CN105486762B - A kind of high-efficiency liquid-phase fingerprint detection method of female clever ball - Google Patents
A kind of high-efficiency liquid-phase fingerprint detection method of female clever ball Download PDFInfo
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- CN105486762B CN105486762B CN201410482791.6A CN201410482791A CN105486762B CN 105486762 B CN105486762 B CN 105486762B CN 201410482791 A CN201410482791 A CN 201410482791A CN 105486762 B CN105486762 B CN 105486762B
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Landscapes
- Investigating Or Analysing Biological Materials (AREA)
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Abstract
The present invention provides a kind of high-efficiency liquid-phase fingerprint detection method of female clever ball, the method includes：The foundation of female spirit ball standard finger-print, the measurement of female clever ball finger-print to be measured and similarity system design judgement and etc..The present invention is by attempting a variety of different elution requirements, the chromatographic condition of the fingerprint map analyzing of female clever ball is finally determined, investigate the reference fingerprint that 8 shared peaks are determined, have the characteristics that method is easy, speed is fast, favorable reproducibility, the standard finger-print established meets related request through methodology validation, strong applicability can more fully reflect product quality situation, and important evidence is provided for quality control and formulation standard.
Description
Technical field
The present invention relates to a kind of high-efficiency liquid-phase fingerprint detection methods of female clever ball, belong to Pharmaceutical Analysis technical field.
Background technology
Female spirit ball is a kind of compound Chinese medicinal preparation, and major function is menstruation regulating blood nourishing, is given birth to by the stasis of blood new.For irregular menstruation,
More or less, menalgia, cold uterus fail to be impregnated for a long time, and habitual abortion, leukorrhea with reddish discharge, uterine bleeding is more than, the long deficiency of vital energy of disease, kidney
Thanks to pain in the back.
The prescription of female spirit ball is as follows：
【Prescription】
(1) north rhizoma cyperi (system) 37g Radix Glycyrrhizaes 7g radix cynanchi atratis 14g motherworts 14g Radix Astragali 14g cockscombs 14g Radix Ophiopogonis 14g
Schisandra chinensis 14g glutinous rehmannia 14g safflowers 14g akebi 10g Rhizoma Atractylodis Macrocephalaes (stir-fry) 14g red halloysite 14g Poria cocos 14g Cortex Magnoliae Officinalis 10g meat deserts
Rong (system) 14g Radix Paeoniae Albas (parched with wine) 14g
(2) rhizoma cyperi (system) 37g schizonepeta 10g moutan barks 14g donkey-hide gelatin 14g Radix Angelicae Sinensis 14g Jehol Ligusticum Rhizome 10g red ginseng 14g deer
The angle rivers glue 14g bulbus fritillariae cirrhosae 14g myrrhs (stir-fry) 14g fructus amomis 14g corydalis tubers 14g fennel seeds (salt system) 14g colla carapacis et plastri testudinis 14g
Rhizome of chuanxiong 14g
【Preparation method】17 taste of the above prescription (one) adds water to cook secondary, 3 hours first times, second 2 hours, merges and decoct
Liquid, filtration, filtrate are placed 24 hours, are taken supernatant that rice vinegar 280g is added, are condensed into thick paste.(2) ten five tastes of the above prescription, powder
It is broken into middle powder, is added in above-mentioned thick paste, mixing, fine powder is dried, crushed into, is sieved, 1800 balls are made with the general ball of yellow rice wine in mixing,
Sugar coating or film-coating, polishing, it is dry to get.
Due to chemical composition of Chinese materia medica complexity, mechanism of action is indefinite, and existing Chinese medicine pharmaceutical technology is caused to be difficult to ensure Chinese medicine
Product quality stability, the type and quantity that can reflect Chinese medicine intrinsic chemical ingredient comprehensively that traditional Chinese medicine fingerprint is established, into
And reflect the quality of Chinese medicine.The middle the effective elements of the medicine overwhelming majority is not clear at this stage, by the way of traditional Chinese medicine fingerprint,
Traditional Chinese medicine quality will effectively be characterized.Finger-print is approved by international community, is conducive to Chinese medicine and product enters international market.
Female spirit ball current standard is recorded in Drug Standard of Ministry of Public Health of the Peoples Republic of China《Traditional Chinese medicine historical preparation》Tenth,
Any qualitative, quantitative item controlled for flavour of a drug is not directed in standard, currently, not carrying out finger-print research to female clever ball
Report, and finger-print can fully characterize the globality and complexity of Chinese medicine preparation, therefore inventor is to the effective of female clever ball
Ingredient is studied.It was found that wherein contain there are many water-soluble and Alcohol soluble composition, the present inventor targetedly to these at
Divide and studied, establish a kind of standard finger-print of female clever ball, matter is carried out to the female clever ball in production using the collection of illustrative plates
Amount supervision, to ensure product quality.
Invention content：
The present invention provides a kind of female clever ball efficient liquid phase standard control finger-print, and method for building up is as follows：
1) prepared by test solution：
Female clever ball is taken, methanol or ethanol water, ultrasonic dissolution is added, adds solvent adjustment solution concentration, micropore filter
Membrane filtration mistake takes filtrate, both；
2) chromatogram is obtained：
Test solution injects high performance liquid chromatograph, obtains chromatogram；
3) reference fingerprint is generated
More batches of qualified female clever ball chromatograms of selection import " the chromatographic fingerprints of Chinese materia medica similarity evaluation of Chinese Pharmacopoeia committee
System A editions " software, calculates to obtain similarity result, and generate standard control finger-print；
The chromatographic condition of wherein high performance liquid chromatography is as follows：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler, (4.6*250mm, 5um)；Mobile phase is second
The aqueous formic acid gradient elution of nitrile -0.1%~5%, is shown in Table 1；Flow velocity is 0.6~1.5ml/min；Column temperature is 25~40 DEG C；Into
Sample amount is 5~20 μ L；Detection wavelength is 274nm.
