CN105548385A - Determination method for liquid-phase fingerprint of Xingnaojing injection and standard fingerprint of Xingnaojing injection - Google Patents
Determination method for liquid-phase fingerprint of Xingnaojing injection and standard fingerprint of Xingnaojing injection Download PDFInfo
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- CN105548385A CN105548385A CN201510907241.9A CN201510907241A CN105548385A CN 105548385 A CN105548385 A CN 105548385A CN 201510907241 A CN201510907241 A CN 201510907241A CN 105548385 A CN105548385 A CN 105548385A
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- 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
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- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The invention relates to a determination method for the fingerprint of a traditional Chinese medicine preparation, specifically to a determination method for the liquid-phase fingerprint of a Xingnaojing injection. The determination method comprises the following steps: preparation of a test solution; preparation of a control solution; determination with a liquid chromatograph; and processing of data and the fingerprint. The invention also relates to the liquid-phase fingerprint of the Xingnaojing injection obtained by using the method. The method is simple, convenient, fast, accurate, stable and reliable, can be combined with the liquid-phase fingerprint of the Xingnaojing injection for quality control of a Xingnaojing injection sample and can more comprehensively, objectively and scientifically evaluate the quality of the Xingnaojing injection and guarantee validity of the Xingnaojing injection.
Description
Technical field
The present invention relates to traditional Chinese medicine fingerprint analytical approach, be specifically related to XINGNAOJING ZHUSHEYE liquid-phase fingerprint assay method, and the XINGNAOJING ZHUSHEYE liquid-phase fingerprint obtained.
Background technology
China's traditional Chinese medicine compound preparation complicated component, in run-of-the-mill standard, assay only relates to 1 ~ 3 composition of monarch drug in a prescription in prescription, be difficult to effectively control its inherent quality, thus security, the validity of medication cannot be ensured, especially through the traditional Chinese medicine of intravenous route medication, existing quality standard cannot ensure its security.Therefore only have the quality standard research constantly carrying out science, progressively could meet the requirement of Chinese medicine and Chinese medicine development, real accomplishes " safely, effectively, stable, controlled ".
XINGNAOJING ZHUSHEYE is by Moschus, borneol, root tuber of aromatic turmeric and the cape jasmine herbal mixture parenteral solution through steam distillation Hydrolysis kinetics; firstly appeared the seventies in last century, prescription is cut out by the Pelleting of traditional Chinese medical science recipe 'An Gong Niu Huang Wan ' and obtains, and has clearing heat and detoxicating; cooling and activating blood, inducing resuscitation effect.Its quality standard State Food and Drug Administration national drug mark WS
3-B-3353-98-2003, wherein differentiate the discriminating comprising Moschus, assay only has the detection of borneol.
The bibliographical information of existing XINGNAOJING ZHUSHEYE quality control, all for quality control index with muskone and/or borneol, detection method is mainly vapor-phase chromatography (GC) and gas chromatography mass spectrometry method (GC-MS), only has 1 section of document to adopt HPLC method to measure the content of muskone in Xingnaojing.And patent (number of patent application 200910186698.X) only sets up the fingerprint spectrum method that a kind of gas phase measures, in this finger-print, the total content of muskone and borneol account for total peak area 90% on, the information of other compositions is covered more; And liquid phase chromatography effectively can eliminate the adverse effect that muskone and borneol too high levels cause.And in theory, all chemical compositions all should have some pharmacologically active, and the effect in whole prescription or preparation of acting on of often micro constitutent holds the balance.
Based on this, the present invention adopts high-efficient liquid phase technique to establish the finger-print of XINGNAOJING ZHUSHEYE first, has a comprehensively understanding to the chemical composition general picture of this parenteral solution.Simultaneously in production run, gas-phase fingerprint pattern and liquid-phase fingerprint use jointly, can further improve the quality controllable sexual demand of preparation, meet " safely, effectively, stable, controlled " of preparation.
