CN106841434A - Ixeris Sonchifolia Hance injection fingerprint checking method - Google Patents
Ixeris Sonchifolia Hance injection fingerprint checking method Download PDFInfo
- Publication number
- CN106841434A CN106841434A CN201710031328.3A CN201710031328A CN106841434A CN 106841434 A CN106841434 A CN 106841434A CN 201710031328 A CN201710031328 A CN 201710031328A CN 106841434 A CN106841434 A CN 106841434A
- Authority
- CN
- China
- Prior art keywords
- peak
- ixeris sonchifolia
- sonchifolia hance
- solution
- hance injection
- 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
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)
- Saccharide Compounds (AREA)
Abstract
The invention discloses a kind of traditional Chinese medicine injection fingerprint checking method, i.e. Ixeris Sonchifolia Hance injection fingerprint checking method.By the investigation of the method such as general condition and system suitability, the preparation method of reference solution, the preparation method of need testing solution, sample size of checking colors, optimal detection method is set up；Prove that this method meets the requirements of fingerprint analysis method by the investigation of precision, stability, repeatability.The Ixeris Sonchifolia Hance injection fingerprint analysis method that the present invention sets up, can with it is sensitive, quality control is carried out to Ixeris Sonchifolia Hance injection exactly, compensate for lacking in Ixeris Sonchifolia Hance injection quality standard the deficiency of finger-print check item, be that Ixeris Sonchifolia Hance injection security revalues the corresponding technical method of offer.
Description
Technical field
The present invention relates to a kind of traditional Chinese medicine injection detection method for quality, i.e. Ixeris Sonchifolia Hance injection fingerprint checking method.
Background technology
In the prior art, Ixeris Sonchifolia Hance injection（Former name：Diemailing injection）List national drug standards product in（State
The quasi- word Z20025450 of medicine）, produced by Tonghua Huaxia Pharmaceutical Co., Ltd..
Prescription：Irexis sonchifolia 1000g, is made 1000ml.
Assay：This product is per 10ml containing general flavone with anhydrous rutin（C27H30O16）Meter, must not be less than 4.0mg.Containing an armful stem
Denticulate ixeris herb is with adenosine（C10H12N5O4）Meter, must not be less than 0.025mg.
Indication：Promoting blood circulation and stopping pain, Qingre Quyu.For the obstruction of qi in the chest of hemostasis impatency, card is shown in：It is uncomfortable in chest, pained, bitter taste, tongue
It is dark red or deposit ecchymosis etc..See above-mentioned symptom person suitable for coronary heart diseases and angina pectoris.Also the person that can be used for cerebral infarction.
Usage and dosage：Drip-feed, a 10-40ml, 1 times a day；It is dilute with 5% glucose or 0.9% sodium chloride injection
Release and applied to 250-500ml；It is within 14 days a course for the treatment of；Or follow the doctor's advice.
Specification：Every dress（1）10ml,（2）20ml,（3）40ml.
The stabilization of traditional Chinese medicine quality, it is controllable be the safe and effective guarantee of clinical application.In traditional Chinese medicine chemistry into
Dividing has complexity and diversity, only can not comprehensively be reflected by the assay of single or several chemical compositions and control Chinese medicine
The quality of injection.This is accomplished by setting up a kind of rationally effective traditional Chinese medicine method of quality control.At present, Chinese medicine fingerprint image
Spectrum has obtained internationally recognized as the core technology of system of modern TCM quality standards, FDA, WHO, Germany, India and Japan etc.
Country uses fingerprint pattern technology as the quality control method of autonomic drug.State food pharmaceuticals administration general bureau（CFDA）
Traditional Chinese medicine is distinctly claimed in safety of Chinese medicine injection revalues guideline and must be set up finger-print check item.
Due to there is no regulation finger-print check item and inspection method in current Ixeris Sonchifolia Hance injection quality standard.Therefore, the present invention can
Method is provided with for Ixeris Sonchifolia Hance injection finger-print inspection, the deficiency of quality standard is made up.