Gradient elution table：
It is preferred to elute table：
The standard reference material of active ingredient can be added as needed using as object of reference peak.
Wherein, the method for building up of preferred standard control finger-print is as follows：
1) preparation of test solution, method are as follows：
It takes female clever ball appropriate (dragee removing sugar-coat), is ground into fine powder, precision weighs 0.3~0.7g to 5~15ml capacity
In bottle, add 30%~70% methanol appropriate, be ultrasonically treated 20~40min, be cooled to room temperature, be settled to scale, shake up, crosses 0.45
μm miillpore filter, takes subsequent filtrate to obtain the final product.It is preferred that taking female clever ball appropriate, dragee removes sugar-coat, is ground into fine powder, precision weighs
In 0.5g to 10ml volumetric flasks, add 50% methanol appropriate, is ultrasonically treated 30min, is cooled to room temperature, is settled to scale, shake up, mistake
0.45 μm of miillpore filter, takes subsequent filtrate to obtain the final product.
2) standard reference material solution is prepared using Paeonol as object of reference, method is as follows：
Precision weighs that Paeonol reference substance is appropriate, adds the dissolving of 30%~70% methanol that every 1ml is made molten containing 8~20 μ g
Liquid to get；It is preferred that plus 50% methanol be made every 1ml contain 15 μ g solution.
3) determination of standard control finger-print, method are as follows：
Test solution and reference substance solution are injected into high performance liquid chromatograph, obtain chromatogram,
It is shared peak by 8 peaks in the finger-print of more batches of female clever ball samples, utilizes chromatographic fingerprints of Chinese materia medica similarity
Evaluation system (2.0 editions), fitting determine female clever ball reference fingerprint, wherein identical as Paeonol reference substance peak retention time
Chromatographic peak be No. 6 peaks, the relative retention time of other 7 chromatographic peaks is respectively：0.08(1)、0.13(2)、0.14(3)、
0.57 (4), 0.79 (5), 1.00 (6), 1.08 (7), 1.13 (8), the relative retention time at each peak is within ± 3%~± 10%
The present invention also provides a kind of efficient liquid-phase chromatograph finger print atlas detection methods of female clever ball, which is characterized in that including
Following steps
1) preparation of testing sample solution：
Female clever ball sample is taken, methanol or ethanol water, ultrasonic dissolution is added, adds solvent adjustment solution concentration, it is micro-
Hole filter membrane filtration；
2) measurement of testing sample solution finger-print：
Filtrate is taken, high performance liquid chromatograph is injected, obtains chromatogram：
Chromatographic condition therein is as follows：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler (4.6*250mm, 5um)；Mobile phase is acetonitrile-
0.1%~5% aqueous formic acid gradient elution, is shown in Table 1；Flow velocity is 0.6~1.5ml/min；Column temperature is 25~40 DEG C；Sample size
For 5-20 μ L；Detection wavelength is 272-276nm.
It is preferred that using -1% formic acid of acetonitrile as mobile phase；Flow velocity 1.0ml/ minutes；30 DEG C of column temperature；Sample size is 10 μ L；Detection
Wavelength：274nm.
1 gradient elution table of table
It is preferred to elute table：
3) sample to be tested chromatogram and standard control fingerprint similarity calculate：
The chromatogram of sample to be tested is imported " similarity evaluation A editions " of Chinese Pharmacopoeia committee
Software compares the chromatogram and standard control fingerprint similarity of sample to be tested；
Wherein, the testing sample solution of the preferred present invention prepare it is as follows：
It takes female clever ball appropriate (dragee removing sugar-coat), is ground into fine powder, precision weighs 0.3~0.7g to 5~15ml capacity
In bottle, add 30%~70% methanol appropriate, be ultrasonically treated 20~40min, be cooled to room temperature, be settled to scale, shake up, crosses 0.45
μm miillpore filter takes subsequent filtrate, injects high performance liquid chromatograph, obtains chromatogram；
It is preferred that：Take female clever ball appropriate, dragee removes sugar-coat, is ground into fine powder, precision weighs 0.5g to 10ml volumetric flasks
In, add 50% methanol appropriate, be ultrasonically treated 30min, be cooled to room temperature, be settled to scale, shake up, crosses 0.45 μm of miillpore filter,
Subsequent filtrate is taken both to obtain.
Wherein, sample to be tested chromatogram and standard control fingerprint similarity calculate：
The chromatogram of sample to be tested is imported " similarity evaluation A editions " of Chinese Pharmacopoeia committee
Software compares the chromatogram and standard control fingerprint similarity of sample to be tested；It is qualification that similarity, which is 0.90 or more, similar
It is to be consistent that degree, which is 0.95 or more, and it is identical that similarity, which is 0.98 or more,.
The present invention further establishes the analysis method of female clever ball, using the party by the foundation of the above finger-print
Method can be obtained discriminating conclusion, more be connect with standard finger-print with the female clever ball of accurate discrimination according to the comparison with standard finger-print
Closely, product quality is better, and similarity can be confirmed using computer approach, is qualified, similarity if similarity is 0.90 or more
For 0.95 or more to be consistent, it is identical that similarity, which is 0.98 or more,.