Summary of the invention
The object of the present invention is to provide a kind of assay method and standard finger-print thereof of XINGNAOJING ZHUSHEYE liquid-phase fingerprint.
The present invention is by the research to XINGNAOJING ZHUSHEYE liquid-phase fingerprint, provide the method for composition quality in a kind of Fast Evaluation said preparation, compensate for the shortcoming of the deficiency of existing Quality Control Technology, make XINGNAOJING ZHUSHEYE Quality Control Technology more perfect, also more science.
The liquid-phase fingerprint assay method of a kind of XINGNAOJING ZHUSHEYE of the present invention, comprises the following steps
An active constituent content measuring method for XINGNAOJING ZHUSHEYE, comprises the following steps:
1) preparation of need testing solution: get XINGNAOJING ZHUSHEYE 3 ~ 5, incline and content, mixing, accurate absorption 5 ~ 10mL, pass through solid phase extraction column, efflux discards, and with 1 ~ 5mL organic solvent wash-out, collects eluent, put in 1 ~ 5mL measuring bottle, add organic solvent to scale, shake up, as need testing solution;
2) preparation of reference substance solution: take eucarvone, camphor, curdione, germacrone, turmeric ketenes, curzerenone and Curcumenol reference substance respectively appropriate, be placed in volumetric flask, add organic solvent dissolution and be diluted to scale, making mixing reference substance solution;
3) assay method: draw reference substance solution and need testing solution respectively, injection liquid chromatography, obtains chromatic graph spectrum, calculates the active constituent content in need testing solution according to chromatogram;
Chromatographic system condition wherein: chromatographic column: C
18post; Mobile phase: acetonitrile (A)-aqueous formic acid (B) gradient elution, flow velocity 1.0 ~ 2.0mL/min; Determined wavelength 254nm; Column temperature 30 ~ 40 DEG C,
Elution requirement: 0-5min, 40%A; 5-50min, 40%-60%A; 50-60min, 60%-100%A; 60-65min, 100%A; 65.01-75min, 40%A.
Wherein, step 1) in solid phase extraction column used be selected from C
18or C
8solid phase extraction column.
Wherein, step 1) and step 2) organic solvent used is selected from: the organic solvents such as methyl alcohol, ethanol, acetonitrile, normal hexane.
Wherein, step 3) aqueous formic acid concentration is 0.01 ~ 0.05%.
Preferably, assay method, comprises the following steps:
1) preparation of need testing solution: get XINGNAOJING ZHUSHEYE 3 ~ 5, incline and content, mixing, accurate absorption 5mL, passes through C
8solid phase extraction column, efflux discards, and uses 1mL methanol-eluted fractions, collects eluent, puts in 1mL measuring bottle, add methyl alcohol to scale, shake up, as need testing solution;
2) preparation of reference substance solution: take eucarvone, camphor, curdione, germacrone, turmeric ketenes, curzerenone and Curcumenol reference substance respectively appropriate, be placed in same volumetric flask, add methyl alcohol dissolve and be diluted to scale, make eucarvone, camphor, curdione, germacrone, turmeric ketenes, curzerenone and Curcumenol after suitably diluting, obtain the single reference substance solution of final mass concentration between 0.1mg/mL ~ 1.0mg/mL;
3) assay method: draw reference substance solution and need testing solution respectively, injection liquid chromatography, obtains chromatic graph spectrum, calculates the active constituent content in need testing solution according to chromatogram;
Wherein, liquid chromatographic system condition:
Chromatographic column: C
18(4.6mm × 250mm, 5 μm); Mobile phase: acetonitrile (A)-0.02% aqueous formic acid (B) gradient elution, elution requirement: 0-5min, 40%A; 5-50min, 40%-60%A; 50-60min, 60%-100%A; 60-65min, 100%A; 65.01-75min, 40%A; Flow velocity 1.0mL/min; Determined wavelength 254nm; Column temperature 35 DEG C; Sample size: 20 μ L.