The content of the invention
The purpose of the present invention is directed to above mentioned problem and demand, and sets up a kind of Ixeris Sonchifolia Hance injection finger-print reviewing party
Method.
Technical solution of the invention is：Ixeris Sonchifolia Hance injection fingerprint checking method is set up, its characterization step is such as
Under：
1st, chromatographic condition and system suitability：
With octadecylsilane chemically bonded silica as filler, chromatographic column：Mm × 250 mm of Waters Symmetry C18 4.6,
5μm；With acetonitrile as mobile phase A, 0.2% phosphoric acid solution is Mobile phase B, and the regulation according to the form below carries out gradient elution；Flow velocity is
1.0ml/min；Detection wavelength：260nm；Column temperature is 40 DEG C.Number of theoretical plate presses cyanidenon 7-O- β-D-Glucose aldehydic acid glycosides peak
Calculating should be not less than 5000.
2nd, the preparation of reference solution：
Adenosine reference substance, cyanidenon 7-O- β-D-Glucose aldehydic acid glycosides reference substance and Cichoric acid reference substance are taken, it is accurately weighed, plus
25% methanol solution is made every 1mL and contains the μ g of adenosine 5, cyanidenon 7-O- β-μ g's of D-Glucose aldehydic acid glycosides 150 and the μ g of Cichoric acid 60
Mixed solution, obtains final product.
3rd, the preparation of need testing solution：
Ixeris Sonchifolia Hance injection is taken, is filtered with 0.45 μm of filter membrane, obtained final product.
4th, determination method：
It is accurate to draw reference solution and each 5 μ L of need testing solution, liquid chromatograph is injected, determine, record the color in 75 minutes
Spectral peak, obtains final product.
Contained principle active component is the compositions such as adenosine, organic acid and flavonoids in Ixeris Sonchifolia Hance injection, according to it
Chemical property, selects reversed-phased high performace liquid chromatographic to carry out fingerprint map analyzing.The Waters Symmetry that the present invention is used
The chromatographic peak peak shape that chromatographic column is obtained is good；Flow phase system have to the main component in Ixeris Sonchifolia Hance injection good wash-out and
Separating power；Under the Detection wavelength of 260nm, the response of adenosine is big, while other masters more can also comprehensively be detected
Want composition.The Ixeris Sonchifolia Hance injection fingerprint analysis method sensitivity that the present invention sets up is high, separating degree and favorable reproducibility, baseline
Noise is small.
Should be presented in finger-print of the present invention and adenosine, cyanidenon -7-O- β-D-Glucose aldehydic acid glycosides and Cichoric acid
The consistent chromatographic peak of three reference substance chromatographic peak retention times, and 10 total peaks should occur, with 1,2 (S), 3,4,5,6,7,8
(S), 9 (S), No. 10 peaks are mark, are calculated through similarity evaluation software, and compare fingerprint image
Spectrum compares, and similarity should be not less than 0.85.
In Fig. 1, peak 2 (S) adenosine；The uridine of peak 3；The guanosine of peak 4；The single coffee acyl group tartaric acid in peak 5；The cyanidenon of peak 7
7-O- β-D- glucopyranosides；Peak 8 (S) cyanidenon -7-O- β-D- glucuronic acid glycosides；Peak 9 (S) Cichoric acid；The celery of peak 10
Dish element -7-O- β-D- glucuronic acid glycosides.
