CN102680628A - Method for establishing fingerprint of An Weiyang - Google Patents
Method for establishing fingerprint of An Weiyang Download PDFInfo
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- CN102680628A CN102680628A CN2012101569449A CN201210156944A CN102680628A CN 102680628 A CN102680628 A CN 102680628A CN 2012101569449 A CN2012101569449 A CN 2012101569449A CN 201210156944 A CN201210156944 A CN 201210156944A CN 102680628 A CN102680628 A CN 102680628A
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- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims abstract description 47
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 claims abstract description 27
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Abstract
The invention provides a method for establishing a fingerprint of a liquorice extract, preferably An Weiyang. The method is characterized by adopting high performance liquid chromatography (HPLC) to detect the content of flavonoids in the liquorice extract, wherein the conditions of HPLC are as follows: the chromatographic column takes octadecylsilane chemically bonded silica as a packing phase; mobile phases are acetonitrile and 0.01-0.1% of trifluoroacetic acid in a volume ratio of (22:78)-(75:25) and are subjected to gradient elution; the flow rate is 0.5-1.5mL/min; the column temperature is 25-40 DEG C; and the ultraviolet detection wavelength is 270nm. The method provided by the invention is simple, convenient, stable, high in precision and good in repeatability, can effectively represent the quality of the liquorice extract, and is favourable for monitoring the product quality.
Description
Technical field
The invention belongs to the Pharmaceutical Analysis detection range, relate to a kind of method for building up of licorice finger-print.
Background technology
Development along with the modern medicines analytical technology; Fingerprint pattern technology is the Quality Control pattern of current internationally recognized control traditional Chinese medicine quality; It in the cultivation of crude drug, introduce a fine variety, the standard of Chinese patent medicine production technology and optimization, aspects such as the formulation of target level of product quality all provide omnibearing quality assurance.
In recent years, the quality assessment of external centering herbal products is also being advocated finger-print.Along with the innovation of various analytical technologies and the continuous development of raising and Computer Applied Technology; Countries in the world are deepening continuously to the understanding and the research of natural drug; The traditional Chinese medicine fingerprint technology has become a kind of development trend at home and abroad; It is ripe perfect that the method for its research and technology more become, and becomes effective method of internationally recognized control Chinese medicine and crude drug quality and means.Japan's Chinese prescription medicine just adopts the high-efficiency liquid-phase fingerprint control of quality in the eighties in 20th century.The European Community also is applied to the autonomic drug quality control with the finger-print monitoring technique; FDA (Food and Drug Adminstration) (FDA) provides chromatographic fingerprint figure when allowing the herb supplement declaration material; Require autonomic drug aspect quality control, must work out the examination criteria of finger-print.The World Health Organization (WHO) estimates in the governing principle at herbal medicine in 1996 and also stipulates: if the active component of herbal medicine is not clear, chromatographic fingerprint figure can be provided the consistance with the proof product quality.Country such as Britain, India, Canada also attaches great importance to finger-print in the research of autonomic drug.In the pharmacopeia of many countries, chromatographic fingerprinting has become main method for separating and analyzing.At present, external many research institutions are mainly the correlation research of setting up finger-print and drug effect to the research of traditional Chinese medicine fingerprint, are to be master's pattern with tcm theory and new drug development research system.
In the Chinese medicine part of China's pharmacopeia, this analytical technology is not also occupied an leading position.In medical sci-tech the Tenth Five-Year Plan (2001-2005), bring forward the Chinese crude drug quality normalization problem that solves.2000, National Drug Administration issued " technical requirement (provisional) of traditional Chinese medicine finger-print research ", requires traditional Chinese medicine must carry out the research of finger-print, and set up its relevant standard.Standard the research of traditional Chinese medicine fingerprint, thereby promoted domestic in recent years to the research boom of finger-print.China still is in the junior stage to the research of traditional Chinese medicine fingerprint, and certain gap is arranged compared with developed countries.Be mainly at present that making ins all sorts of ways and set up the finger-print of Chinese crude drug and preparation, and corresponding information is carried out digitized processing, make it can estimate and control the quality of Chinese crude drug and preparation.
One of most important reason that influences the development of Chinese medicine and ethnic drug is the quality and quantity that can't confirm its effective constituent; Since this field of quality control that finger-print comes to light and is applied to Chinese medicine and ethnic drug; Obtain the support energetically and the popularization of country; Domestic many universities and research institute are all carrying out the work of this respect, and have obtained certain success, like ginkgo leaf, Radix Isatidis etc.More domestic well-known pharmacy corporations begin one's study and use chromatographic technique to improve the quality control standard of Chinese crude drug and products thereof; Pass through the effort of more than ten years along with the development of detection technique and instrument; The finger-print of existing several herbal species (injection) is succeedd; But utilize fingerprint pattern technology also not popularize, have only the famous strong pharmacy corporation of several families to obtain the finger-print of several tcm products and be applied to produce (the isatis root particle of White Cloud Mountain medicine company) at the study on the industrialization in solid preparation of traditional Chinese medicine field.