The preparation method that the above method is especially the standard control finger-print of female clever ball is obtained by screening, below
For screening process：
1.1 instruments and reagent
Instrument：Waters2695-2996 high performance liquid chromatographs；Empower II chromatographic work stations；Milli-Q ultra-pure waters
Device；A ten thousandth balance (Sai Duolisi)；Ten a ten thousandth balances (Sai Duolisi).
Chromatographic column：Agilent ZORBAX(4.6*250mm,5μm)；
Reagent：Methanol (chromatographically pure, Tianjin Concord Technology Co., Ltd.)；Acetonitrile (chromatographically pure, Tianjin Concord section
Skill Co., Ltd)；Formic acid (analyzes pure, Tianjin Chemical Reagents Factory No.1)；Water is ultra-pure water.
Reference substance：Nat'l Pharmaceutical ＆ Biological Products Control Institute；Paeonol (lot number：110708-200506, assay are used,
It is provided for Nat'l Pharmaceutical ＆ Biological Products Control Institute；
Sample：(Tianjin Tasly (Liaoning) Pharmaceutical Co., Ltd., totally 11 batches, specific lot number is shown in Table 2 to female spirit ball,
It is qualified to be examined through Product Quality Verification Centers.
The female clever ball sample message table of table 2
The selection of 1.2 analysis conditions
1.2.1 the selection of Detection wavelength
With reference to content detection of paeonol chromatographic condition in product, chromatographic column is selected：Agilent ZORBAX SB-C18(4.6
× 250mm, 5 μm), eluted with condition of gradient elution in table 3, the selection for being detected wavelength is investigated.
3 gradient elution table of table
The Detection wavelength of document report is often the content for being a certain special component of measurement, not necessarily entirely appropriate fingerprint image
The needs of spectrum need to select several different Detection wavelengths, while female clever ball is big compound system to obtain multi-level information
Agent, contains 31 taste Chinese medicines, and there are many contained chemical composition.Therefore, in test the detection of DAD detector all-wave lengths should be used to obtain
3D finger-prints are obtained, see Fig. 1.The result shows that more chemical information can be obtained at 274nm, therefore select 274nm as detection
Wavelength is shown in Fig. 2.
1.2.2 the selection of Extraction solvent
It takes female clever ball appropriate, is ground into fine powder, precision weighs 0.5g, and respectively plus water, 30% methanol solution, 50% methanol are molten
Liquid, 70% methanol solution, methanol 25mL, be ultrasonically treated 30min, take supernatant cross 0.45 μm of filter membrane to get.
It is shown by Fig. 3, it is more complete and similar that 50% methanol and 70% methanol solution extraction sample obtain spectral peak information, from economy
And from the point of view of environmental pollution, the final Extraction solvent chosen 50% methanol and prepared as test solution.
1.2.3 the selection of extractant dosage
Take female clever ball appropriate, be ground into fine powder, precision weighs 0.5g, be separately added into 50% methanol 10ml, 15ml, 20ml,
25ml, be ultrasonically treated 30min, take supernatant cross 0.45 μm of filter membrane to get.Compare the extractant of different amounts to chromatographic peak number
And the influence of peak area, see Fig. 4.As seen from the figure, extractant dosage has no effect on the number of chromatographic peak, but removes retention time
Remaining outer chromatographic peak at the big peak of 42min or so is smaller, therefore considers that selective extraction agent dosage is 10ml.
1.2.4 the selection of flow phase system
When carrying out above-mentioned experiment investigation, using methanol-water flow visualizing, chromatographic column chromatographic column column after a period of use
Pressure increases obviously, and individual chromatographic peak peak shapes are obviously deteriorated in chromatogram, therefore has investigated acetonitrile-water flow visualizing, acetonitrile-
0.1% formic acid water flow visualizing, -0.1% phosphoric acid flow visualizing of acetonitrile.During experiment, using linear gradient elution point
From the active ingredient in female clever ball.The result shows that when mobile phase is -0.1% phosphoric acid of acetonitrile, acetonitrile-water, it cannot be by 31 minutes
The chromatographic peak at place separates, therefore final choice flow visualizing is：- 0.1% aqueous formic acid of acetonitrile.
1.2.4 the selection of eluent gradient elution program
Selection compares influence of about 20 kinds of different gradients to female clever ball finger-print chromatographic peak, finally determines gradient
Elution requirement is as shown in table 1：
The determination of 1.3 analysis methods
It to sum up analyzes, finally determines that female clever ball fingerprint analysis method is as follows：
Take female clever ball appropriate, dragee removes sugar-coat, is ground into fine powder, precision weighs in 0.5g to 10ml volumetric flasks, adds
50% methanol is appropriate, is ultrasonically treated 30min, is cooled to room temperature, is settled to scale, shake up, and crosses 0.45 μm of miillpore filter, takes continuous filter
Liquid to obtain the final product.Using octadecyl silane as filler；Using -1% formic acid of acetonitrile as mobile phase, gradient elution is shown in Table 2-3；Stream
It is 1.0ml/ minutes fast；30 DEG C of column temperature；Detection wavelength：274nm.
1.4 chemical composition qualitative research and the selection with reference to peak
For ingredient in further clearly female clever ball, being fixed tentatively using reference substance retention time method of comparison may in female clever ball
The chemical composition contained.By consulting literatures, in female spirit ball the ingredient that may contain be Paeonol, α-cyperolone, echinacoside,
Honokiol, tetrahydropalmatine, magnolol, Kaempferol, Catalpol, ammonium glycyrrhetate, L-PROLINE, Astragaloside IV, ginsenoside Rf,
Ginsenoside Re, ginsenoside Rg1, hydrochloric acid leonurine etc..It is found by the retention time between contrast sample and reference substance,
Under the chromatographic condition, the chemical composition that can position in the sample has Paeonol, an echinacoside, and Paeonol contains in chromatogram
Highest is measured, and is the index components of assay item in product, therefore selects Paeonol for reference to peak.Refer to Fig. 6.