It is an advantage of the invention that：1st, this experiment establishes the HPLC chromatogram analysis method of Ixeris Sonchifolia Hance injection, and carries out
Instrument precision, method repeatability and sample stability checking, meet fingerprint analysis method requirement.2nd, this experiment is most
Ixeris Sonchifolia Hance injection is established eventually in Agilent, Waters and three reference fingerprints of instrument of Shimadzu, the matching of each sample
Similarity is all higher than 0.85, and the reference fingerprint set up can be used for the inspection of Ixeris Sonchifolia Hance injection fingerprint map analyzing.3、
The Ixeris Sonchifolia Hance injection reference fingerprint that this experiment is set up can rapidly and accurately identify 10 characteristic peaks, more comprehensively right
The quality of Ixeris Sonchifolia Hance injection is controlled.4th, the final HPLC fingerprint map analyzing sides for establishing Ixeris Sonchifolia Hance injection of this experiment
Method, sensitivity is high, and separating degree is good, and chromatogram applicability is stronger.5th, the final finger-print inspection for establishing favorable reproducibility of this experiment
Survey method, main chemical compositions more comprehensively contained by reflection Ixeris Sonchifolia Hance injection, improves the stability of product.
Brief description of the drawings
Fig. 1 Ixeris Sonchifolia Hance injection reference fingerprints.
10 batches of parenteral solution matching chromatograms of Fig. 2 Agilent instruments.
Fig. 3 Agilent instrument sample reference fingerprints.
Fig. 4 Agilent instrument object of reference chromatographic fingerprintings.
10 batches of parenteral solution matching chromatograms of Fig. 5 Waters instruments.
Fig. 6 Waters instrument sample reference fingerprints.
Fig. 7 Waters instrument object of reference chromatographic fingerprintings.
10 batches of parenteral solution matching chromatograms of Fig. 8 Shimadzus instrument.
Fig. 9 Shimadzu instrument reference fingerprints.
Figure 10 Shimadzu instrument object of reference chromatograms.
Specific embodiment
The present invention is described below by specific embodiment.Unless stated otherwise, technological means used in the present invention
It is method known in those skilled in the art.In addition, embodiment is interpreted as illustrative, it is not intended to limit the present invention
Scope, the spirit and scope of the invention are limited only by the claims that follow.To those skilled in the art, without departing substantially from this
On the premise of invention spirit and scope, the various changes that are carried out to the material component and consumption in these embodiments or change
Belong to protection scope of the present invention.Ixeris Sonchifolia Hance injection, related chemistry raw material and reagent used of the invention are commercially available.
Embodiment 1
1 instrument and material
The highly effective liquid phase chromatographic systems of Agilent Technologies 1200（Containing quaternary pump, automatic sampler, column oven,
1260 DAD detectors；Agilent companies of the U.S.）；The efficient liquid phase liquid chromatographs of Waters 2695（Containing quaternary pump, enter automatically
Sample device, column oven, 2698DAD detectors；Waters, US）；Shimadzu LC-20AT liquid chromatographs（Containing binary pump, automatically
Injector, LC-20AT PDA detectors；Japanese Shimadzu Corporation）；The external column oven of M320 types（Tianjin Puxiang）.
Acetonitrile（Sigma companies, the U.S., chromatographically pure）；Distilled water（Guangzhou Watson food and drink Co., Ltd）；Phosphoric acid
（Tianjin Ke Miou chemical reagent Co., Ltd）.Adenosine, Cichoric acid standard items are bought in National Institute for Food and Drugs Control, batch
Number 110879-200202 and 111752-200902 is respectively, purity is all higher than 98%；Cyanidenon -7-O- β-D glucuronic acids
Glycosides is provided by Tonghua Huaxia Pharmaceutical Co., Ltd., and purity is more than 98%.Ixeris Sonchifolia Hance injection 10 batches, lot number is respectively
151108,151221,160101,160104,160106,160309,160310,160405,160411,160417.
Method and result
It is prepared by 2.1 solution
It is prepared by sample solution：Each batch Ixeris Sonchifolia Hance injection, crosses 0.45 μm of miillpore filter, takes subsequent filtrate sample introduction.