The present invention further provides a kind of method for building up of XINGNAOJING ZHUSHEYE liquid phase standard diagram, step is as follows:
1) get multiple batches of qualified XINGNAOJING ZHUSHEYE, incline and content, mixing, accurate absorption 5mL, passes through C
8solid phase extraction column, efflux discards, and uses 1mL methanol-eluted fractions, collects eluent, puts in 1mL measuring bottle, add methyl alcohol to scale, shake up, as need testing solution;
2) draw need testing solution, injection liquid chromatography, obtain chromatic graph spectrum, according to the chromatogram of many batches of obtained specification product, return 11 XINGNAOJING ZHUSHEYE standard control liquid-phase fingerprint with finger-print software, wherein absorption peak adds up to 11;
Wherein, the chromatographic condition of described liquid chromatography is as follows:
Chromatographic column: C
18(4.6mm × 250mm, 5 μm); Mobile phase: acetonitrile (A)-0.02% aqueous formic acid (B) gradient elution, elution requirement: 0-5min, 40%A; 5-50min, 40%-60%A; 50-60min, 60%-100%A; 60-65min, 100%A; 65.01-75min, 40%A; Flow velocity 1.0mL/min; Determined wavelength 254nm; Column temperature 35 DEG C; Sample size: 20 μ L.
Assay method of the present invention is through screening acquisition, and screening process is as follows:
1. instrument and reagent
1.1 instrument
Japan Shimadzu LC-20AT high performance liquid chromatograph (SIL-20A automatic sampler, CTO-10AS column oven, detecting device: SPD-M20A), Labsolutions chromatographic work station; 1/10 ten thousand electronic analytical balance (plum Teller-Tuo benefit Instrument Ltd., Switzerland).
1.2 reagent
Curdione (lot number E-009-110603) and germacrone (lot number 111665-201103) are purchased from Bi Site bio tech ltd, Chengdu.Camphor (lot number Z-018-140801) is purchased from Rui Fensi bio tech ltd, Chengdu.Eucarvone (2,6,6-trimethyl-2,4-cycloheptene-1-ketone), turmeric ketenes, Curcumenol and curzerenone are made by oneself by this laboratory, determine structure through NMR and MS.Above reference substance measures purity >98% through HPLC.
2. chromatographic system condition:
Chromatographic column: C
18(4.6mm × 250mm, 5 μm); Mobile phase: acetonitrile (A)-0.02% aqueous formic acid (B) gradient elution, elution requirement: 0-5min, 40%A; 5-50min, 40%-60%A; 50-60min, 60%-100%A; 60-65min, 100%A; 65.01-75min, 40%A; Flow velocity 1.0mL/min; Determined wavelength 254nm; Column temperature 35 DEG C; Sample size: 20 μ L.
3. need testing solution preparation
Get XINGNAOJING ZHUSHEYE 3 ~ 5, incline and content, mixing, accurate absorption 5mL, passes through C
8solid phase extraction column, efflux discards, and uses 1mL methanol-eluted fractions, collects eluent, puts in 1mL measuring bottle, add methyl alcohol to scale, shake up, as need testing solution.
4. reference substance solution preparation
Precision takes eucarvone, camphor, curdione, germacrone, turmeric ketenes, curzerenone and Curcumenol reference substance in right amount respectively, is placed in same volumetric flask, adds methyl alcohol and dissolve and be diluted to scale, make certain density mixing reference substance solution.
5. Method validation
5.1 stability test
Same lot number XINGNAOJING ZHUSHEYE (120107) need testing solution of accurate absorption, by chromatographic condition respectively at sample introduction analysis in 0h, 2h, 4h, 6h, 12h and 24h after sample preparation hour, record chromatogram.The relative retention time at each total peak and the RSD of relative peak area are all less than 3% (n=6), and result illustrates having good stability of test sample.
