CN108445124A - Method for building up, standard finger-print and the application of thoroughfare Fructus Aurantii HPLC finger-prints - Google Patents
Method for building up, standard finger-print and the application of thoroughfare Fructus Aurantii HPLC finger-prints Download PDFInfo
- Publication number
- CN108445124A CN108445124A CN201810229362.6A CN201810229362A CN108445124A CN 108445124 A CN108445124 A CN 108445124A CN 201810229362 A CN201810229362 A CN 201810229362A CN 108445124 A CN108445124 A CN 108445124A
- Authority
- CN
- China
- Prior art keywords
- fructus aurantii
- thoroughfare fructus
- finger
- thoroughfare
- 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.)
- Pending
Links
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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Abstract
The present invention provides a kind of construction methods of thoroughfare Fructus Aurantii HPLC finger-prints, and the standard finger-print that thus method obtains, and the application in thoroughfare Fructus Aurantii quality control；The HPLC finger-prints established with the method for the present invention, can effectively characterize the quality of thoroughfare Fructus Aurantii medicinal material, be conducive to the quality of overall monitor medicinal material；The shared peak of integrated use of the present invention finger-print compares, the methods of clustering and peculiar peak analysis differentiates thoroughfare Fructus Aurantii and its adulterant, realize the discriminating to thoroughfare Fructus Aurantii medicinal material and its Its Common Confused Varieties, and common adulterant can be sorted out, for thoroughfare Fructus Aurantii medicinal material quality control, clinical proper use of provide foundation；The present invention has easy method, stable, precision height, high repeatability and other advantages, can quickly and accurately differentiate that the true and false of product is good and bad.
Description
(1) technical field
The present invention relates to the method for quality control of Chinese medicinal material, and in particular to thoroughfare Fructus Aurantii medicinal material HPLC (high performance liquid chromatography
Method) finger-print construction method, the standard finger-print that thus method obtains, and answering in thoroughfare Fructus Aurantii quality control
With.
(2) background technology
" thoroughfare Fructus Aurantii " is also known as Hu shaddock piece, is Rutaceae citrus plant.Mr. Zhang Yunbing in 1991 is according to its botany spy
For property by its definite designation, the entitled Citrus changshan-huyou Y.B.Chang of botany Latin make Chinese mandarin orange
One novel species of tangerine platymiscium, Zhejiang Quzhou area are major production areas.July, the still green Hu shaddock Chinese olive of pericarp was existed as Fructus Aurantii
It is civil using long-standing, by the research of chemical composition and pharmacological effect in the past to Hu shaddock and with《Chinese Pharmacopoeia》In " trifoliate orange
Shell " is compared, it is found that the two pharmacological action is almost the same.2015 editions《Zhejiang Province's Chinese medicine preparation specification》By Changshan grapefruit Chinese olive
It includes wherein, is officially named " thoroughfare Fructus Aurantii ".
Ripe Hu shaddock fruit and Hu shaddock ped, Hu pomelo flower etc. were had focused largely on using report to the research of Hu shaddock and new resources in the past
It is less to the research of Hu shaddock Chinese olive chemical composition and its medical value in the utilization of food and health products, its quality is commented
It is the researches of valence and few.To sum up, it is main study subject that the present invention, which selects the specific thoroughfare Fructus Aurantii in the place of production, passes through liquid chromatogram
Technology establishes the finger-print of thoroughfare Fructus Aurantii, by similarity-rough set and clustering, from globality angle, overall merit thoroughfare
The quality of medicinal material of Fructus Aurantii, the quality control for thoroughfare Fructus Aurantii provide scientific basis.
(3) invention content
The present invention is intended to provide a kind of construction method of thoroughfare Fructus Aurantii Herbal HPLC Fingerprint, the standard that thus method obtains
Finger-print, and the application in thoroughfare Fructus Aurantii quality control.
