CN109633043A - A kind of method for building up and its standard diagram of gadol injection HPLC finger-print - Google Patents
A kind of method for building up and its standard diagram of gadol injection HPLC finger-print Download PDFInfo
- Publication number
- CN109633043A CN109633043A CN201910147591.8A CN201910147591A CN109633043A CN 109633043 A CN109633043 A CN 109633043A CN 201910147591 A CN201910147591 A CN 201910147591A CN 109633043 A CN109633043 A CN 109633043A
- Authority
- CN
- China
- Prior art keywords
- peak
- solution
- finger
- rhodioside
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Library & Information Science (AREA)
- Engineering & Computer Science (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention is the method for building up and its standard diagram of a kind of gadol injection HPLC finger-print, it is related to traditional Chinese medicine fingerprint analysis method, more particularly to gadol injection HPLC finger print measuring method and its obtained gadol injection preparation finger.Its step are as follows: (1) preparation of test solution.Reference solution preparation.Measuring method: taking test solution, injects high performance liquid chromatograph, obtains chromatic graph spectrum.Gained chromatogram and reference fingerprint are compareed, it is qualified product that similarity, which is greater than 0.90,.Reference fingerprint shares 6 shared peaks: peak 1, gallic acid；Peak 2, P-hydroxybenzoic acid；Peak 3, tyrosol；Peak 5(S), rhodioside；Peak 6, p-Coumaric Acid.By research, the disadvantage of existing Quality Control Technology deficiency is compensated for, keeps gadol injection quality of the pharmaceutical preparations control technology more perfect, it is also more scientific.
Description
Technical field
The present invention relates to traditional Chinese medicine fingerprint analysis methods, and in particular to the determining fingerprint pattern side gadol injection HPLC
Method and its obtained gadol injection preparation finger.
Background technique
In the prior art, cardiovascular and cerebrovascular disease is the common disease for seriously endangering human health in recent years.Due to the mankind
The raising of quality of life, cardiovascular and cerebrovascular disease are in rising trend.Cardiovascular and cerebrovascular disease is treated, although Chinese medicine list target spot action intensity
It is weaker than Western medicine, but the small advantage of multipath, multiple target point, dynamic wholistic therapy, toxic side effect then outclass Western medicine, especially curative effect
The combined therapy effect of exact Chinese patent drug is better than Western medicine.
Traditional Chinese medicine is multi-component complex system, therefore evaluates its quality and should can be provided rich using adaptable therewith
The detection method of rich authentication information, but existing the methods of microscopical characters, physical and chemical identification and assay is all not enough to solve this
One problem.
Rhodiola kirilowii Regel injection is made of rhodiola kirilowii Regel single medicinal material, is Tonghua Yusheng Medicine Co., Ltd.'s production
Exclusive product.Function with the major functions: activating microcirculation and removing stasis medicinal.Coronary heart disease stable type angina pectoris.Symptoms include: stabbing pain over the chest, colic pain are fixed
It does not move, draws on the inside of shoulder back and arm bitterly, uncomfortable in chest, palpitation and uneasiness, words are purple dark, thready and hesitant pulse.Usage and dosage: intravenous drip.Once
10ml is added in 250ml sodium chloride injection or 5% glucose injection, once a day, 10 days as one therapeutic course.
Summary of the invention
The purpose of the present invention is to provide a kind of gadol injection HPLC finger print measuring methods and its obtained
Gadol injection preparation finger.The present invention is root of kirilow rhodiola by the research to gadol injection HPLC finger-print
The quality control of injection provides a kind of new method, compensates for the disadvantage of existing Quality Control Technology deficiency, infuses root of kirilow rhodiola
It is more perfect to penetrate liquid formulation Quality Control Technology, it is also more scientific.
The technical scheme is that:
A kind of HPLC detection method of the finger-print of gadol injection, comprising the following steps:
(1) preparation of test solution: precision measures this product 0.5ml and adds water to scale in 10ml volumetric flask, shakes up, and filters
It crosses, takes subsequent filtrate to get test solution；Reference solution is accurately weighed specifically, take rhodioside reference substance, adds water system
At the solution of every 1ml 0.05mg containing rhodioside, as reference solution.