5.2 precision test
Accurate draw same lot number XINGNAOJING ZHUSHEYE (120107) need testing solution, according to chromatographic condition continuous sample introduction 6 times, record chromatogram.The relative retention time at each total peak and the RSD of relative peak area are all less than 3% (n=6), and result illustrates that the precision of instrument is good.
5.3 replica test
Get same lot number XINGNAOJING ZHUSHEYE (120107) need testing solution, each precision draws 6 parts, prepares need testing solution respectively, sample detection, record chromatogram.The relative retention time at each total peak and the RSD of relative peak area are all less than 3% (n=6), and the repeatability of result illustration method is good.
5.4 sample determination
21 batches of XINGNAOJING ZHUSHEYEs are pressed test sample extracting method to extract, and measure by this finger print measuring method, record each chromatogram.
6. data analysis
Calculate by the Chinese Pharmacopoeia council " chromatographic fingerprints of Chinese materia medica similarity evaluation software " version in 2012, obtain each batch of Similarity value.Sample similarity is 0.95 ~ 0.99.From similarity result, between different batches sample, difference is less.
The screening of chromatographic condition of the present invention:
(1) selection of chromatographic column:
Select ThermoBDSHypersilC
18(4.6mm × 250mm, 5 μm), Topsil-TMC
18(4.6mm × 250mm, 5 μm), DikmaspursilC
18(4.6mm × 250mm, 5 μm), WatersxtcrraC
18(4.6mm × 250mm, 5 μm) carry out serviceability test, and chromatographic column has impact to its degree of separation, wherein WatersxtcrraC
18(4.6mm × 250mm, 5 μm) and ThermoBDSHypersilC
18(4.6mm × 250mm, 5 μm), the separating effect of two kinds of chromatographic columns is better.
(2) selection of mobile phase: select pure acetonitrile, pure methyl alcohol, methanol-water, acetonitrile-water, the mobile phases such as acetonitrile-aqueous formic acid, carry out gradient elution, find that acetonitrile-aqueous formic acid separating effect is better, therefore select this mobile phase.
(3) selection of elution requirement: the present invention adopts the mobile phases such as acetonitrile-aqueous formic acid, and elution requirement adopts isocratic elution respectively, finds that its degree of separation cannot reach expection; After adopting gradient elution, can realize the separation of effective constituent, the final elution requirement selected is: 0-5min, 40%A; 5-50min, 40%-60%A; 50-60min, 60%-100%A; 60-65min, 100%A; 65.01-75min, 40%A;
Compared with prior art, the present invention has the following advantages in the present invention:
1, the present invention adopts liquid phase chromatography, and in the XINGNAOJING ZHUSHEYE liquid-phase fingerprint of foundation, total peak amounts to 11, can effectively characterize XINGNAOJING ZHUSHEYE composition quality, supplement the composition beyond gas-phase fingerprint pattern and assay.
2, liquid phase chromatography effectively can eliminate the adverse effect that muskone and borneol too high levels cause, and reacts other composition situations except muskone and borneol more accurately.
3, finger-print is focused on each and is formed the mutual relationship at fingerprint characteristic peak, more holistic feature, avoids the assessment of individual chemical composition and the one-sidedness of total quality that causes.
4, the present invention adopts solid phase extraction column to carry out sample pretreatment, simple aspect, is beneficial to operation; And can the accuracy of ensuring method.
5, this method has precision, stability, reproducible advantage, and easy, quick, accurate, stable, reliable, can be used for XINGNAOJING ZHUSHEYE quality control.
Below in conjunction with embodiment and accompanying drawing, the present invention is described further.
Accompanying drawing explanation
Fig. 1 XINGNAOJING ZHUSHEYE standard liquid-phase fingerprint
Fig. 2 XINGNAOJING ZHUSHEYE reference substance collection of illustrative plates
Fig. 3 XINGNAOJING ZHUSHEYE 21 batches of liquid-phase fingerprints
Embodiment
Below in conjunction with embodiment, the present invention is further described, to do more detailed understanding to the present invention.