Technical scheme is as follows：
A kind of construction method of thoroughfare Fructus Aurantii HPLC finger-prints, described method includes following steps：
(1) preparation of test solution
Thoroughfare Fructus Aurantii test sample is weighed, by solid-liquid ratio 1：50~100 (preferably 1：75, w/v, g/mL) volume fraction 50% is added
In methanol aqueous solution, ultrasonic (30~70KHz, 200~500w of power) handles 10~30min, is cooled to room temperature (20~30 DEG C),
It centrifuges (10000~20000rpm), takes supernatant, filter, gained filtrate is test solution；
The thoroughfare Fructus Aurantii test sample is thoroughfare Fructus Aurantii medicinal material or thoroughfare Fructus Aurantii Praeparata powder, can pass through conventional route on the market
It is commercially available；
The filtering uses 0.45 μm of nylon micro porous filter membrane；
(2) chromatography
Test solution obtained by accurate aspiration step (1), injects high performance liquid chromatograph, and detection obtains the fingerprint of test sample
Collection of illustrative plates；
The chromatographiccondition is：Chromatographic column using octadecylsilane chemically bonded silica as filler, mobile phase by acetonitrile and
0.1%~0.3% aqueous formic acid of volume fraction forms, and using gradient elution, ultraviolet detection wavelength is 330~360nm；
Preferably, the chromatographiccondition is：
Chromatographic column is using octadecylsilane chemically bonded silica as filler, and mobile phase is by acetonitrile and volume fraction 0.1%~0.3%
Aqueous formic acid forms, using gradient elution, 25~40 DEG C of column temperature, ultraviolet detection 320~350nm of wavelength, flow velocity 1.0ml/
Min, 60~70min of analysis time, 5~10 μ L of sample size；
More preferred, the chromatographiccondition is：
Chromatographic column is using octadecylsilane chemically bonded silica as filler, and mobile phase is by 0.1% formic acid water of acetonitrile and volume fraction
Solution composition, using gradient elution, elution program is as shown in table 1,30 DEG C of column temperature, ultraviolet detection wavelength 330nm, flow velocity 1.0ml/
Min, analysis time 70min, 5~10 μ L of sample size；
Table 1
The invention further relates to the acquisitions of standard finger-print：By the thoroughfare Fructus Aurantii of several (preferably 10~20) batches for examination
Product are operated according to above-mentioned steps (1)~(2), obtain liquid chromatogram, import the Chinese medicine fingerprint image that Chinese Pharmacopoeia Commission provides
Similarity evaluation software (2.0) is composed, thoroughfare Fructus Aurantii standard finger-print is automatically generated by software.
The thoroughfare Fructus Aurantii standard finger-print is as shown in Figure 1, have 19 shared peaks, it is determined that the chemistry at wherein 9 peaks
Ingredient, respectively：
No. 4 peaks of rue aurantiin, No. 5 peaks of aurantiin, No. 7 peaks of aurantiamarin, No. 8 peaks of neohesperidin, orange peel lactone hydrate 9
Number No. 18 peak, No. 10 peaks of cyanidenon, No. 13 peaks of orange peel lactone, No. 16 peaks of Nobiletin, hesperetin peaks.
It is with reference to peak with No. 5 peaks of aurantiin, the retention time and relative peak area at 19 shared peaks are as shown in table 2.
2 standard finger-print of table shares peak retention time and relative peak area
Gained standard finger-print can be applied in the quality control of thoroughfare Fructus Aurantii or true and false discriminating, specifically, the application
Method is：
Thoroughfare Fructus Aurantii sample is operated according to above-mentioned steps (1)~(2), the finger-print of sample is obtained, with standard fingerprint figure
It composes as a contrast, the traditional Chinese medicine fingerprint similarity evaluation software (2.0) provided using Chinese Pharmacopoeia Commission, with full spectral peak
Determining fingerprint pattern and similarity calculation are carried out to sample with pattern, with similarity not less than 0.90 for standard judgement sample whether
It is qualified.
Beneficial effects of the present invention are as follows：
(1) the HPLC finger-prints established with method provided by the invention, can effectively characterize the quality of thoroughfare Fructus Aurantii medicinal material,
Be conducive to the quality of overall monitor medicinal material.
(2) the shared peak of integrated use finger-print compares, the methods of clustering and peculiar peak analysis is to thoroughfare Fructus Aurantii
And its adulterant is differentiated, realizes the discriminating to thoroughfare Fructus Aurantii medicinal material and its Its Common Confused Varieties, and can be carried out to common adulterant
Classification, which is the quality control of thoroughfare Fructus Aurantii medicinal material, clinic is proper use of provides foundation.