(2) measuring method: taking test solution, injects high performance liquid chromatograph, obtains chromatic graph spectrum.Wherein chromatographic condition
Are as follows:
Chromatographic column is using octadecylsilane chemically bonded silica as filler, using 0.07% phosphate aqueous solution as mobile phase A, is with acetonitrile
Mobile phase B, the regulation according to the form below carry out gradient elution, and 30 DEG C of column temperature, Detection wavelength 278nm, flow velocity 0.8ml/min,
Number of theoretical plate is calculated by rhodioside peak, should be not less than 30000.
(3) gained chromatogram and reference fingerprint are compareed, it is qualified product that similarity, which is greater than 0.90, and similarity evaluation uses
" similarity evaluation 2004A editions " is evaluated.
(4) reference fingerprint shares 6 shared peak (see figure 2)s: peak 1, gallic acid；Peak 2, P-hydroxybenzoic acid；Peak
3, tyrosol；Peak 5(S), rhodioside；Peak 6, p-Coumaric Acid.
In above scheme,
The concentration of reference substance solution described in step (1) is 50 μ g/mL.
Chromatographic column described in step (2) are as follows: Agilent XDB-C18 chromatographic column, column length 150mm, internal diameter 4.6mm,
Partial size is 5 μm.
It is accurate respectively described in step (2) to draw reference solution and each 20 μ l of test solution, liquid chromatograph is injected,
Measurement, the chromatographic peak in record 60 minutes.
It is preferred that the HPLC detection method of the finger-print of gadol injection, it is characterised in that steps are as follows:
(1) preparation of reference control solution:
Reference solution is accurately weighed specifically, take rhodioside reference substance, adds water that every 1ml 0.05mg containing rhodioside is made
Solution, as reference solution.
(2) preparation of test solution: precision measures this product 0.5ml and adds water to scale in 10ml volumetric flask, shakes up,
Filtration, takes subsequent filtrate, as test solution.
(3) accurate respectively to draw reference solution and each 20 μ l of test solution, inject high performance liquid chromatograph, record
The chromatogram of 60min to get.
Wherein chromatographic condition are as follows: using octadecylsilane chemically bonded silica as filler, Agilent XDB-C18 chromatographic column,
Column length is 150mm, and internal diameter 4.6mm, partial size is 5 μm, using 0.07% phosphate aqueous solution as mobile phase A, using acetonitrile as Mobile phase B,
Regulation progress gradient elution according to the form below, 30 DEG C of column temperature, Detection wavelength 278nm, flow velocity 0.8ml/min, number of theoretical plate
It is calculated by rhodioside peak, 30000 should be not less than.
(4) chromatogram of the gadol injection of the multiple batches of qualification of gained is fitted to by a standard control fingerprint using computer
Map.
The invention has the advantages that:
1, the present invention relates to the construction method of the HPLC finger-print of gadol injection, the preparation including test solution is right
According to the preparation of product solution, chromatographic condition is limited, and accurate respectively to draw test solution, each 20 μ l injects liquid chromatograph, according to height
The measurement of effect liquid phase chromatogram method, obtains HPLC finger-print.
2, the positive effect of the present invention is: judging the quality conformance between batch from the similarity of finger-print, may be used also
It traces to its source, finds the problems in technological operation.
3, it can effectively reflect the quality of finished product between batches, be conducive to the quality of overall monitor product, avoid matter
The unicity and one-sidedness of control are measured, and has the characteristics that convenient, fast, stable, accurate, favorable reproducibility.
4, test sample is simple for production, and chromatographic condition is easy to accomplish.
5, the peak of gadol injection finger-print obtained by the method for the present invention is more, and peak shape is good, is easy to identify, and similitude is high,
Accurately and reliably.
6, it can quantitatively compare, full figure spectrum matching, 6 points of corrections carry out similarity evaluation.
Below with reference to embodiment and attached drawing, the present invention is described further.
Detailed description of the invention
Fig. 1 is 22 batches of gadol injection finger-prints (R is reference fingerprint).
Fig. 2 is gadol injection reference fingerprint.
Fig. 3 is the finger-print and standard control trace analysis figure of 1 gadol injection of embodiment measurement.
Fig. 4 is the finger-print and standard control trace analysis figure of 2 gadol injection of embodiment measurement.