It is prepared by reference solution：Take adenosine reference substance, cyanidenon 7-O- β-D-Glucose aldehydic acid glycosides reference substance and witloof
Sour reference substance is appropriate, accurately weighed, plus methanol-water（25:75）It is made every 1mL μ g containing adenosine 5, cyanidenon 7-O- β-D- grapes
The μ g of glycuronide 150, the mixed solution of the μ g of Cichoric acid 60, obtain final product.4 DEG C of preservations of the solution prepared.
Chromatographic condition
Chromatographic column：Waters Symmetry C18（4.6 mm × 250 mm, 5 μm）, Part No. WAT054275, Lot
No.0294353071；Detection wavelength 260nm；Mobile phase：0.2% phosphate aqueous solution (A)-acetonitrile (B), the gradient such as institute of table 1
Show, the mL/min of flow velocity 1.0；The μ L of sample size 5；40 DEG C of column temperature.
Methodological study
2.3.1 Agilent instrumental methods checking
1) precision
The need testing solution prepared under " 2.2 " is taken, according to chromatographic condition continuous sample introduction shown under " 2.3 " 6 times, each feature
The peak area RSD at peak the results are shown in Table 2.
Result of the test shows, RSD ＜ 3%, and precision is good.
Repeatability
6 parts of need testing solutions are prepared by method under " 2.2 " is parallel, are analyzed according to chromatographic condition sample introduction shown under " 2.3 ",
The peak area RSD of each characteristic peak the results are shown in Table 3.
Result of the test shows that RSD ＜ 3%, method repeatability is good.
Sample stability
Take the need testing solution prepared under " 2.2 ", according to chromatographic condition shown under " 2.3 " after sample preparation 0h, 2h,
4h, 8h, 12h, 24h, sample introduction analysis, the peak area RSD of each characteristic peak the results are shown in Table 4.
Result of the test shows：RSD is respectively less than 3%, and sample places 24 hours stabilizations.
Instrumental method is verified
1) precision
The need testing solution prepared under " 2.2 " is taken, according to chromatographic condition continuous sample introduction shown under " 2.3 " 6 times, each feature
The peak area RSD at peak the results are shown in Table 5.
Result of the test shows, RSD ＜ 3%, and precision is good.
Repeatability
6 parts of need testing solutions are prepared by method under " 2.2 " is parallel, are analyzed according to chromatographic condition sample introduction shown under " 2.3 ",
The peak area RSD of each characteristic peak the results are shown in Table 6.
Result of the test shows that RSD ＜ 3%, method repeatability is good.
）Sample stability
Take the need testing solution prepared under " 2.2 ", according to chromatographic condition shown under " 2.3 " after sample preparation 0h, 2h,
4h, 8h, 12h, 24h, sample introduction analysis, the peak area RSD of each characteristic peak the results are shown in Table 7.
Result of the test shows：RSD is respectively less than 3%, and sample places 24 hours stabilizations.
Shimadzu instrumental method is investigated
1) precision
The need testing solution prepared under " 2.2 " is taken, according to chromatographic condition continuous sample introduction shown under " 2.3 " 6 times, each feature
The peak area RSD at peak the results are shown in Table 8.
Result of the test shows, RSD ＜ 3%, and precision is good.
Repeatability
6 parts of need testing solutions are prepared by method under " 2.2 " is parallel, are analyzed according to chromatographic condition sample introduction shown under " 2.3 ",
The peak area RSD of each characteristic peak the results are shown in Table 9.
Result of the test shows that RSD ＜ 3%, method repeatability is good.
）Sample stability
Take the need testing solution prepared under " 2.2 ", according to chromatographic condition shown under " 2.3 " after sample preparation 0h, 2h,
4h, 8h, 12h, 24h, sample introduction analysis, the peak area RSD of each characteristic peak the results are shown in Table 10.
Result of the test shows：RSD is respectively less than 3%, and sample places 24 hours stabilizations.