(3) present invention has easy method, stable, precision height, high repeatability and other advantages.
(4) this method can quickly and accurately differentiate that the true and false of product is good and bad.
(4) it illustrates
Fig. 1：Thoroughfare Fructus Aurantii HPLC standard finger-prints；
Fig. 2：9 mixed mark HPLC chromatograms；Wherein, 1- rues aurantiin, 2- aurantiins, 3- aurantiamarins, 4- neohesperidins,
5- orange peel lactones hydrate, 6- cyanidenons, 7- orange peels lactone, 8- Nobiletins, 9- hesperetins；
Fig. 3：16 batches of sample HPLC characteristic fingerprint patterns；
Fig. 4：Cluster analysis result dendrogram.
(5) specific implementation mode
Below by specific embodiment, the invention will be further described, but protection scope of the present invention is not limited in
This.
Embodiment 1：Detect the finger-print of thoroughfare Fructus Aurantii and its common adulterant
1 instrument and reagent
1.1 instrument
The U.S. HP-1100 Agilent high performance liquid chromatograph (Agilent companies of the U.S.)；Agilent G1316A series of columns
Incubator；Agilent 1314A Train detectors；Aglient 1311A series quaternary pumps；Aglient 1313A series injectors；
6430 liquid chromatograies of Agilent-triple level four bars mass spectrometer (ESI ion sources)；CP225D electronic analytical balances；4020P
Ultrasonic cleaner (JAC companies of South Korea).
1.2 reagent
Chromatographically pure grade acetonitrile (Merck companies of the U.S.), formic acid, methanol are that analysis is pure, and water is ultra-pure water.
1.3 reference substance information
Rue aurantiin (Wei Keqi biotechnologies>98%)；
Aurantiin (Chinese pharmaceutical biological product examines and determine research institute, based on 94.7%)；
Aurantiamarin (Chinese pharmaceutical biological product examines and determine research institute, based on 95.3%)；
Neohesperidin (Chinese pharmaceutical biological product examines and determine research institute, based on 99.6%)；
Orange peel lactone hydrate (ethylmercuric cloride object, based on 98%)；
Orange peel lactone (ethylmercuric cloride object, based on 98%)；
Cyanidenon (Chinese pharmaceutical biological product examines and determine research institute)；
Hesperetin (Wei Keqi biotechnologies,>98%)；
Nobiletin (bio tech ltd Wei Keqi,>98%).
1.4 sample message
3 sample message table of table
2 experimental methods and result
2.1 chromatographic condition
With Extend XDB C18 (250mm × 4.6mm, 5 μm) for chromatographic column, mobile phase is water-soluble by -0.1% formic acid of acetonitrile
Liquid forms, using gradient elution, column temperature：30 DEG C, ultraviolet detection wavelength 330nm, flow velocity：1.0ml/min, analysis time 70min,
5 μ L of sample size, elution program are as shown in table 4：
4 gradient elution program of table
2.2 Mass Spectrometry Conditions
Electric spray ion source (ESI), 350 DEG C, flow rate of carrier gas 10L/min, spray voltage 35MPa of carrier gas temperature, capillary
Voltage 4000V, positive ion detection pattern are collision voltage, and range m/z 100-1000 are with cation mould for level-one full scan mass number
Formula analyzes each ingredient, and second order ms are Product ion scans pattern.
The preparation of 2.3 mixed reference substance solutions
Precision weighs following reference substance：Rue aurantiin, aurantiin, aurantiamarin, neohesperidin, orange peel lactone hydrate,
Cyanidenon, orange peel lactone, Nobiletin, hesperetin prepare mixing control using 50% methanol aqueous solution of volume fraction as solvent
Product solution；
In the mixed reference substance solution, the concentration of each reference substance is as follows：
46.59 μ g/mL of rue aurantiin, 360.80 μ g/mL of aurantiin, 3.45 μ g/mL of aurantiamarin, neohesperidin 312.35
μ g/mL, 1.82 μ g/mL of orange peel lactone hydrate, 6.26 μ g/mL of cyanidenon, 4.47 μ g/mL of orange peel lactone, Nobiletin
1.09 μ g/mL, 1.01 μ g/mL of hesperetin.