Fig. 5 is the finger-print and standard control trace analysis figure of 3 gadol injection of embodiment measurement.
Specific embodiment
For this purpose, the present invention is provided a kind of foundation of gadol injection liquid chromatogram standard finger-print and is referred to using this
The method that line map is measured the gadol injection in production and selling.
Rhodiola kirilowii Regel injection HPLC detection method, the described method comprises the following steps:
(1) preparation of reference substance solution:
Reference solution specifically: take rhodioside reference substance appropriate, it is accurately weighed, add water that every 1ml is made containing rhodioside
The solution of 0.05mg, as reference solution.The concentration of reference substance solution is 50 μ g/mL.
(2) preparation of test solution: test solution is prepared specifically: precision measures this product 0.5ml, in 10ml capacity
In bottle, scale is added water to, is shaken up, filtered, subsequent filtrate is taken, as test solution.
(3) accurate respectively to draw reference solution and each 20 μ l of test solution, inject high performance liquid chromatograph, record
The chromatogram of 60min to get.
Wherein chromatographic condition are as follows: using octadecylsilane chemically bonded silica as filler, (Agilent XDB-C18 chromatographic column,
Column length is 150mm, and internal diameter 4.6mm, partial size is 5 μm), using 0.07% phosphate aqueous solution as mobile phase A, using acetonitrile as mobile phase
B, the regulation according to the form below carry out gradient elution；30 DEG C of column temperature；Detection wavelength is 278nm, flow velocity 0.8ml/min；Theoretical plate
Number is calculated by rhodioside peak, should be not less than 30000.It is shown in Table 1.
(4) chromatogram of the gadol injection of the multiple batches of qualification of gained is fitted to by a standard control fingerprint using computer
Map.
(5) gained chromatogram and standard finger-print are compareed, it is qualified product that similarity, which is greater than 0.90, and similarity evaluation is adopted
It is evaluated with " similarity evaluation 2012 editions ".
The technical scheme is that obtained by screening, screening process is as follows:
1. instrument and reagent
1.1 instrument
Ten a ten thousandth electronic balances (METTLER TOLEDO), Shimadzu LC-20A high performance liquid chromatograph (binary geopressure gradient
Pump), Agilent Agilent XDB-C18 (4.6 × 15cm, 4.6um) chromatographic column.
1.2 reagent
Rhodioside reference substance, methanol, acetonitrile.
2. liquid chromatographic system condition:
Using octadecylsilane chemically bonded silica as filler, (Agilent XDB-C18 chromatographic column, column length 150mm, internal diameter are
4.6mm, partial size are 5 μm), using 0.07% phosphate aqueous solution as mobile phase A, using acetonitrile as Mobile phase B, regulation according to the form below into
Row gradient elution；30 DEG C of column temperature；Detection wavelength is 278nm, flow velocity 0.8ml/min；Number of theoretical plate is calculated by rhodioside peak,
30000 should be not less than.It is shown in Table 1.
3. prepared by test solution
The preparation of test solution: test solution is prepared specifically: precision measures this product 0.5ml and adds in 10ml volumetric flask
Water shakes up to scale, filters, subsequent filtrate is taken, as test solution.
4. prepared by reference solution
Take rhodioside reference substance appropriate, it is accurately weighed, add water that the solution of every 1ml 0.05mg containing rhodioside is made, as ginseng
According to object solution.
Methodological study
5.1 Precision Experiment
By standard preparation method operation preparation test solution, same test solution is taken, continuous sample introduction 6 times, presses and determines
The chromatographic condition of standard measures, and selects 6 shared peaks to be compared, selects the 5th shared peak rhodioside for base peak (S),
As a result (2.1,2.2 are shown in Table) and show each shared peak relative retention time RSD≤0.157%, each shared peak relative peak area RSD≤
1.903%, show that this method precision is good.
The experiment of 5.2 reproducibility
It takes with a collection of gadol injection, by 6 parts of test liquids of standard preparation method operation preparation, by standard chromatostrip
Part measurement, as a result (is shown in Table 2.3,2.4) and shows each shared peak relative retention time RSD≤0.172%, each shared peak is with respect to peak face
Product RSD≤0.315%.Show that this method reproducibility is preferable.