The methodology validation of 1.5 finger-prints experiment
1.5.1 Precision Experiment
Take female clever ball sample (film-coating lot number：20121002；Sugar-coat lot number：20120903) 0.5g, it is accurately weighed, it presses
Liquid phase fingerprint analysis method under " 1.3 " item, 6 needle of continuous sample introduction record each shared chromatographic peak retention time and peak area.With reference
The retention time and peak area of object Paeonol are reference, calculate the relative retention time and relative peak area ratio at each shared peak
Value.
It the results are shown in Table 4,5.
As a result it shows：8 shared peak area ratio relative standard deviations are in 0.00%~2.76% range, retention time
Ratio relative standard deviation is in 0.00%~0.25% range.Meet the requirement of fingerprint pattern technology standard, as a result the side of display
The precision of method is preferable.
1.5.2 repeated experiment
Take female clever ball sample (film-coating lot number：20121002；Sugar-coat lot number：20120901) 0.5g, each six parts, precision claims
It is fixed, it is measured by liquid phase fingerprint assay method under " 1.3 " item, records each shared chromatographic peak retention time and peak area.With object of reference
The retention time and peak area of Paeonol are reference, calculate the relative retention time and relative peak area ratio at each shared peak.
It the results are shown in Table 6,7.
As a result it shows：8 shared peak area ratio relative standard deviations are in 0.00%~2.39% range, retention time
Ratio relative standard deviation is in 0.00%~0.40% range.Meet the requirement of fingerprint pattern technology standard, the weight of this method
Renaturation is preferable.
1.5.3 stability experiment
Take female clever ball sample (film-coating lot number：20121002；Sugar-coat lot number：20120903) 0.5g, it is accurately weighed, it presses
Liquid phase fingerprint assay method under " 1.3 " item was measured respectively at 0,1,2,4,6,8,16,24 hour once, with object of reference Paeonol
Retention time and peak area be reference, calculate the relative retention time at each shared peak and relative peak area ratio.As a result see
Table 8,9.
As a result it shows：8 shared peak area ratio relative standard deviations are in 0.00%~5.51% range, retention time
Ratio relative standard deviation is in 0.00%~0.55% range.Meet the requirement of fingerprint pattern technology standard, the weight of this method
Renaturation is preferable.
2.1 fingerprint spectrum methods are analyzed
2.1.1 finger-print shares the determination at peak
Female clever 7 batches, ball film-coating ball, dragee 5 batches are chosen, is measured respectively by liquid phase fingerprint assay method under " 1.3 " item,
According to the relevant parameter given by 12 batches of female clever ball test sample HPLC collection of illustrative plates, 8 chromatographic peaks are each batch shared, see Fig. 7, figure
8。
Separately the relative retention time at 8 shared peaks in 12 batches of samples and relative peak area are analyzed, with No. 6 peak root barks of tree peony
Phenol is to calculate the relative retention time and peak area ratio at other 7 shared peaks with reference to peak, then the shared peak of 11 batches of samples is average
Relative retention time (peak number) is followed successively by：0.08(1)、0.13(2)、0.14(3)、0.57(4)、0.79(5)、1.00(6)、1.08
(7), 1.13 (8), relative deviation is within ± 10%.It is shown in Table 10,11.
10 11 batches of samples of table share peak relative retention time
11 11 batches of samples of table share peak relative peak area
2.1.2 the fitting of reference fingerprint
It is shared peak with 8 peaks in the finger-print of above-mentioned 12 batches of samples, is commented using chromatographic fingerprints of Chinese materia medica similarity
Valence system (2.0 editions), fitting determine female clever ball reference fingerprint, see Fig. 9.
2.1.3 the standard of finger-print limits
Because the product lot number of current Liaoning day scholar's power production is less, the follow-up of quality of a large amount of samples, data product are subsequently also needed
Tired, the fingerprint similarity of tentatively tentative female clever ball is qualified 0.90 or more.
The beneficial effects of the present invention are：
The present invention finally determines the chromatostrip of the fingerprint map analyzing of female clever ball by attempting a variety of different elution requirements
Part investigates the reference fingerprint that 8 shared peaks are determined, method is easy, quick, reproducible, meets through methodology validation
Related request.
A kind of fingerprint analysis method strong applicability for female clever ball that the present invention establishes, can more comprehensively reflect product
Quality condition.
Description of the drawings
The female clever ball 200-400nm full wavelength scanner chromatograms of Fig. 1
Fig. 2 274nm wavelength graph spectrograms
Fig. 3 different solvents compare chromatogram
Fig. 4 different solvents compare chromatogram
Fig. 5 difference flow visualizings compare chromatogram
The qualitative relatively chromatography of Fig. 6 chemical compositions
The liquid phase overlay chart of the female clever ball samples of Fig. 7 11 crowdes
The shared peak match figure of the female clever ball samples of Fig. 8 11 crowdes
The reference fingerprint that Fig. 9 is fitted by 12 batches of female clever ball samples
Specific implementation mode：
It further illustrates the present invention by the following examples, but not as limitation of the present invention.