The preparation of 2.4 test solutions
Take sample powder 0.3g, it is accurately weighed, set in 25mL measuring bottles, add 50% methanol appropriate, ultrasonic 20min, let cool to
Room temperature adds 50% methanol to scale, shakes up, and centrifugation takes supernatant, as examination after using 0.45 μm of nylon micro porous filter membrane to filter
Product solution.
2.5 experimental results and analysis
2.5.1 the generation of thoroughfare Fructus Aurantii reference fingerprint
To collected Y1~Y11, totally 11 batches of thoroughfare Fructus Aurantii samples are measured, and data processing uses Chinese Pharmacopoeia Commission
The traditional Chinese medicine fingerprint similarity evaluation software of offer carries out similarity analysis to it, and generates reference fingerprint, sees Fig. 1.
2.5.2 thoroughfare Fructus Aurantii characteristic peak is pointed out
Comparative analysis thoroughfare Fructus Aurantii each batch chromatogram determines shared 19, peak, using cation scan pattern, to thoroughfare Fructus Aurantii
Characteristic spectrum shares peak and carries out mass spectrum confirmation, and molecular ion and fragment ion are shown in Table 5, and the chromatographic behavior at shared peak, structure are believed
Breath combines mixing reference substance and document report, identifies the chemical composition at 9 shared peaks.
Compound and predominant secondary fragment ion information in 5 thoroughfare Fructus Aurantii of table
2.5.3 sample measures and adulterant differentiates
It is control, the traditional Chinese medicine fingerprint similarity evaluation provided using Chinese Pharmacopoeia Commission with thoroughfare Fructus Aurantii standard diagram
Software (2.0) carries out determining fingerprint pattern and similarity calculation to sample with full Peak tracking pattern, the results are shown in Table 6.
Compared with thoroughfare Fructus Aurantii standard finger-print, similarity >=0.90 is certified products, and similarity ＜ 0.90 is suspected of adulterant.
6 16 batches of sample similarity results of table
It has selected each batch to repeat to stablize 19 peaks occurred to share peak, has been to compare with thoroughfare Fructus Aurantii standard finger-print
The sample similarity result that arrives is it is found that after computer auxiliary similarity evaluation software calculates, the wherein thoroughfare trifoliate orange of Y1~Y11 batches
The similarity of the opposite reference fingerprint established of shell medicine materical crude slice, can by clustering dendrogram (Fig. 4) 0.99 or more
See, 11 batches of thoroughfare Fructus Aurantiis gather for one kind, and sample room difference is small, and quality is more consistent.The chromatography of remaining Its Common Confused Varieties finger-print
Peak and similarity knot sample room differ greatly, and after clustering, citron and sweet orange gather for one kind, and it is one that shaddock and bowl mandarin orange, which gather,
Class.Had differences in conjunction between the visible different adulterant chemical compositions of finger-print and thoroughfare Fructus Aurantii, by this method can effectively by
It differentiates.
2.6 methodological study
2.6.1 precision test
Test solution, METHOD FOR CONTINUOUS DETERMINATION 6 times are prepared by test solution preparation method, gained shares the relative peak area at peak
The equal ＜ 1.7% of RSD, the equal ＜ 0.1% of RSD of the relative retention time at each shared peak show that instrument precision is good.
2.6.2 stability test
Prepare test solution by test solution preparation method, respectively 0,4,8,12,16, the period measures for 24 hours, institute
The equal ＜ 1.7% of RSD of peak relative peak area must be shared, the equal ＜ 0.1% of RSD of the relative retention time at each shared peak show to supply
Test sample solution is interior for 24 hours basicly stable.
2.4.3 repetitive test
It prepares 6 parts of test solution by test solution preparation method is parallel and measures, gained shares peak relative peak area
The equal ＜ 2.0% of RSD, the equal ＜ 0.1% of RSD of the relative retention time at each shared peak, show that this method repeatability is good.
Some embodiments of the invention above described embodiment only expresses, in this revealed embodiment and all sights
Point should be considered as illustrating the present invention, the description thereof is more specific and detailed, but can not therefore be interpreted as to model of the present invention
The limitation enclosed.It should be pointed out that for those of ordinary skill in the art, in the premise for not departing from present inventive concept
Under, several modifications and improvements can also be gone out, these are all within the scope of protection of the present invention.Therefore, protection scope of the present invention is answered
It is subject to claim, and covers legal equivalents.