5.3 stability experiment
By standard preparation method operation preparation test liquid, same test solution is taken, respectively at 0,2,6,10,12, is pressed for 24 hours
The measurement of standard chromatographic condition, each shared peak relative retention time RSD≤0.826% that as a result (is shown in Table 2.5,2.6) are each shared
Peak relative peak area RSD≤1.631%.Show that test solution is good in internal stability for 24 hours.
The above method investigate the result shows that, this research institute establish chromatographic fingerprinting precision, reproducibility and stability
It is good, it can be analyzed with gadol injection finger-print.
6. the foundation of reference fingerprint and the analysis of batches of products fingerprint similarity
The foundation of 6.1 reference fingerprints
According to standard method, the chromatographic fingerprinting of 22 batches of rhodiola kirilowii Regel injections is analyzed, and by 22 batches of root of kirilow rhodiola
Injection chromatogram imports similarity evaluation (2012 version), and the shared peak of 6 determined carries out
Correction generates gadol injection reference fingerprint.See Fig. 1, Fig. 2.
The similarity analysis of 6.2 multiple batches of gadol injection chromatographic fingerprintings
27 batches of gadol injections are taken, are detected by the finger print measuring method of above-mentioned foundation, and by gained finger-print
With gadol injection reference fingerprint carry out full figure spectrum matching, 6 points correction, calculate each sample finger-print with compare map
Similarity.27 annotations are penetrated liquid similarity and are all larger than equal to 0.90(table 2.7), the results showed that different batches gadol injection phase
Higher like spending, finger-print similitude well illustrates process stabilizing.
The formulation of 6.3 Measurement of Similarity
The traditional Chinese medicine injection quality of active chemical group is stablized, depend primarily in gadol injection contained primary chemical at
It is grouped as the stabilization with ratio, the stabilization of this respect depends on the raw medicinal material quality of production, production technology (including mentions
Take, the processing of alcohol precipitation, active carbon, ultrafiltration etc.) reproducibility and process control (medicinal material, intermediate, filling front and back analysis and Control) three
A aspect.Result (being shown in Table 2.7) is analyzed to multiple batches of gadol injection fingerprint similarity according to this research, is considered simultaneously
To the possibility variation of mass production and acquisition crude drug source, it is more than or equal to 0.90 that Measurement of Similarity is drafted in this research.
See Fig. 1: 22 batches of gadol injection finger-prints (R is reference fingerprint).
See Fig. 2 gadol injection reference fingerprint, wherein 1. gallic acid of peak；2. P-hydroxybenzoic acid of peak；Peak
3. tyrosol；Peak 5(S) rhodioside；6. p-Coumaric Acid of peak.
7. data are analyzed
It is calculated, is obtained each by the Chinese Pharmacopoeia committee " chromatographic fingerprints of Chinese materia medica similarity evaluation software " version in 2012
Batch similarity value.Sample similarity is 0.910~0.972.
Embodiment
Determining fingerprint pattern is carried out to gadol injection, the specific steps are as follows:
The preparation of step (1) reference control solution:
Reference solution is accurately weighed specifically, take rhodioside reference substance appropriate, adds water that every 1ml is made containing rhodioside
The solution of 0.05mg, as reference solution.
The preparation of step (2) test solution: test solution is prepared specifically: precision measures this product 0.5ml, in 10ml
In volumetric flask, scale is added water to, is shaken up, filters, subsequent filtrate is taken, as test solution；
Step (3) is accurate respectively to draw reference solution and each 20ml of test solution, injects high performance liquid chromatograph, record
The chromatogram of 60min to get.
Wherein chromatographic condition are as follows: using octadecylsilane chemically bonded silica as filler, (Agilent XDB-C18 chromatographic column,
Column length is 150mm, and internal diameter 4.6mm, partial size is 5 μm), using 0.07% phosphate aqueous solution as mobile phase A, using acetonitrile as mobile phase
B, the regulation according to the form below carry out gradient elution；30 DEG C of column temperature；Detection wavelength is 278nm, flow velocity 0.8ml/min；Theoretical plate
Number is calculated by rhodioside peak, should be not less than 30000.
