN113759003B (en) Licorice origin distinguishing method based on UPLC fingerprint spectrum and chemometrics method
CN113866293A (en) Method for rapidly identifying and analyzing chemical components in chamomile
Li et al. Chromatographic fingerprints analysis and determination of seven components in Danmu preparations by HPLC–DAD/QTOF-MS
Zhao et al. Quality assessment and traceability study of Angelicae Sinensis Radix via binary chromatography, triple quadrupole tandem mass spectrometry, and multivariate statistical analysis
Yi et al. Identification and comparative determination of senkyunolide A in traditional Chinese medicinal plants Ligusticum chuanxiong and Angelica sinensis by HPLC coupled with DAD and ESI-MS
Deng et al. Quantitative and qualitative analysis of Artemisiae Verlotori Folium and Artemisiae Argyi Folium by high‐performance liquid chromatography coupled with quadrupole‐time‐of‐flight mass spectrometry
Du et al. Chemical profiling and marker characterization of Huangqin decoction prepared with three types of peony root by liquid chromatography with electrospray ionization mass spectrometry
Zhou et al. A multivariate analysis on the comparison of raw notoginseng (Sanqi) and its granule products by thin-layer chromatography and ultra-performance liquid chromatography
Long et al. A simple and effective method for identification of Fraxini Cortex from different sources by multi‐mode fingerprint combined with chemometrics
CN111208253A (en) Method for detecting effective components of patrinia and evaluating quality
CN110954617A (en) Method for establishing forsythia suspense fingerprint spectrum quality control system
CN113945674B (en) Characteristic spectrum and analysis method of processed rehmannia root product
CN107607654B (en) Method for analyzing flavonoid chemical components in walnut flower
CN111721880B (en) Method for establishing fingerprint of sarcandra glabra by using double-column tandem HPLC-MS
CN110297047B (en) Establishment method of HPLC fingerprint of lysimachia capillipes hemsl medicinal material and fingerprint thereof
CN113820420A (en) Method for measuring chemical components in intelligence-developing wine by using UPLC-Q-TOF-MS
CN113884597A (en) Sonchus brachyotus DC HPLC-IT-TOF/MS fingerprint detection method and fingerprint thereof
CN112147265A (en) Honeysuckle anti-inflammatory quality marker screening and quality identification method and application
Wei et al. The Comparison of Cinnamomi Cortex and Cinnamomum burmannii Blume Using 1 H NMR and GC-MS Combined with Multivariate Data Analysis
CN111024842A (en) Method for establishing polygonum cuspidatum fingerprint spectrum quality control system

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication

Application publication date: 20200403

WW01 Invention patent application withdrawn after publication