Claims (9)
1. a kind of construction method of thoroughfare Fructus Aurantii HPLC finger-prints, which is characterized in that described method includes following steps：
(1) preparation of test solution
Thoroughfare Fructus Aurantii test sample is weighed, by solid-liquid ratio 1：50~100 are added in 50% methanol aqueous solution of volume fraction, are ultrasonically treated 10
~30min, is cooled to room temperature, and centrifugation takes supernatant, filters, gained filtrate is test solution；
(2) chromatography
Test solution obtained by accurate aspiration step (1), injects high performance liquid chromatograph, and detection obtains the fingerprint image of test sample
Spectrum；
The chromatographiccondition is：Chromatographic column is using octadecylsilane chemically bonded silica as filler, and mobile phase is by acetonitrile and volume
0.1%~0.3% aqueous formic acid of score forms, and using gradient elution, ultraviolet detection wavelength is 330~360nm.
2. the construction method of thoroughfare Fructus Aurantii HPLC finger-prints as described in claim 1, which is characterized in that described in step (1)
Thoroughfare Fructus Aurantii test sample is thoroughfare Fructus Aurantii medicinal material or thoroughfare Fructus Aurantii Praeparata powder.
3. the construction method of thoroughfare Fructus Aurantii HPLC finger-prints as described in claim 1, which is characterized in that described in step (1)
Filtering uses 0.45 μm of nylon micro porous filter membrane；
4. the construction method of thoroughfare Fructus Aurantii HPLC finger-prints as described in claim 1, which is characterized in that described in step (2)
Chromatographiccondition is：
Chromatographic column is using octadecylsilane chemically bonded silica as filler, and mobile phase is by 0.1%~0.3% formic acid of acetonitrile and volume fraction
Aqueous solution forms, and using gradient elution, 25~40 DEG C of column temperature, ultraviolet detection 320~350nm of wavelength, flow velocity 1.0ml/min divide
Analyse 60~70min of time, 5~10 μ L of sample size.
5. the construction method of thoroughfare Fructus Aurantii HPLC finger-prints as described in claim 1, which is characterized in that described in step (2)
Chromatographiccondition is：
Chromatographic column is using octadecylsilane chemically bonded silica as filler, and mobile phase is by 0.1% aqueous formic acid of acetonitrile and volume fraction
Composition, using gradient elution, elution program is as shown in table 1：
Table 1
30 DEG C of column temperature, ultraviolet detection wavelength 330nm, flow velocity 1.0ml/min, analysis time 70min, 5~10 μ L of sample size.
6. thoroughfare Fructus Aurantii standard finger-print, which is characterized in that the thoroughfare Fructus Aurantii standard finger-print obtains as follows：
The thoroughfare Fructus Aurantii test sample of several batches is operated according to Claims 1 to 5 any one of them method, obtains liquid phase color
Spectrogram imports the traditional Chinese medicine fingerprint similarity evaluation software that Chinese Pharmacopoeia Commission provides, thoroughfare Fructus Aurantii is automatically generated by software
Standard finger-print.
7. thoroughfare Fructus Aurantii standard finger-print as claimed in claim 6, which is characterized in that have 19 shared peaks, it is determined that its
In 9 peaks chemical composition, respectively：
No. 4 peaks of rue aurantiin, No. 5 peaks of aurantiin, No. 7 peaks of aurantiamarin, No. 8 peaks of neohesperidin, orange peel lactone hydrate 9
No. 18 peak, No. 10 peaks of cyanidenon, No. 13 peaks of orange peel lactone, No. 16 peaks of Nobiletin, hesperetin peaks；
It is with reference to peak with No. 5 peaks of aurantiin, the retention time and relative peak area at 19 shared peaks are as shown in table 2：
2 standard finger-print of table shares peak retention time and relative peak area
8. application of the thoroughfare Fructus Aurantii standard finger-print as claimed in claim 6 in the quality control of thoroughfare Fructus Aurantii or the true and false differentiate.