High performance liquid chromatography (HPLC) high performance liquid chromatography has the separation efficiency height, and analysis speed is fast, and quantitatively precision is high, and the detecting device kind is many, characteristics such as good stability.Do not receive the restriction of sample volatile grade and thermal stability, most of compositions all can carry out analyzing and testing in the sample on high performance liquid chromatograph, are one of main method that makes up by finger-print.
Peace stomach ulcer is a licorice, has tonifying middle-Jiao and Qi, detoxify and promote granulation; Suppress gastric secretion, repair and protect the effect of gastric mucosa, be applicable to stomach and duodenal bulbar ulcer; Better to asthenic cold type and Qi-stagnation type patient curative effect, also can be used for the treatment of keeping behind the ulcer healing.Present quality standard is the total content of tens kinds of total flavonoid compounds in the inspection peace stomach ulcer, can't embody the characteristic of various flavones, and quality does not obtain real effectively control, and the existing quality standard of for example pacifying stomach ulcer (bulk drug) is numbered WS
3-001-(Z-001)-98-(Z), wherein the method for regulation determination of total flavonoids is a gravimetric method, because the gravimetric method operate miss is bigger, receives artificial factor bigger, so reappearance is relatively poor.
Summary of the invention
The present invention utilizes the HPLC-TOF-MS technology, points out several flavones monomeric compounds with different chromatographic processes, finds out the fingerprint characteristic that it has characteristic, has set up the high performance liquid chromatography characteristic spectrum of flavones ingredient in the peace stomach ulcer.Obtain the chromatographic condition of this compounds, set up fingerprint file, make the quality of this compounds be able to real control,, also be the controlled foundation that reliably provides of its product for the raising of pacifying stomach ulcer quality standard provides technical support.
Therefore, the objective of the invention is, a kind of licorice is provided, for example pacify the finger-print method for building up of stomach ulcer.
Another object of the present invention is, a kind of licorice is provided, and for example pacifies the detection method of stomach ulcer.
The objective of the invention is to realize through following technical scheme.
On the one hand; The present invention provides a kind of licorice; Be preferably the finger-print method for building up of peace stomach ulcer; Said method comprises that the employing high performance liquid chromatography detects licorice, is preferably content of flavonoids in the peace stomach ulcer, and the condition of wherein said high performance liquid chromatography is following: chromatographic column is to fill phase with the octadecylsilane chemically bonded silica; Moving phase is that volume ratio is that the trifluoroacetic acid aqueous solution of the acetonitrile and 0.01 ~ 0.1% (volume ratio) of 22:78 ~ 75:25 carries out gradient elution; Flow velocity is 0.5 ~ 1.5 mL/min; Column temperature is 25 ~ 40 ℃; The ultraviolet detection wavelength is 270nm; Theoretical cam curve is pressed the chalcone A peak and is calculated, and should be not less than 3000.
Preferably, said method also comprises through following method and prepares reference substance solution: extracting liquorice chalcone A reference substance adds 70% (volume ratio) ethanol water and processes the solution that every 1ml contains 0.8mg, as reference substance solution.
Preferably, said method also comprises through following method and prepares need testing solution: extracting liquorice extract content 0.1g, put in the 25ml measuring bottle; Add 70% (volume ratio) ethanol water 20ml, ultrasonic Extraction 5 minutes is taken out; Put coldly, be settled to scale, shake up with 70% ethanol water; Filter with 0.2 μ m miillpore filter, as need testing solution.
In a preferred embodiment, method provided by the invention comprises the steps:
(1) preparation of reference substance solution: extracting liquorice chalcone A reference substance adds 70% (volume ratio) ethanol water and processes the solution that every 1ml contains 0.8mg, as reference substance solution;
(2) preparation of need testing solution: extracting liquorice extract content 0.1g, put in the 25ml measuring bottle, add 70% (volume ratio) ethanol water 20ml; Ultrasonic Extraction 5 minutes is taken out, and puts cold; Be settled to scale with 70% (volume ratio) ethanol water; Shake up, filter with 0.2 μ m miillpore filter, as need testing solution; And
(3) measure: accurate reference substance solution and each 10 μ l of need testing solution of drawing, inject high performance liquid chromatograph, measure according to following chromatographic condition, obtain finger-print:
Chromatographic column: Agela Venusil MP 5 μ m C
18-100 4.6 * 250mm;
Moving phase: volume ratio is the trifluoroacetic acid aqueous solution of the acetonitrile and 0.01% (volume ratio) of 22:78 ~ 75:25, carries out gradient elution;
Flow velocity: 1.0 mL/min;
Column temperature: 30 ℃;
Ultraviolet detection wavelength: 270 nm.