Analysis and data are derived
10 batches of parenteral solutions shown under " 2.1 " are used as shown under " 2.1 " according to chromatographic process under " 2.3 " respectively
Agilent, Waters and three liquid chromatograph analytical controls of Shimadzu, carry work station and process and derive AIA lattice by instrument
Formula chromatographic data, the integral parameter of three instruments is set to as follows：Agilent：Slope Sensitivity（Slope sensitivity）
5, Peak Width（Peak width）0.05, Area Reject（Minimum peak area）1, Height Reject（Minimum peak height）1.
Waters：Threshold value 50, peak width 30, minimum peak area 1000, minimum peak height 0.Shimadzu：Slope 2000, half-peak breadth 5, smallest peaks face
Product/peak height 1000.
Reference fingerprint is set up
Open chromatographic fingerprints of Chinese materia medica similarity evaluation software（2.0 editions, Chinese Pharmacopoeia Commission, 2010）, mode of operation choosing
Generation control is selected, the initial data that three instruments are analyzed is directed respectively into；It is respectively with reference to collection of illustrative plates parameter setting：Compiled with reference to collection of illustrative plates
Number it is S1, control collection of illustrative plates generation method is average method, and time window width is defaulted as 0.1；10 are selected under Supplements module
Individual common characteristic peaks；Peak match mode selects Mark peak matches；Generation control is clicked on after the completion of matching, you can obtain compareing fingerprint
Collection of illustrative plates, the control collection of illustrative plates of gained is preserved, in case being used during analytical control.Click on matched data and calculate similarity button, look into
See and preserve matching result.Ixeris Sonchifolia Hance injection reference fingerprint is as shown in Figure 1.
Instrument
Reference fingerprint is set up according to the method under " 2.5 ".10 batches of parenteral solutions match chromatogram, and reference fingerprint is as schemed
Shown in 2, Fig. 2：Peak 2（S）Adenosine；The uridine of peak 3；The guanosine of peak 4；The single coffee acyl group tartaric acid in peak 5；The cyanidenon 7-O- of peak 7
β-D- glucopyranosides；Peak 8（S）Cyanidenon -7-O- β-D- glucuronic acid glycosides；Peak 9（S）Cichoric acid；The apiolin of peak 10-
7-O- β-D- glucuronic acid glycosides.Each batch parenteral solution is shown in Table 11 with the similarity of reference fingerprint.Object of reference chromatogram such as Fig. 3
It is shown.
In Fig. 3：Peak 2（S）Adenosine；The uridine of peak 3；The guanosine of peak 4；The single coffee acyl group tartaric acid in peak 5；The cyanidenon 7- of peak 7
O- β-D- glucopyranosides；Peak 8（S）Cyanidenon -7-O- β-D- glucuronic acid glycosides；Peak 9（S）Cichoric acid；The celery of peak 10
Element -7-O- β-D- glucuronic acid glycosides.
It can be seen that through occurred in that in each batch parenteral solution finger-print of Agilent Instrumental Analysis with adenosine, cyanidenon-
7-O- β-D-Glucose aldehydic acid glycosides and Cichoric acid three occur in that 10 with reference to the consistent chromatographic peak of chromatographic peak retention time
Total peak, is mark with 1,2 (S), 3,4,5,6,7,8 (S), 9 (S), No. 10 peaks, through chromatographic fingerprints of Chinese materia medica similarity evaluation
Systems soft ware is calculated, and compared with reference fingerprint, similarity is all higher than 0.85.
Instrument
Reference fingerprint is set up according to the method under " 2.5 ".10 batches of parenteral solutions match chromatogram, and reference fingerprint is as schemed
Shown in 4, Fig. 4：Peak 2（S）Adenosine；The uridine of peak 3；The guanosine of peak 4；The single coffee acyl group tartaric acid in peak 5；The cyanidenon 7- of peak 7
O- β-D- glucopyranosides；Peak 8（S）Cyanidenon -7-O- β-D- glucuronic acid glycosides；Peak 9（S）Cichoric acid；The celery of peak 10
Element -7-O- β-D- glucuronic acid glycosides.Each batch parenteral solution is shown in Table 12 with the similarity of reference fingerprint.Object of reference chromatogram is such as
Shown in Fig. 5.