Embodiment 1
1) preparation of need testing solution: get XINGNAOJING ZHUSHEYE 3 ~ 5, incline and content, mixing, accurate absorption 5mL, passes through C
8solid phase extraction column, efflux discards, and uses 1mL methanol-eluted fractions, collects eluent, puts in 1mL measuring bottle, add methyl alcohol to scale, shake up, as need testing solution;
2) preparation of reference substance solution: take eucarvone, camphor, curdione, germacrone, turmeric ketenes, curzerenone and Curcumenol reference substance respectively appropriate, be placed in same volumetric flask, add methyl alcohol dissolve and be diluted to scale, make eucarvone, camphor, curdione, germacrone, turmeric ketenes, curzerenone and Curcumenol after suitably diluting, obtain the single reference substance solution of final mass concentration between 0.1mg/mL ~ 1.0mg/mL;
3) assay method: draw reference substance solution and need testing solution respectively, injection liquid chromatography, obtains chromatic graph spectrum, calculates the active constituent content in need testing solution according to chromatogram;
Wherein, liquid chromatographic system condition:
Chromatographic column: C
18(4.6mm × 250mm, 5 μm); Mobile phase: acetonitrile (A)-0.02% aqueous formic acid (B) gradient elution, elution requirement: 0-5min, 40%A; 5-50min, 40%-60%A; 50-60min, 60%-100%A; 60-65min, 100%A; 65.01-75min, 40%A; Flow velocity 1.0mL/min; Determined wavelength 254nm; Column temperature 35 DEG C; Sample size: 20 μ L.
Claims (6)
1. an active constituent content measuring method for XINGNAOJING ZHUSHEYE, comprises the following steps:
1) preparation of need testing solution: get XINGNAOJING ZHUSHEYE 3 ~ 5, incline and content, mixing, accurate absorption 5 ~ 10mL, pass through solid phase extraction column, efflux discards, and with 1 ~ 5mL organic solvent wash-out, collects eluent, put in 1 ~ 5mL measuring bottle, add organic solvent to scale, shake up, as need testing solution;
2) preparation of reference substance solution: take eucarvone, camphor, curdione, germacrone, turmeric ketenes, curzerenone and Curcumenol reference substance respectively appropriate, be placed in volumetric flask, add organic solvent dissolution and be diluted to scale, making mixing reference substance solution;
3) assay method: draw reference substance solution and need testing solution respectively, injection liquid chromatography, obtains chromatic graph spectrum, calculates the active constituent content in need testing solution according to chromatogram;
Chromatographic system condition wherein: chromatographic column: C
18post; Mobile phase: acetonitrile (A)-aqueous formic acid (B) gradient elution, flow velocity 1.0 ~ 2.0mL/min; Determined wavelength 254nm; Column temperature 30 ~ 40 DEG C,
Elution requirement: 0-5min, 40%A; 5-50min, 40%-60%A; 50-60min, 60%-100%A; 60-65min, 100%A; 65.01-75min, 40%A.
2. assay method according to claim 1, is characterized in that: step 1) in solid phase extraction column used be selected from C
18or C
8solid phase extraction column.
3. assay method according to claim 1, is characterized in that: step 1) and step 2) organic solvent used is selected from: the organic solvents such as methyl alcohol, ethanol, acetonitrile, normal hexane.
4. assay method according to claim 1, is characterized in that: step 3) aqueous formic acid concentration is 0.01 ~ 0.05%.