Embodiment 1, the determining fingerprint pattern of female spirit ball
Take the female clever ball film-coating ball that lot number is 20121102
Step 1, the preparation of test solution
It takes female clever film-coating ball appropriate, is ground into fine powder, precision weighs in 0.5g to 10ml volumetric flasks, adds 50% methanol suitable
Amount is ultrasonically treated 30min, is cooled to room temperature, is settled to scale, shake up, and crosses 0.45 μm of miillpore filter, takes subsequent filtrate to obtain the final product.Step
Rapid 2, the foundation of finger-print
Using high performance liquid chromatography, chromatographic condition is：Chromatographic column fixed phase is to fill out with octadecylsilane chemically bonded silica
Material, Agilent ZORBAX (4.6*250mm, 5um)；Mobile phase is -1% aqueous formic acid gradient elution of acetonitrile；Flow velocity is
1.0ml/min；Column temperature is 30 DEG C；Sample size is 10 μ L,；Detection wavelength is 274nm.Test solution is analyzed with this condition,
Obtain the finger-print of female clever ball to be measured.
Gradient elution table
According to the method provided by the invention, the HPLC reference fingerprints established with female clever ball are control, using Chinese medicine color
Compose (2.0 editions) calculating of fingerprint similarity evaluation system, similarity 0.989.
Embodiment 2, the determining fingerprint pattern of female spirit ball
Take the female clever ball film-coating ball that lot number is 20121002
Step 1, the preparation of test solution
It takes female clever film-coating ball appropriate, is ground into fine powder, precision weighs in 0.4g to 10ml volumetric flasks, adds 40% methanol suitable
Amount is ultrasonically treated 25min, is cooled to room temperature, is settled to scale, shake up, and crosses 0.45 μm of miillpore filter, takes subsequent filtrate to obtain the final product.Refer to
The determination of line collection of illustrative plates,
Step 2, the foundation of finger-print
Using high performance liquid chromatography, chromatographic condition is：Chromatographic column fixed phase is to fill out with octadecylsilane chemically bonded silica
Material, Agilent ZORBAX (4.6*250mm, 5um)；Mobile phase is -1% aqueous formic acid gradient elution of acetonitrile；Flow velocity is
1.0ml/min；Column temperature is 35 DEG C；Sample size is 10 μ L,；Detection wavelength is 274nm.Test solution is analyzed with this condition,
Obtain the finger-print of female clever ball to be measured.
Gradient elution table
According to the method provided by the invention, the HPLC reference fingerprints established with female clever ball are control, using Chinese medicine color
Compose (2.0 editions) calculating of fingerprint similarity evaluation system, similarity 0.984.
Embodiment 3, the determining fingerprint pattern of female spirit ball
Take the female clever ball dragee that lot number is 20120901
Step 1, the preparation of test solution
It takes female clever ball dragee appropriate, removes sugar-coat (directly beaing method), be ground into fine powder, precision weighs 0.6g to 10ml appearances
In measuring bottle, add 60% methanol appropriate, be ultrasonically treated 35min, be cooled to room temperature, be settled to scale, shake up, crosses 0.45 μm of micropore filter
Film takes subsequent filtrate to obtain the final product.
Step 2, the foundation of finger-print
Using high performance liquid chromatography, chromatographic condition is：Chromatographic column fixed phase is to fill out with octadecylsilane chemically bonded silica
Material, Agilent ZORBAX (4.6*250mm, 5 μm)；Mobile phase is -1% aqueous formic acid gradient elution of acetonitrile；Flow velocity is
1.0ml/min；Column temperature is 30 DEG C；Sample size is 10 μ L；Detection wavelength is 274nm.Test solution is analyzed with this condition, is obtained
To the finger-print of female clever ball to be measured.
Gradient elution table
According to the method provided by the invention, the HPLC reference fingerprints established with female clever ball are control, using Chinese medicine color
Compose (2.0 editions) calculating of fingerprint similarity evaluation system, similarity 0.998.
Embodiment 4, the determining fingerprint pattern of female spirit ball
1) preparation of testing sample solution：
It takes female clever ball appropriate, is ground into fine powder, precision weighs in 0.3g to 5ml volumetric flasks, adds 30% methanol appropriate, at ultrasound
20min is managed, is cooled to room temperature, is settled to scale, shake up, crosses 0.4 μm of miillpore filter；
2) measurement of sample to be tested finger-print：
Filtrate is taken, high performance liquid chromatograph is injected, obtains chromatogram, chromatographic condition is：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler, Agilent ZORBAX；Mobile phase is acetonitrile-
Aqueous formic acid gradient elution, aqueous formic acid a concentration of 0.1%, flow velocity 0.6ml/min, column temperature be 25 DEG C, sample size
For 5 μ L；Detection wavelength is 272nm；
Gradient elution mode is：
3) sample to be tested chromatogram and standard control fingerprint similarity calculate：
The chromatogram of sample to be tested is imported " similarity evaluation A editions " of Chinese Pharmacopoeia committee
Software compares the chromatogram and standard control fingerprint similarity of sample to be tested.
Embodiment 5, the determining fingerprint pattern of female spirit ball
1) preparation of testing sample solution：
It takes female clever ball appropriate, is ground into fine powder, precision weighs in 0.7g to 15ml volumetric flasks, adds 70% methanol appropriate, ultrasound
40min is handled, is cooled to room temperature, is settled to scale, shake up, crosses 0.5 μm of miillpore filter；
2) measurement of sample to be tested finger-print：
Filtrate is taken, high performance liquid chromatograph is injected, obtains chromatogram, chromatographic condition is：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler, Agilent ZORBAX；Mobile phase is acetonitrile-
Aqueous formic acid gradient elution, aqueous formic acid a concentration of 5%, flow velocity 1.5ml/min, column temperature be 40 DEG C, sample size is
20μL；Detection wavelength is 276nm；
Gradient elution mode is：
3) sample to be tested chromatogram and standard control fingerprint similarity calculate：
The chromatogram of sample to be tested is imported " similarity evaluation A editions " of Chinese Pharmacopoeia committee
Software compares the chromatogram and standard control fingerprint similarity of sample to be tested.