Reference fingerprint is shown in Fig. 2,1. gallic acid of peak；2. P-hydroxybenzoic acid of peak；3. tyrosol of peak；Peak 5(S) the red scape of
Its glycosides；6. p-Coumaric Acid of peak.By the Chinese Pharmacopoeia committee " chromatographic fingerprints of Chinese materia medica similarity evaluation software " version in 2012
It is calculated, compares the similarity of the finger-print of reference fingerprint and said determination, similarity is being greater than 0.90 for qualification.
Embodiment 1 carries out determining fingerprint pattern to 1001190105 batch of gadol injection, the specific steps are as follows: step (1) ginseng
Than the preparation of reference substance solution: reference solution is accurately weighed specifically, take rhodioside reference substance appropriate, and water is added to be made often
The solution of 1ml 0.05mg containing rhodioside, as reference solution.The preparation of step (2) test solution: test sample is prepared
Solution specifically: precision measures this product 0.5ml and adds water to scale in 10ml volumetric flask, shakes up, and filters, takes subsequent filtrate, makees
For test solution.Step (3) is accurate respectively to draw reference solution and each 20ml of test solution, injects high-efficient liquid phase color
Spectrometer, record the chromatogram of 60min to get.Wherein chromatographic condition are as follows: using octadecylsilane chemically bonded silica as filler,
(Agilent XDB-C18 chromatographic column, column length 150mm, internal diameter 4.6mm, partial size are 5 μm) is with 0.07% phosphate aqueous solution
Mobile phase A, using acetonitrile as Mobile phase B, the regulation according to the form below carries out gradient elution；30 DEG C of column temperature；Detection wavelength is 278nm,
Flow velocity is 0.8ml/min；Number of theoretical plate is calculated by rhodioside peak, should be not less than 30000.
Reference fingerprint is shown in Fig. 2,1. gallic acid of peak；2. P-hydroxybenzoic acid of peak；3. tyrosol of peak；Peak 5(S) the red scape of
Its glycosides；6. p-Coumaric Acid of peak.By the Chinese Pharmacopoeia committee " chromatographic fingerprints of Chinese materia medica similarity evaluation software " version in 2012 into
Row calculates, and compares the similarity of the finger-print of reference fingerprint and said determination, and similarity is being greater than 0.90 for qualification.Phase
3-1 is shown in Table like degree calculated result.
Test result: the finger-print and standard control trace analysis of 1001190105 batch gadol injections measurement are (see figure
3), similarity 0.950 meets the requirement not less than 0.90.
Embodiment 2
Determining fingerprint pattern is carried out to 1001190106 batch of gadol injection, the specific steps are as follows:
The preparation of step (1) reference control solution:
Reference solution is accurately weighed specifically, take rhodioside reference substance appropriate, adds water that every 1ml is made containing rhodioside
The solution of 0.05mg, as reference solution.
The preparation of step (2) test solution: test solution is prepared specifically: precision measures this product 0.5ml, in 10ml
In volumetric flask, scale is added water to, is shaken up, filters, subsequent filtrate is taken, as test solution.
Step (3) is accurate respectively to draw reference solution and each 20ml of test solution, injects high performance liquid chromatograph, note
Record 60min chromatogram to get.
Wherein chromatographic condition are as follows: using octadecylsilane chemically bonded silica as filler, (Agilent XDB-C18 chromatographic column,
Column length is 150mm, and internal diameter 4.6mm, partial size is 5 μm), using 0.07% phosphate aqueous solution as mobile phase A, using acetonitrile as mobile phase
B, the regulation according to the form below carry out gradient elution；30 DEG C of column temperature；Detection wavelength is 278nm, flow velocity 0.8ml/min；Theoretical plate
Number is calculated by rhodioside peak, should be not less than 30000.
Reference fingerprint is shown in Fig. 2,1. gallic acid of peak；2. P-hydroxybenzoic acid of peak；3. tyrosol of peak；Peak 5(S) the red scape of
Its glycosides；6. p-Coumaric Acid of peak.
It is calculated, is compared by the Chinese Pharmacopoeia committee " chromatographic fingerprints of Chinese materia medica similarity evaluation software " version in 2012
The similarity of the finger-print of reference fingerprint and said determination, similarity are being greater than 0.90 for qualification.Similarity calculation knot
Fruit is shown in Table 3-2.