It can be seen that through occurred in that in each batch parenteral solution finger-print of Waters Instrumental Analysis with adenosine, cyanidenon-
7-O- β-D-Glucose aldehydic acid glycosides and Cichoric acid three occur in that 10 with reference to the consistent chromatographic peak of chromatographic peak retention time
Total peak, is mark with 1,2 (S), 3,4,5,6,7,8 (S), 9 (S), No. 10 peaks, through chromatographic fingerprints of Chinese materia medica similarity evaluation
Systems soft ware is calculated, and compared with reference fingerprint, similarity is all higher than 0.85.
Shimadzu instrument
Reference fingerprint is set up according to the method under " 2.5 ".10 batches of parenteral solution matching chromatograms are as shown in figure 8, control refers to
As shown in figure 9, the similarity of each batch parenteral solution and reference fingerprint is shown in Table 13, object of reference chromatogram is shown in Figure 10 to line collection of illustrative plates.
Fig. 9：Peak 2（S）Adenosine；The uridine of peak 3；The guanosine of peak 4；The single coffee acyl group tartaric acid in peak 5；The cyanidenon 7-O- β-D- pyrroles of peak 7
Glucopyranoside glycosides；Peak 8（S）Cyanidenon -7-O- β-D- glucuronic acid glycosides；Peak 9（S）Cichoric acid；Apiolin-7-O- the β of peak 10-
D- glucuronic acid glycosides.
It can be seen that through occurred in that in each batch parenteral solution finger-print of Shimadzu Instrumental Analysis with adenosine, cyanidenon -7-O- β -
D-Glucose aldehydic acid glycosides and Cichoric acid three occur in that 10 have with reference to the consistent chromatographic peak of chromatographic peak retention time
Peak, is mark with 1,2 (S), 3,4,5,6,7,8 (S), 9 (S), No. 10 peaks, through similarity evaluation
Software is calculated, and compared with reference fingerprint, similarity is all higher than 0.85.
Conclusion
This experiment establishes the HPLC chromatogram analysis method of Ixeris Sonchifolia Hance injection, and has carried out instrument precision, method repeatability
And sample stability checking, meet fingerprint analysis method requirement.This experiment finally establishes Ixeris Sonchifolia Hance injection and exists
Agilent, Waters and three reference fingerprints of instrument of Shimadzu, the matching similarity of each sample are all higher than 0.85, are built
Vertical reference fingerprint can be used for the inspection of Ixeris Sonchifolia Hance injection fingerprint map analyzing.
It is described above, simply specific embodiment of the invention, various illustrations are not to substance structure of the invention
Into limitation.