5. assay method according to claim 1, is characterized in that, comprise the following steps:
1) preparation of need testing solution: get XINGNAOJING ZHUSHEYE 3 ~ 5, incline and content, mixing, accurate absorption 5mL, passes through C
8solid phase extraction column, efflux discards, and uses 1mL methanol-eluted fractions, collects eluent, puts in 1mL measuring bottle, add methyl alcohol to scale, shake up, as need testing solution;
2) preparation of reference substance solution: take eucarvone, camphor, curdione, germacrone, turmeric ketenes, curzerenone and Curcumenol reference substance respectively appropriate, be placed in same volumetric flask, add methyl alcohol dissolve and be diluted to scale, make eucarvone, camphor, curdione, germacrone, turmeric ketenes, curzerenone and Curcumenol after suitably diluting, obtain the single reference substance solution of final mass concentration between 0.1mg/mL ~ 1.0mg/mL;
3) assay method: draw reference substance solution and need testing solution respectively, injection liquid chromatography, obtains chromatic graph spectrum, calculates the active constituent content in need testing solution according to chromatogram;
Wherein, liquid chromatographic system condition:
Chromatographic column: C
18(4.6mm × 250mm, 5 μm); Mobile phase: acetonitrile (A)-0.02% aqueous formic acid (B) gradient elution, elution requirement: 0-5min, 40%A; 5-50min, 40%-60%A; 50-60min, 60%-100%A; 60-65min, 100%A; 65.01-75min, 40%A; Flow velocity 1.0mL/min; Determined wavelength 254nm; Column temperature 35 DEG C; Sample size: 20 μ L.
6. a method for building up for XINGNAOJING ZHUSHEYE liquid phase standard diagram, is characterized in that, step is as follows:
1) get multiple batches of qualified XINGNAOJING ZHUSHEYE, incline and content, mixing, accurate absorption 5mL, passes through C
8solid phase extraction column, efflux discards, and uses 1mL methanol-eluted fractions, collects eluent, puts in 1mL measuring bottle, add methyl alcohol to scale, shake up, as need testing solution;
2) draw need testing solution, injection liquid chromatography, obtain chromatic graph spectrum, according to the chromatogram of many batches of obtained specification product, return 11 XINGNAOJING ZHUSHEYE standard control liquid-phase fingerprint with finger-print software, wherein absorption peak adds up to 11;
Wherein, the chromatographic condition of described liquid chromatography is as follows:
Chromatographic column: C
18(4.6mm × 250mm, 5 μm); Mobile phase: acetonitrile (A)-0.02% aqueous formic acid (B) gradient elution, elution requirement: 0-5min, 40%A; 5-50min, 40%-60%A; 50-60min, 60%-100%A; 60-65min, 100%A; 65.01-75min, 40%A; Flow velocity 1.0mL/min; Determined wavelength 254nm; Column temperature 35 DEG C; Sample size: 20 μ L.
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| CN107907611A (en) * | 2017-11-14 | 2018-04-13 | 大理药业股份有限公司 | A kind of cape jasmine quality evaluating method for XINGNAOJING ZHUSHEYE |
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| CN107688072B (en) * | 2016-08-05 | 2021-06-29 | 河南天地药业股份有限公司 | Detection method of Xingnaojing injection |
| CN107091893A (en) * | 2017-05-26 | 2017-08-25 | 浙江中医药大学 | The assay method of multi-target ingredient content in a kind of XINGNAOJING ZHUSHEYE or its intermediate |
| CN107091893B (en) * | 2017-05-26 | 2019-06-11 | 浙江中医药大学 | The measuring method of multi-target ingredient content in a kind of XINGNAOJING ZHUSHEYE or in which mesosome |
| CN107907611A (en) * | 2017-11-14 | 2018-04-13 | 大理药业股份有限公司 | A kind of cape jasmine quality evaluating method for XINGNAOJING ZHUSHEYE |
| CN108693140A (en) * | 2018-06-29 | 2018-10-23 | 无锡济民可信山禾药业股份有限公司 | A kind of method of muskone content in quick detection Xingnaojing oral preparation |
| CN109613152A (en) * | 2018-11-23 | 2019-04-12 | 无锡济民可信山禾药业股份有限公司 | The measuring method and its standard finger-print of XINGNAOJING ZHUSHEYE GCMS finger-print |
| WO2022222250A1 (en) * | 2021-04-24 | 2022-10-27 | 无锡济煜山禾药业股份有限公司 | Method for detecting macromolecular substance in xingnaojing injection |
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