Preferably, said gradient elution program is undertaken by following volume ratio setting:
In the time of 0 minute, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 22% acetonitrile and 78%;
In the time of 10 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 25% acetonitrile and 75%;
In the time of 15 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 30% acetonitrile and 70%;
In the time of 25 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 35% acetonitrile and 65%;
In the time of 40 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 45% acetonitrile and 55%;
In the time of 80 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 60% acetonitrile and 40%;
In the time of 90 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 75% acetonitrile and 25%;
In the time of 100 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 75% acetonitrile and 25%.
Preferably; Comprise 7 characteristic peaks in the finger-print of said foundation, and the relative retention time of said each characteristic peak is respectively: 0.52 ± 0.05 (peak 1), 0.65 ± 0.05 (peak 2), 0.80 ± 0.05 (peak 3), 0.93 ± 0.05 (peak 4), 1.00 ± 0.05 (S peaks), 1.07 ± 0.05 (peaks 6), 1.15 ± 0.05 (peaks 7).
On the other hand, the present invention provides a kind of detection licorice, for example pacifies the method for flavone compound in the stomach ulcer, and the finger-print that said method adopts said method to set up detects licorice, for example pacifies the flavone compound in the stomach ulcer.
It is thus clear that; The inventor studies with different chromatographic processes and finds out the fingerprint characteristic that it has characteristic, obtains the chromatographic condition of this compounds, sets up fingerprint file; Make the quality of this compounds be able to real control, for the raising of pacifying stomach ulcer quality standard provides technical support.Particularly, through document retrieval and methodology demonstration, grope chromatographic condition (peak kind, peak area, retention time); Compare kind and content; Utilize high-efficient liquid phase technique to set up and be applicable to the finger-print of pacifying the stomach ulcer, improve the quality standard of peace stomach ulcer and preparation thereof, make controllable product quality reliable; According to finger-print, select to utilize raw material, improve product yield, increase economic benefit.
Method provided by the invention is easy, stable, precision is high, favorable reproducibility, can effectively characterize the quality of licorice (for example pacifying the stomach ulcer), and the quality that is used in monitoring product is arranged.
Description of drawings
Below, specify embodiment of the present invention in conjunction with accompanying drawing, wherein:
Figure 1A points out collection of illustrative plates for sample peak among the embodiment 2;
Figure 1B is a stack collection of illustrative plates in reference substance peak among the embodiment 2;
Fig. 2 is the finger-print of peace stomach ulcer provided by the invention;
Fig. 3 is precision is investigated among the embodiment 4 chromatogram figure as a result;
Fig. 4 is the chromatogram figure as a result of study on the stability among the embodiment 4;
Fig. 5 is repeatability is investigated among the embodiment 4 chromatogram figure as a result.
Embodiment
The concrete embodiment of following reference explains the present invention.It will be appreciated by those skilled in the art that these embodiment only are used to explain the present invention, the scope that it does not limit the present invention in any way.
Below employed reference substance source is as follows among each embodiment:
Liquiritin, available from Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 111610-200604; Ammonium glycyrrhetate, available from Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 111731-200614; Licochalcone A, available from Tongtian Biochemical Technology Co., Ltd., Shanghai, lot number: 10091421.
Below among each embodiment employed test sample can pacify pharmaceutcal corporation, Ltd entirely available from Xinjiang, its preparation method is following: learn from else's experience and extract the glycyrrhiza residue behind extract of licorice root or the glycyrrhizic acid powder, with twice of the extraction of the ethanol water more than 93%; Every all over 1 hour, merge extract and be concentrated into the thick paste shape, add 2.0% sodium carbonate liquor dissolving; Precipitate 24 hours; Get supernatant and be neutralized to pH value 2-3 with 10.0% hydrochloric acid, filter, sediment washs to pH value 6 with purified water; Sediment promptly gets licorice after 40-50 ℃ of drying.
Below among each embodiment employed chromatograph be U.S. Agilent 1100 series (the online vacuum degassing machine of G1322A, G1311A quaternary gradient pump, G1313A automatic sampler, G1316A column oven, G1315B PDADs).
Embodiment 1The preparation of need testing solution
Present embodiment is investigated from the preparation method of following several respects to need testing solution.
1, extracts solvent
With water, 30% ethanol water, 50% ethanol water, 70% ethanol water, absolute ethyl alcohol serves as to extract solvent, adopts ultrasonic extracting method, investigates carried out the extraction solvent with a collection of test sample.