Claims (1)
1. Ixeris Sonchifolia Hance injection fingerprint checking method, it is characterised in that carry out as follows：
（1）Chromatographic condition and system suitability：
With octadecylsilane chemically bonded silica as filler, chromatographic column：Mm × 250 mm of Waters Symmetry C18 4.6,
5μm；With acetonitrile as mobile phase A, 0.2% phosphoric acid solution is Mobile phase B, and gradient elution is carried out by the regulation in following:
Time minute mobile phase A % Mobile phase Bs %
0~12 0 → 2 100 → 98
12~30 2 → 15 98 → 85
30~55 15 → 17 85 → 83
55~65 17 → 25 83 → 75
65~70 25 → 0 75 → 100
70~75 0 100
Flow velocity is 1.0ml/min；Detection wavelength：260nm；Column temperature is 40 DEG C, and number of theoretical plate presses cyanidenon 7-O- β-D- grapes
Glycuronide peak is calculated and should be not less than 5000；
（2）The preparation of reference solution
Adenosine reference substance, cyanidenon 7-O- β-D-Glucose aldehydic acid glycosides reference substance and Cichoric acid reference substance are taken, it is accurately weighed, plus
25% methanol solution is made every 1mL and contains the μ g of adenosine 5, cyanidenon 7-O- β-μ g's of D-Glucose aldehydic acid glycosides 150 and the μ g of Cichoric acid 60
Mixed solution, obtains final product；
（3）The preparation of need testing solution：
Ixeris Sonchifolia Hance injection is taken, is filtered with 0.45 μm of filter membrane, obtained final product；
（4）Determination method：
It is accurate to draw reference solution and each 5 μ L of need testing solution, liquid chromatograph is injected, determine, record the color in 75 minutes
Spectral peak, obtains final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710031328.3A CN106841434A (en) | 2017-01-17 | 2017-01-17 | Ixeris Sonchifolia Hance injection fingerprint checking method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710031328.3A CN106841434A (en) | 2017-01-17 | 2017-01-17 | Ixeris Sonchifolia Hance injection fingerprint checking method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106841434A true CN106841434A (en) | 2017-06-13 |
Family
ID=59123884
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710031328.3A Pending CN106841434A (en) | 2017-01-17 | 2017-01-17 | Ixeris Sonchifolia Hance injection fingerprint checking method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106841434A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110297061A (en) * | 2019-07-25 | 2019-10-01 | 广西中医药大学 | Survey the methods for commenting method measurement Chinese ixeris herb Content of Chlorogenic Acid, caffeic acid and galuteolin content using one more |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1762406A (en) * | 2005-10-11 | 2006-04-26 | 沈阳双鼎制药有限公司 | Quality control method of ixeris sonchifolia injection |
| CN1868498A (en) * | 2006-04-10 | 2006-11-29 | 华玉强 | Gutweed total flavone, its prepn. method, freeze-drying powder injection containing it and quality control method therefor |
| CN102249917A (en) * | 2011-05-20 | 2011-11-23 | 沈阳双鼎科技有限公司 | Chicoric acid and extraction and separation method and application thereof |
| CN102283879A (en) * | 2011-07-19 | 2011-12-21 | 沈阳双鼎科技有限公司 | Preparation method and quality control method for Ixeris sonchifolia Hance injection |
| CN104316630A (en) * | 2014-01-17 | 2015-01-28 | 通化华夏药业有限责任公司 | Method for determining content of saccharide components in ixeri sonhifolia injection |
| CN104359968A (en) * | 2014-11-14 | 2015-02-18 | 通化华夏药业有限责任公司 | Research for realizing quick classification and identification of chemical components in ixeris sonchifolia hance injection based on UPLC-Q-TOF-MS technology |
-
2017
- 2017-01-17 CN CN201710031328.3A patent/CN106841434A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1762406A (en) * | 2005-10-11 | 2006-04-26 | 沈阳双鼎制药有限公司 | Quality control method of ixeris sonchifolia injection |
| CN1868498A (en) * | 2006-04-10 | 2006-11-29 | 华玉强 | Gutweed total flavone, its prepn. method, freeze-drying powder injection containing it and quality control method therefor |
| CN102249917A (en) * | 2011-05-20 | 2011-11-23 | 沈阳双鼎科技有限公司 | Chicoric acid and extraction and separation method and application thereof |
| CN102283879A (en) * | 2011-07-19 | 2011-12-21 | 沈阳双鼎科技有限公司 | Preparation method and quality control method for Ixeris sonchifolia Hance injection |