Embodiment 6, the determining fingerprint pattern of female spirit ball
1) preparation of testing sample solution：
It takes female clever ball appropriate, is ground into fine powder, take female clever ball appropriate, dragee removes sugar-coat, is ground into fine powder, precision weighs
In 0.5g to 10ml volumetric flasks, add 50% methanol appropriate, is ultrasonically treated 30min, is cooled to room temperature, is settled to scale, shake up, mistake
0.45 μm of miillpore filter；
2) measurement of sample to be tested finger-print：
Filtrate is taken, high performance liquid chromatograph is injected, obtains chromatogram, chromatographic condition is：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler, Agilent ZORBAX；With -1% first of acetonitrile
Acid is mobile phase, flow velocity 1.0ml/ minutes, 30 DEG C of column temperature, Detection wavelength：274nm, sample size are 10 μ L；
Gradient elution mode is：
3) sample to be tested chromatogram and standard control fingerprint similarity calculate：
The chromatogram of sample to be tested is imported " similarity evaluation A editions " of Chinese Pharmacopoeia committee
Software compares the chromatogram and standard control fingerprint similarity of sample to be tested.
Embodiment 7, the determining fingerprint pattern of female spirit ball
1) preparation of testing sample solution：
It takes female clever ball appropriate, is ground into fine powder, take female clever ball appropriate, dragee removes sugar-coat, is ground into fine powder, precision weighs
In 0.5g to 10ml volumetric flasks, add 50% methanol appropriate, is ultrasonically treated 30min, is cooled to room temperature, is settled to scale, shake up, mistake
0.45 μm of miillpore filter；
2) measurement of sample to be tested finger-print：
Filtrate is taken, high performance liquid chromatograph is injected, obtains chromatogram, chromatographic condition is：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler, Agilent ZORBAX；With -1% first of acetonitrile
Acid is mobile phase, flow velocity 1.0ml/ minutes, 30 DEG C of column temperature, Detection wavelength：274nm, sample size are 10 μ L；
Gradient elution mode is：
3) sample to be tested chromatogram and standard control fingerprint similarity calculate：
The chromatogram of sample to be tested is imported " similarity evaluation A editions " of Chinese Pharmacopoeia committee
Software compares the chromatogram and standard control fingerprint similarity of sample to be tested.
Embodiment 8, a kind of female clever ball efficient liquid phase standard control finger-print, method for building up are as follows：
1) prepared by test solution：
Take female clever ball appropriate, dragee removes sugar-coat, is ground into fine powder, precision weighs in 0.5g to 10ml volumetric flasks, adds
50% methanol is appropriate, is ultrasonically treated 30min, is cooled to room temperature, is settled to scale, shake up, and crosses 0.45 μm of miillpore filter, takes continuous filter
Liquid to obtain the final product；
The preparation method of reference substance solution is：Paeonol is taken, adds 50% methanol that the solution that every 1ml contains 15 μ g is made；
2) chromatogram is obtained：
Test solution and reference substance solution inject high performance liquid chromatograph, obtain chromatogram, wherein high performance liquid chromatography
Chromatographic condition it is as follows：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler, Agilent ZORBAX, with -1% first of acetonitrile
Acid is mobile phase, flow velocity 1.0ml/ minutes, 30 DEG C of column temperature, Detection wavelength：274nm, sample size 15ul；
Gradient elution table：
3) reference fingerprint is generated
More batches of qualified female clever ball chromatograms of selection import similarity evaluation system, calculate to obtain similarity result, and generate
Standard control finger-print；Be shared peak by 8 peaks in the finger-print of more batches of female clever ball samples, with Paeonol reference substance peak
The identical chromatographic peak of retention time is with reference to peak, and the relative retention time of other 7 chromatographic peaks is respectively：0.08、0.13、
0.14,0.57,0.79,1.00,1.08,1.13, the relative retention time at each peak is within ± 3%~± 10%.
Embodiment 9, a kind of female clever ball efficient liquid phase standard control finger-print, method for building up are as follows：
1) prepared by test solution：
It takes female clever ball appropriate, is ground into fine powder, precision weighs in 0.3g to 5ml volumetric flasks, adds 30% methanol appropriate, at ultrasound
It manages 20min, is cooled to room temperature, is settled to scale, shake up, cross 0.45 μm of miillpore filter, take subsequent filtrate to obtain the final product；
Paeonol standard reference material solution, preparation method are：It is appropriate that precision weighs Paeonol reference substance, adds 30% methanol molten
Solution be made every 1ml containing 8 μ g solution to get；
2) chromatogram is obtained：
Test solution injects high performance liquid chromatograph, obtains chromatogram, the wherein chromatographic condition of high performance liquid chromatography such as
Under：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler, Agilent ZORBAX；Mobile phase is acetonitrile-
Aqueous formic acid gradient elution, a concentration of the 0.1% of aqueous formic acid；Flow velocity is 0.6ml/min；Column temperature is 25 DEG C；Sample size
For 5 μ L；Detection wavelength is 272nm,
Gradient elution table：
3) reference fingerprint is generated
More batches of qualified female clever ball chromatograms of selection import similarity evaluation system, calculate to obtain similarity result, and generate
Standard control finger-print；Be shared peak by 8 peaks in the finger-print of more batches of female clever ball samples, with Paeonol reference substance peak
The identical chromatographic peak of retention time is with reference to peak, and the relative retention time of other 7 chromatographic peaks is respectively：0.08、0.13、
0.14,0.57,0.79,1.00,1.08,1.13, the relative retention time at each peak is within ± 3%~± 10%.