9. application as claimed in claim 8, which is characterized in that the method for the application is：
Thoroughfare Fructus Aurantii sample is operated according to Claims 1 to 5 any one of them method, the finger-print of sample is obtained, with mark
Quasi- finger-print as a contrast, using Chinese Pharmacopoeia Commission provide traditional Chinese medicine fingerprint similarity evaluation software, to compose entirely
Peak match pattern carries out determining fingerprint pattern and similarity calculation to sample, with similarity not less than 0.90 for standard judgement sample
It is whether qualified.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810229362.6A CN108445124A (en) | 2018-03-20 | 2018-03-20 | Method for building up, standard finger-print and the application of thoroughfare Fructus Aurantii HPLC finger-prints |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810229362.6A CN108445124A (en) | 2018-03-20 | 2018-03-20 | Method for building up, standard finger-print and the application of thoroughfare Fructus Aurantii HPLC finger-prints |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108445124A true CN108445124A (en) | 2018-08-24 |
Family
ID=63195303
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810229362.6A Pending CN108445124A (en) | 2018-03-20 | 2018-03-20 | Method for building up, standard finger-print and the application of thoroughfare Fructus Aurantii HPLC finger-prints |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108445124A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109342631A (en) * | 2018-12-19 | 2019-02-15 | 吉林修正药业新药开发有限公司 | The construction method of the HPLC finger-print of Chinese medicine composition and the quality determining method of Chinese medicine composition |
| CN109507311A (en) * | 2018-10-24 | 2019-03-22 | 扬子江药业集团有限公司 | A kind of identification method of radix scutellariae and its application |
| CN112557563A (en) * | 2019-09-10 | 2021-03-26 | 泰州医药城国科化物生物医药科技有限公司 | Method for identifying medicinal material fructus aurantii in western and Jiangxi regions |
| CN113884591A (en) * | 2021-09-27 | 2022-01-04 | 辽宁中医药大学 | Method for controlling material quality and quantity of bitter orange |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020032308A1 (en) * | 2000-05-18 | 2002-03-14 | Strobel Gary A. | Oocydin and methods of use for protection of plants from Oomyocyte pathogens |
| CN103487528A (en) * | 2013-10-11 | 2014-01-01 | 天津中新药业集团股份有限公司第六中药厂 | HPLC fingerprint determination method of cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills |
| CN106525988A (en) * | 2016-03-11 | 2017-03-22 | 湖南汉森制药股份有限公司 | Detection method for fructus aurantii immaturus medicine finger-print, and standard finger-print |
| CN106525989A (en) * | 2016-03-11 | 2017-03-22 | 湖南汉森制药股份有限公司 | Detection method of fructus aurantii medicine material fingerprint and standard fingerprint |
| CN107290456A (en) * | 2017-07-19 | 2017-10-24 | 山西大学 | A kind of construction method of tussilago liquid-phase fingerprint and application |
| CN107714805A (en) * | 2017-09-11 | 2018-02-23 | 浙江省医学科学院 | Application of the thoroughfare Fructus Aurantii extract in Chinese medicine preparation or functional food is prepared |
-
2018
- 2018-03-20 CN CN201810229362.6A patent/CN108445124A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020032308A1 (en) * | 2000-05-18 | 2002-03-14 | Strobel Gary A. | Oocydin and methods of use for protection of plants from Oomyocyte pathogens |
| CN103487528A (en) * | 2013-10-11 | 2014-01-01 | 天津中新药业集团股份有限公司第六中药厂 | HPLC fingerprint determination method of cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills |
| CN106525988A (en) * | 2016-03-11 | 2017-03-22 | 湖南汉森制药股份有限公司 | Detection method for fructus aurantii immaturus medicine finger-print, and standard finger-print |
| CN106525989A (en) * | 2016-03-11 | 2017-03-22 | 湖南汉森制药股份有限公司 | Detection method of fructus aurantii medicine material fingerprint and standard fingerprint |
| CN107290456A (en) * | 2017-07-19 | 2017-10-24 | 山西大学 | A kind of construction method of tussilago liquid-phase fingerprint and application |
| CN107714805A (en) * | 2017-09-11 | 2018-02-23 | 浙江省医学科学院 | Application of the thoroughfare Fructus Aurantii extract in Chinese medicine preparation or functional food is prepared |
Non-Patent Citations (3)