Test result: the finger-print and standard control trace analysis of 1001190106 batch gadol injections measurement are (see figure
4), similarity 0.934 meets the requirement not less than 0.90.Embodiment 3 to 1001190107 batch of gadol injection into
Row determining fingerprint pattern, the specific steps are as follows: the preparation of step (1) reference control solution: reference solution is specifically, take
Rhodioside reference substance is appropriate, accurately weighed, adds water that the solution of every 1ml 0.05mg containing rhodioside is made, molten as object of reference
Liquid.The preparation of step (2) test solution: test solution is prepared specifically: precision measures this product 0.5ml, in 10ml capacity
In bottle, scale is added water to, is shaken up, filtered, subsequent filtrate is taken, as test solution.Step (3) is accurate respectively to draw object of reference
Solution and each 20ml of test solution, inject high performance liquid chromatograph, record the chromatogram of 60min to get.Wherein chromatostrip
Part are as follows: using octadecylsilane chemically bonded silica as filler, (Agilent XDB-C18 chromatographic column, column length 150mm, internal diameter are
4.6mm, partial size are 5 μm), using 0.07% phosphate aqueous solution as mobile phase A, using acetonitrile as Mobile phase B, regulation according to the form below into
Row gradient elution；30 DEG C of column temperature；Detection wavelength is 278nm, flow velocity 0.8ml/min；Number of theoretical plate is calculated by rhodioside peak,
30000 should be not less than.
Reference fingerprint is shown in Fig. 2: 1. gallic acid of peak；2. P-hydroxybenzoic acid of peak；3. tyrosol of peak；Peak 5(S) the red scape of
Its glycosides；6. p-Coumaric Acid of peak.
It is calculated, is compared by the Chinese Pharmacopoeia committee " chromatographic fingerprints of Chinese materia medica similarity evaluation software " version in 2012
The similarity of the finger-print of reference fingerprint and said determination, similarity are being greater than 0.90 for qualification.Similarity calculation knot
Fruit is shown in Table 3-3.
Test result: the finger-print and standard control trace analysis of 1001190107 batch gadol injections measurement are (see figure
5), similarity 0.966 meets the requirement not less than 0.0.90.
Claims (5)
1. a kind of HPLC detection method of the finger-print of gadol injection, comprising the following steps:
(1) preparation of test solution: precision measures this product 0.5ml and adds water to scale in 10ml volumetric flask, shakes up, and filters
It crosses, takes subsequent filtrate to get test solution；Reference solution is accurately weighed specifically, take rhodioside reference substance, adds water system
At the solution of every 1ml 0.05mg containing rhodioside, as reference solution；
(2) measuring method: taking test solution, injects high performance liquid chromatograph, obtains chromatic graph spectrum；Wherein chromatographic condition are as follows:
Chromatographic column is using octadecylsilane chemically bonded silica as filler, using 0.07% phosphate aqueous solution as mobile phase A, is with acetonitrile
Mobile phase B, the regulation according to the form below carry out gradient elution, and 30 DEG C of column temperature, Detection wavelength 278nm, flow velocity 0.8ml/min,
Number of theoretical plate is calculated by rhodioside peak, should be not less than 30000；
Gained chromatogram and reference fingerprint are compareed, it is qualified product that similarity, which is greater than 0.90, and similarity evaluation uses " Chinese medicine
Chromatographic fingerprinting similarity evaluation system 2004A editions " it is evaluated；
Reference fingerprint shares 6 shared peaks: peak 1, gallic acid；Peak 2, P-hydroxybenzoic acid；Peak 3, tyrosol；Peak 5
(S), rhodioside；Peak 6, p-Coumaric Acid.
2. the HPLC detection method of the finger-print of gadol injection according to claim 1, it is characterised in that: step
(1) concentration of reference substance solution described in is 50 μ g/mL.
3. the HPLC detection method of the finger-print of gadol injection according to claim 1, it is characterised in that: step
(2) chromatographic column described in are as follows: Agilent XDB-C18 chromatographic column, column length 150mm, internal diameter 4.6mm, partial size are 5 μm.