Embodiment 10, a kind of female clever ball efficient liquid phase standard control finger-print, method for building up are as follows：
1) prepared by test solution：
It takes female clever ball appropriate, is ground into fine powder, precision weighs in 0.7g to 15ml volumetric flasks, adds 70% methanol appropriate, ultrasound
It handles 40min, is cooled to room temperature, is settled to scale, shake up, cross 0.45 μm of miillpore filter, take subsequent filtrate to obtain the final product；
Paeonol standard reference material solution, preparation method are：It is appropriate that precision weighs Paeonol reference substance, adds 70% methanol molten
Solution be made every 1ml containing 20 μ g solution to get；
2) chromatogram is obtained：
Test solution injects high performance liquid chromatograph, obtains chromatogram, the wherein chromatographic condition of high performance liquid chromatography such as
Under：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler, Agilent ZORBAX；Mobile phase is acetonitrile-
Aqueous formic acid gradient elution, a concentration of the 5% of aqueous formic acid；Flow velocity is 1.5ml/min；Column temperature is 40 DEG C；Sample size is
20μL；Detection wavelength is 276nm,
Gradient elution table：
3) reference fingerprint is generated
More batches of qualified female clever ball chromatograms of selection import similarity evaluation system, calculate to obtain similarity result, and generate
Standard control finger-print；Be shared peak by 8 peaks in the finger-print of more batches of female clever ball samples, with Paeonol reference substance peak
The identical chromatographic peak of retention time is with reference to peak, and the relative retention time of other 7 chromatographic peaks is respectively：0.08、0.13、
0.14,0.57,0.79,1.00,1.08,1.13, the relative retention time at each peak is within ± 3%~± 10%.
Embodiment 11, a kind of female clever ball efficient liquid phase standard control finger-print, method for building up are as follows：
1) prepared by test solution：
It takes female clever ball appropriate, is ground into fine powder, precision weighs in 0.3g to 5ml volumetric flasks, adds 30% methanol appropriate, at ultrasound
It manages 20min, is cooled to room temperature, is settled to scale, shake up, cross 0.45 μm of miillpore filter, take subsequent filtrate to obtain the final product；
Paeonol standard reference material solution, preparation method are：It is appropriate that precision weighs Paeonol reference substance, adds 30% methanol molten
Solution be made every 1ml containing 8 μ g solution to get；
2) chromatogram is obtained：
Test solution injects high performance liquid chromatograph, obtains chromatogram, the wherein chromatographic condition of high performance liquid chromatography such as
Under：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler, Agilent ZORBAX；Mobile phase is acetonitrile-
Aqueous formic acid gradient elution, a concentration of the 0.1% of aqueous formic acid；Flow velocity is 0.6ml/min；Column temperature is 25 DEG C；Sample size
For 5 μ L；Detection wavelength is 272nm,
Gradient elution table：
3) reference fingerprint is generated
More batches of qualified female clever ball chromatograms of selection import similarity evaluation system, calculate to obtain similarity result, and generate
Standard control finger-print；Be shared peak by 8 peaks in the finger-print of more batches of female clever ball samples, with Paeonol reference substance peak
The identical chromatographic peak of retention time is with reference to peak, and the relative retention time of other 7 chromatographic peaks is respectively：0.08、0.13、
0.14,0.57,0.79,1.00,1.08,1.13, the relative retention time at each peak is within ± 3%~± 10%.
Embodiment 12, a kind of female clever ball efficient liquid phase standard control finger-print, method for building up are as follows：
1) prepared by test solution：
It takes female clever ball appropriate, is ground into fine powder, precision weighs in 0.7g to 15ml volumetric flasks, adds 70% methanol appropriate, ultrasound
It handles 40min, is cooled to room temperature, is settled to scale, shake up, cross 0.45 μm of miillpore filter, take subsequent filtrate to obtain the final product；
Paeonol standard reference material solution, preparation method are：It is appropriate that precision weighs Paeonol reference substance, adds 70% methanol molten
Solution be made every 1ml containing 20 μ g solution to get；
2) chromatogram is obtained：
Test solution injects high performance liquid chromatograph, obtains chromatogram, the wherein chromatographic condition of high performance liquid chromatography such as
Under：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler, Agilent ZORBAX；Mobile phase is acetonitrile-
Aqueous formic acid gradient elution, a concentration of the 5% of aqueous formic acid；Flow velocity is 1.5ml/min；Column temperature is 40 DEG C；Sample size is
20μL；Detection wavelength is 276nm,
Gradient elution table：
3) reference fingerprint is generated
More batches of qualified female clever ball chromatograms of selection import similarity evaluation system, calculate to obtain similarity result, and generate
Standard control finger-print；Be shared peak by 8 peaks in the finger-print of more batches of female clever ball samples, with Paeonol reference substance peak
The identical chromatographic peak of retention time is with reference to peak, and the relative retention time of other 7 chromatographic peaks is respectively：0.08、0.13、
0.14,0.57,0.79,1.00,1.08,1.13, the relative retention time at each peak is within ± 3%~± 10%.
Claims (7)
1. a kind of efficient liquid-phase chromatograph finger print atlas detection method of female clever ball, which is characterized in that include the following steps：
1) preparation of testing sample solution：
Female clever ball sample is taken, methanol aqueous solution is added, ultrasonic dissolution adds solvent adjustment solution concentration, miillpore filter filtration；
2) measurement of sample to be tested finger-print：
Filtrate is taken, high performance liquid chromatograph is injected, obtains chromatogram, chromatographic condition is：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler；Flow velocity is 0.6~1.5ml/min, column temperature be 25~
40 DEG C, sample size be 5~20 μ L；Detection wavelength is 272-276nm；
Gradient elution mode is：
Or
Or
Or
Or
3) sample to be tested chromatogram and standard control fingerprint similarity calculate：
The chromatogram of sample to be tested is imported to A editions softwares of similarity evaluation of Chinese Pharmacopoeia committee,
Compare the chromatogram and standard control fingerprint similarity of sample to be tested.