| Title |
|---|
| CHUNMEI LI ET AL: "Identification of flavanones from peel of Citrus changshan-huyou Y. B. Chang, by HPLC–MS and NMR", 《EUR FOOD RES TECHNOL》 * |
| 王笑笑等: "衢枳壳不同组分体外降糖活性研究及4种黄酮组分含量分析", 《中国现代应用药学》 * |
| 赵宇: "《枳实、枳壳色谱指纹图谱研究》", 《硕士学位论文》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109507311A (en) * | 2018-10-24 | 2019-03-22 | 扬子江药业集团有限公司 | A kind of identification method of radix scutellariae and its application |
| CN109342631A (en) * | 2018-12-19 | 2019-02-15 | 吉林修正药业新药开发有限公司 | The construction method of the HPLC finger-print of Chinese medicine composition and the quality determining method of Chinese medicine composition |
| CN112557563A (en) * | 2019-09-10 | 2021-03-26 | 泰州医药城国科化物生物医药科技有限公司 | Method for identifying medicinal material fructus aurantii in western and Jiangxi regions |
| CN113884591A (en) * | 2021-09-27 | 2022-01-04 | 辽宁中医药大学 | Method for controlling material quality and quantity of bitter orange |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108445124A (en) | Method for building up, standard finger-print and the application of thoroughfare Fructus Aurantii HPLC finger-prints | |
| CN105424850A (en) | Quality evaluation method for dendrobe medicinal material | |
| CN108226313A (en) | In glutinous rehmannia while methods of glycosides measure and fingerprint map construction method | |
| CN105259269A (en) | Establishing method for dendrobe characteristic fingerprint spectrum | |
| CN104950052B (en) | A kind of method that Dementholized mint oil dripping pill quality is detected with gas chromatograph | |
| CN106198782A (en) | A kind of can realize the content analysis of 18 components in Folium Ilicis and the method for quality control of similarity evaluation simultaneously | |
| CN107356691A (en) | Build the detection method of bent finger-print | |
| CN106404942B (en) | A kind of construction method and its standard finger-print of kidney-healing particle finger-print | |
| CN104330489B (en) | A kind of detection method of dispelling wind detoxicating capsule | |
| CN107132304B (en) | A kind of Polygala tenuifolia finger-print and index component content method for measuring | |
| CN111487347B (en) | Method for detecting fingerprint of Zhishu granules | |
| CN107340348A (en) | A kind of method for building up of Bletilla striata medicinal materials HPLC finger-prints | |
| CN109444290A (en) | The construction method and detection method of Asiatic plantain medicinal material UPLC characteristic spectrum | |
| CN109632995A (en) | A kind of method for building up of semen ziziphi spinosae flavones ingredient UPLC finger-print and application | |
| CN106290645B (en) | A kind of construction method and its standard finger-print of Lhasa rhubarb finger-print | |
| CN112666277A (en) | Method for constructing and detecting HPLC (high performance liquid chromatography) characteristic spectrum of rhizoma cyperi medicinal materials, decoction pieces, standard decoction and formula granules | |
| CN107782811A (en) | A kind of detection method of stilbene Siberian cocklebur kidney reinforcing patch finger-print and the stilbene Siberian cocklebur kidney reinforcing patch finger-print of acquisition | |
| CN108267535A (en) | Green peel medicinal materials fingerprint detection method and its finger-print | |
| CN110441413A (en) | The construction method and detection method of qianbai biyan tablets HPLC finger-print | |
| CN111855867A (en) | Method for establishing characteristic spectrum of traditional Chinese medicine or traditional Chinese medicine composition preparation and application thereof | |
| CN110274970A (en) | The method for building up for melting poor finger-print and its application in Yixiesheng capsule Quality Control | |
| CN109374788A (en) | The UPLC characteristic spectrum construction method and detection method of Fructus cnidii | |
| CN113341007B (en) | HPLC (high Performance liquid chromatography) characteristic spectrum-based method for measuring content of all ingredients of jujube kernel nerve-soothing capsules | |
| CN109856262B (en) | Method for qualitative and quantitative analysis of main components of Erding preparation simultaneously | |
| CN103575823A (en) | Detection method of 8 chemical components in Tangminling preparation |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180824 |