4. the HPLC detection method of the finger-print of gadol injection according to claim 1, it is characterised in that: step
(2) accurate respectively described in draw reference solution and each 20 μ l of test solution, inject liquid chromatograph, measurement, record 60
Chromatographic peak in minute.
5. the HPLC detection method of the finger-print of gadol injection according to claim 1, it is characterised in that step
It is as follows:
(1) preparation of reference control solution:
Reference solution is accurately weighed specifically, take rhodioside reference substance, adds water that every 1ml 0.05mg containing rhodioside is made
Solution, as reference solution；
(2) preparation of test solution: precision measures this product 0.5ml and adds water to scale in 10ml volumetric flask, shakes up, and filters
It crosses, takes subsequent filtrate, as test solution；
(3) accurate respectively to draw reference solution and each 20 μ l of test solution, high performance liquid chromatograph is injected, 60min is recorded
Chromatogram to get；
Wherein chromatographic condition are as follows: using octadecylsilane chemically bonded silica as filler, Agilent XDB-C18 chromatographic column, column length
For 150mm, internal diameter 4.6mm, partial size is 5 μm, using 0.07% phosphate aqueous solution as mobile phase A, using acetonitrile as Mobile phase B, is pressed
Regulation in table carries out gradient elution, and 30 DEG C of column temperature, Detection wavelength 278nm, flow velocity 0.8ml/min, number of theoretical plate is by red
Red-spotted stonecrop glycosides peak calculates, and should be not less than 30000；
(4) chromatogram of the gadol injection of the multiple batches of qualification of gained is fitted to by a standard control fingerprint using computer
Map.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910147591.8A CN109633043A (en) | 2019-02-27 | 2019-02-27 | A kind of method for building up and its standard diagram of gadol injection HPLC finger-print |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910147591.8A CN109633043A (en) | 2019-02-27 | 2019-02-27 | A kind of method for building up and its standard diagram of gadol injection HPLC finger-print |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109633043A true CN109633043A (en) | 2019-04-16 |
Family
ID=66066142
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910147591.8A Pending CN109633043A (en) | 2019-02-27 | 2019-02-27 | A kind of method for building up and its standard diagram of gadol injection HPLC finger-print |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109633043A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110716000A (en) * | 2019-11-18 | 2020-01-21 | 吉林大学 | Method for measuring content of p-hydroxyphenylacetic acid in rhodiola crenulata injection |
| CN112213431A (en) * | 2019-07-10 | 2021-01-12 | 贵州广济堂药业有限公司 | Detection method and quality control method of rhodiola rosea wall-broken decoction pieces |
| CN115032311A (en) * | 2022-07-11 | 2022-09-09 | 景忠山国药（唐山）有限公司 | Xinnaoxin medicine component content determination method based on one-measurement-multiple evaluation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091118A (en) * | 2010-03-09 | 2011-06-15 | 成都中医药大学 | Quality detection method for rhodiola crenulata |
| CN102998383A (en) * | 2012-11-12 | 2013-03-27 | 江苏康缘药业股份有限公司 | Method for testing content of main components in Rhodiola rosea extracts |
| WO2017148426A1 (en) * | 2016-03-03 | 2017-09-08 | 石家庄以岭药业股份有限公司 | Method for determining fingerprint of chinese medicine composition |
| CN107543889A (en) * | 2016-06-28 | 2018-01-05 | 江苏康缘药业股份有限公司 | A kind of rhodiola kirilowii Regel capsule fingerprint pattern and its construction method |
-
2019
- 2019-02-27 CN CN201910147591.8A patent/CN109633043A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091118A (en) * | 2010-03-09 | 2011-06-15 | 成都中医药大学 | Quality detection method for rhodiola crenulata |
| CN102998383A (en) * | 2012-11-12 | 2013-03-27 | 江苏康缘药业股份有限公司 | Method for testing content of main components in Rhodiola rosea extracts |
| WO2017148426A1 (en) * | 2016-03-03 | 2017-09-08 | 石家庄以岭药业股份有限公司 | Method for determining fingerprint of chinese medicine composition |
| CN107543889A (en) * | 2016-06-28 | 2018-01-05 | 江苏康缘药业股份有限公司 | A kind of rhodiola kirilowii Regel capsule fingerprint pattern and its construction method |