2. fingerprint atlas detection method according to claim 1, which is characterized in that the preparation method of step 1) testing sample solution
For：
It takes female clever ball appropriate, is ground into fine powder, precision weighs in 0.3~0.7g to 5~15ml volumetric flasks, adds 30%~70% methanol
In right amount, it is ultrasonically treated 20~40min, is cooled to room temperature, is settled to scale, shake up, crosses 0.4-0.5 μm of miillpore filter.
3. fingerprint atlas detection method according to claim 2, which is characterized in that the wherein preparation of step 1) testing sample solution
Mode is：Take female clever ball appropriate, dragee removes sugar-coat, is ground into fine powder, precision weighs in 0.5g to 10ml volumetric flasks, adds 50%
Appropriate methanol is ultrasonically treated 30min, is cooled to room temperature, is settled to scale, shake up, and crosses 0.45 μm of miillpore filter.
4. fingerprint atlas detection method according to claim 1, which is characterized in that the chromatographic condition of wherein step 2) is：Flow velocity
1.0ml/ minutes, 30 DEG C of column temperature, Detection wavelength：274nm, sample size are 10 μ L.
5. fingerprint atlas detection method according to claim 1, which is characterized in that wherein gradient elution mode is：
6. fingerprint atlas detection method according to claim 1, which is characterized in that standard control finger-print described in step 3)
Method for building up includes the following steps：
(1) prepared by test solution：
Female clever ball is taken, methanol aqueous solution is added, ultrasonic dissolution adds solvent adjustment solution concentration, and miillpore filter filtration takes filter
Liquid to get；
(2) chromatogram is obtained：
Test solution injects high performance liquid chromatograph, obtains chromatogram；
(3) reference fingerprint is generated
More batches of qualified female clever ball chromatograms of selection import similarity evaluation system, calculate to obtain similarity result, and generate standard
Reference fingerprint；
Chromatographic condition is：
Chromatographic column fixed phase is using octadecylsilane chemically bonded silica as filler；Flow velocity is 0.6~1.5ml/min, column temperature be 25~
40 DEG C, sample size be 5~20 μ L；Detection wavelength is 272-276nm；
Gradient elution mode is：
Or
Or
Or
Or
The standard reference material of active ingredient can be added as needed using as object of reference peak.
7. fingerprint atlas detection method according to claim 6, which is characterized in that standard control finger-print described in step 3)
Method for building up includes the following steps：
(1) preparation of test solution, method are as follows：
It takes female clever ball appropriate, is ground into fine powder, precision weighs in 0.3~0.7g to 5~15ml volumetric flasks, adds 30%~70% methanol
In right amount, it is ultrasonically treated 20~40min, is cooled to room temperature, is settled to scale, shake up, 0.45 μm of miillpore filter is crossed, takes subsequent filtrate i.e.
,
(2) chromatogram is obtained：
Test solution injects high performance liquid chromatograph, obtains chromatogram, while using Paeonol as object of reference；
Paeonol standard reference material solution, preparation method are：It is appropriate that precision weighs Paeonol reference substance, adds 30%~70% methanol
Dissolving be made every 1ml containing 8~20 μ g solution to get；
(3) reference fingerprint is generated, method is as follows：
It is shared peak by 8 peaks in the finger-print of more batches of female clever ball samples, with identical as Paeonol reference substance peak retention time
Chromatographic peak be with reference to peak, the relative retention time of other 7 chromatographic peaks is respectively：0.08、0.13、0.14、0.57、0.79、
1.00,1.08,1.13, the relative retention time at each peak is within ± 3%~± 10%.
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| CN112444588A (en) * | 2019-08-27 | 2021-03-05 | 中国科学院大连化学物理研究所 | Fingerprint spectrum detection method for quality of Xiaojin capsules, Xiaojin pills or Xiaojin tablets |
| CN112697949B (en) * | 2020-12-09 | 2022-05-27 | 浙江金城阜通制药有限公司 | Thin-layer identification method for Baoyuan decoction, similar formula extract and preparation thereof |
| CN114636779B (en) * | 2022-03-29 | 2024-05-24 | 陕西盘龙药业集团股份有限公司 | Construction method of three-conversion soup reference sample freeze-dried powder fingerprint and fingerprint thereof |
| CN117233306B (en) * | 2023-11-16 | 2024-01-30 | 江西省药品检验检测研究院 | Fingerprint establishment and component content determination method for jindan Fuyan particles |
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| CN1785391A (en) * | 2005-12-07 | 2006-06-14 | 宛六一 | Chinese medicinal composition and its preparation method |
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| CN104069463A (en) * | 2014-07-10 | 2014-10-01 | 仵爱涛 | Traditional Chinese medicinal medicament for treating gynaecological metrorrhagia and metrostaxis |
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| US10359407B2 (en) * | 2016-02-22 | 2019-07-23 | Hong Kong Baptist University | Quality control marker and its use in cordyceps species authentication |
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| CN1785391A (en) * | 2005-12-07 | 2006-06-14 | 宛六一 | Chinese medicinal composition and its preparation method |
| CN101073587A (en) * | 2006-05-18 | 2007-11-21 | 天津天士力制药股份有限公司 | Method for separating and extracting Chinese Thorowax Root |
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