| CN104316630A (en) * | 2014-01-17 | 2015-01-28 | 通化华夏药业有限责任公司 | Method for determining content of saccharide components in ixeri sonhifolia injection |
| CN104359968A (en) * | 2014-11-14 | 2015-02-18 | 通化华夏药业有限责任公司 | Research for realizing quick classification and identification of chemical components in ixeris sonchifolia hance injection based on UPLC-Q-TOF-MS technology |
Non-Patent Citations (3)
| Title |
|---|
| 刘荣荣 等: "超高效液相色谱-质谱/质谱串联法快速测定苦碟子注射液中10种活性成分的含量", 《中南药学》 * |
| 刘颖 等: "苦碟子注射液HPLC指纹图谱与化学模式识别分析", 《中国药学杂志》 * |
| 彭振宇 等: "苦碟子注射液指纹图谱的研究", 《药物研究》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110297061A (en) * | 2019-07-25 | 2019-10-01 | 广西中医药大学 | Survey the methods for commenting method measurement Chinese ixeris herb Content of Chlorogenic Acid, caffeic acid and galuteolin content using one more |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103257188B (en) | Construction method for compound thrombus clearing preparation bioactivity chromatography finger print | |
| CN104569170B (en) | A kind of detection method of ginkgo-dipyridamine injection | |
| CN101167788B (en) | Quality control method of traditional Chinese medicine 'zhenqi fuzheng' containing glossy privet fruit and radix astragali for strengthening the body resistance for aeipathia deficiency damage and qi | |
| CN107727753B (en) | Method for establishing baile sleeping capsule fingerprint | |
| CN108226321B (en) | Fingerprint detection method and fingerprint of fructus piperis longi and fructus piperis longi stomach-ache granules | |
| CN104359968A (en) | Research for realizing quick classification and identification of chemical components in ixeris sonchifolia hance injection based on UPLC-Q-TOF-MS technology | |
| CN103149301A (en) | Method for simultaneously determining contents of 10 nucleoside components in sowthistle-leaf ixeris seedling injection by utilizing HPLC-DAD (High Performance Liquid Chromatography-Diode Array detector) method | |
| CN107860832B (en) | Method for establishing fingerprint of compound rhubarb clear pancreas soup | |
| CN113252821A (en) | Method for establishing fingerprint of flavonoid component in ginkgo leaf extraction intermediate or preparation thereof and established fingerprint | |
| CN103969350B (en) | A kind of method for building up of antiphlogistic Chunwang capsule HPLC finger printing | |
| CN101843667B (en) | Shuanghuanglian medicinal composition and preparation method thereof | |
| CN108627581A (en) | Rhynchophyllin and isorhynchophylline content assaying method in a kind of Xiao ' erqixingcha particle | |
| CN105911192B (en) | A kind of extracting method and fingerprint atlas detection method of Pterospermi Heterophylli active site promoting blood circulation and removing blood stasis | |
| CN107688061A (en) | A kind of construction method of the finger-print of anti-inflammatory sterilization capsule | |
| CN103630633A (en) | Method for measuring contents of six amino acids in ixeris sonchifolia injection by using pre-column derivatization method | |
| CN103163243B (en) | Method for simultaneously determining five organic acid components content in Ixeris sonchifolia Hance injection by HPLC-DAD method | |
| CN109633043A (en) | A kind of method for building up and its standard diagram of gadol injection HPLC finger-print | |
| CN106841434A (en) | Ixeris Sonchifolia Hance injection fingerprint checking method | |
| CN110057950A (en) | A kind of construction method of the Pudilan sulfathiazole HPLC finger-print based on Detection wavelength switching | |
| CN114062533A (en) | Method for measuring content of multi-index components in Fuchun tablets | |
| CN110554103B (en) | Radix astragali and radix puerariae particle component detection method and fingerprint spectrum construction method thereof | |
| CN113155994A (en) | Method for establishing fingerprint spectrum of carpet bugle medicinal preparation | |
| CN109709222B (en) | Component detection method of Ganmaoling and compound Ganmaoling | |
| CN103115985B (en) | Method for synchronously detecting six flavonoid constituents in sowthistle-leaf ixeris seedling injection in HPLC-DAD (High Performance Liquid Chromatography-Diode Array detector) method | |
| CN111721880A (en) | Method for establishing fingerprint of sarcandra glabra by using double-column tandem HPLC-MS |
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: 20170613 |