Non-Patent Citations (2)
| Title |
|---|
| 姚令文 等: "大株红景天注射液指纹图谱研究", 《中国药事》 * |
| 杨胜岩 等: "红景天注射液HPLC指纹图谱研究", 《天津医科大学学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112213431A (en) * | 2019-07-10 | 2021-01-12 | 贵州广济堂药业有限公司 | Detection method and quality control method of rhodiola rosea wall-broken decoction pieces |
| CN110716000A (en) * | 2019-11-18 | 2020-01-21 | 吉林大学 | Method for measuring content of p-hydroxyphenylacetic acid in rhodiola crenulata injection |
| CN110716000B (en) * | 2019-11-18 | 2021-12-10 | 吉林大学 | Method for measuring content of p-hydroxyphenylacetic acid in rhodiola crenulata injection |
| CN115032311A (en) * | 2022-07-11 | 2022-09-09 | 景忠山国药（唐山）有限公司 | Xinnaoxin medicine component content determination method based on one-measurement-multiple evaluation method |
| CN115032311B (en) * | 2022-07-11 | 2024-03-22 | 景忠山国药（唐山）有限公司 | Method for measuring content of Xinnaoxin medicine components based on one-measurement-multiple-evaluation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109633043A (en) | A kind of method for building up and its standard diagram of gadol injection HPLC finger-print | |
| CN103728387B (en) | Ginseng-astragalus blood-sugar lowering preparation HPLC standard finger-print and construction method thereof | |
| CN109001346A (en) | The method for building up and its finger-print of wuwei xiaodu drink preparation finger | |
| CN110780007B (en) | Method for evaluating 6 component contents of mango cough relieving tablet by HPLC (high performance liquid chromatography) method | |
| CN102445514A (en) | Detection method of traditional Chinese medicine preparation jinshuibao capsule | |
| CN111537630A (en) | Method for establishing HPLC fingerprint spectrum and multi-index quantification of gynecological reconstruction pill | |
| CN110568099B (en) | Fingerprint spectrum construction method of radix acanthopanacis senticosi, radix angelicae sinensis and radix astragali refining agent and multi-index component synchronous content determination method | |
| CN109709222B (en) | Component detection method of Ganmaoling and compound Ganmaoling | |
| CN116879424A (en) | Method for measuring content of terprivet glycoside in shengxuebao preparation | |
| CN104569217B (en) | The method for building up of gold Rong Xiaopi Granules finger-print | |
| CN113092640B (en) | Method for detecting benzyl alcohol and benzaldehyde in heparin sodium injection | |
| CN111487351B (en) | Method for detecting fingerprint of blood-activating pain-relieving capsule | |
| CN104155399A (en) | Quality control method of four-time treated rhizoma cyperi decoction pieces | |
| CN114577918A (en) | Ultra-high performance liquid chromatography detection method for active ingredient content and fingerprint spectrum of compound sophora flavescens injection | |
| CN115184490B (en) | Establishment method and application of HPLC standard fingerprint of Hirudo vein relaxing capsule | |
| CN110118841A (en) | A kind of construction method of the HPLC characteristic spectrum of oral liquid for clearing liver and gallbladder | |
| CN111413429A (en) | Detection method of gardenia intermediate and fingerprint spectrum construction method thereof | |
| CN107632075A (en) | Golden three kinds of component contents of bavin KANGGAN JIAONANG while assay method and its HPLC fingerprint map construction methods | |
| CN110196299A (en) | The finger-print of diplopia ' Yanming ' capsules for clearing and its application in quality control and constituent analysis | |
| CN113391003B (en) | Method for simultaneously detecting content of active ingredients in pulse-activating decoction | |
| CN114216995B (en) | Fingerprint detection method for traditional Chinese medicine ointment | |
| CN113125620B (en) | Fingerprint detection method of traditional Chinese medicine composition with kidney tonifying and yang strengthening effects | |
| CN113219095B (en) | Construction method of fingerprint of Fukean tablet and fingerprint thereof | |
| CN112268968B (en) | Detection method of fingerprint spectrum of medicinal preparation | |
| CN116953105A (en) | Construction method of HPLC fingerprint spectrum of snake medicinal liquor and component content determination method thereof |
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: 20190416 |