The result shows (scheming not shown); Water and 30% ethanol water extraction ratio are low excessively; And the chromatographic peak composition does not almost extract behind the 40min; 50% ethanol water is suitable with 70% ethanol water extraction effect, and the absolute ethyl alcohol extraction ratio is lower than 50% ethanol water and 70% ethanol water, therefore select for use with pharmacopeia in 70% identical ethanol water of content assaying method extract solvent as test sample.
2, test sample sampling amount
Precision takes by weighing peace stomach ulcer content 0.02g, 0.05g, 0.1g respectively, 0.2g puts in the 25ml measuring bottle, is solvent with 70% ethanol water, ultrasonic Extraction 30 minutes, preparation test sample.
The result shows, sampling amount 0.02 ~ 0.05g, more chromatographic peak response is corresponding lower in the collection of illustrative plates (not shown), and take a sample 0.1, each chromatogram cutting edge of a knife or a sword composition of 0.2g all can obviously show in collection of illustrative plates, considers the protection of chromatographic column, selects then 0.1g as the test sample sampling amount.
3, extraction time is investigated
When sampling amount is investigated, find that content is prone to dissolving, has investigated 15,30,45 minutes extraction effect of ultrasonic time respectively when therefore investigating extraction time, and has used the method for artificial jolting to prepare a test sample simultaneously.
The result finds; Four kinds of methods are indifference almost, but jolting extracts and need jolting energetically that sample is all dissolved, relatively effort; Therefore investigated the method for ultrasonic 5 minutes hydrotropies again; Contrast collection of illustrative plates (not shown), also therefore indifference selects the method for easy-operating ultrasonic 5 minutes hydrotropies to prepare test sample.
Embodiment 2Chromatographic condition and system suitability test are investigated
Present embodiment has carried out the test investigation from following each side to the chromatographic condition of peace stomach ulcer finger-print with system suitability.
1, the selection of fingerprint atlas detection method
Literature survey shows that composition is main with flavones ingredient mainly in the glycyrrhiza residue, and specific examples of such components all has uv absorption preferably, therefore selects for use the HPLC-UV detection method to carry out finger-print research.
2, finger-print detects the selection of wavelength
Literature research shows, mainly contains flavones ingredient in the glycyrrhiza residue, and wherein mostly is chalcone, flavanone, isoflavones etc., and still contains the glycyrrhizin constituents in the Radix Glycyrrhizae crude drug, and its ultraviolet is inhaled wavelength characteristic and had nothing in common with each other, and has bibliographical information to use the wavelength gradient; Adopt PDAD that sample is carried out the long detection of all-wave; According to the three-dimensional collection of illustrative plates of collecting (scheming not shown), and collect the collection of illustrative plates (scheming not shown) of 245 nm, 270 nm, 276nm (liquiritin absorption maximum), 330nm, 360 nm wavelength simultaneously.
Integrated survey, glycyrrhiza residue is suitable at the quantity of information maximum and the chromatographic peak peak height of 270 nm wavelength, and therefore last definite 270 nm are the detection wavelength of glycyrrhiza residue finger-print.
3, finger-print reference substance peak is pointed out
In the research process; Peace stomach ulcer sample has been carried out the HPLC-MS analysis; Through the HPLC-MS data; And complementary clause is offered report and reference substance is pointed out (reference substance stack collection of illustrative plates is seen Figure 1B), confirms that containing liquiritin, glycyrrhizic acid, onocerin and Radix Glycyrrhizae in the peace stomach ulcer sample looks into youngster's ketone A composition and the corresponding chromatographic peak of each composition, specifically referring to Figure 1A.
4, chromatographic column is investigated
Agela, Agilent, GRACE and four kinds of chromatographic columns of Kromasil have been investigated respectively.
The result shows that the detection collection of illustrative plates of four kinds of chromatographic columns has nothing in common with each other, to the separation of chromatographic peak have their own characteristics each (scheming not shown).Relatively; Under similarity condition; The Agela chromatographic column is best to the degree of separation of each chromatographic peak of sample, and most of chromatogram peak energy reaches basic separation, therefore selects for use Agela Venusil MP 5 μ m C18-100 4.6 * 250mm chromatographic column to carry out the mensuration of glycyrrhiza residue finger-print.
5, the moving phase elution system is investigated
At the experiment initial stage, once list of references has been investigated acetonitrile-0.4% glacial acetic acid water, acetonitrile-0.1% phosphoric acid water system respectively when groping the finger-print chromatographic condition, comparing result, and phosphoric acid water is superior to glacial acetic acid water to the separating effect of chromatographic peak; After compared acetonitrile-0.01% trifluoracetic acid water system again; The result finds that phosphoric acid water is suitable to the separating effect of most of chromatographic peak with the trifluoracetic acid water system; Have only indivedual chromatographic peaks slightly variant; The separating effect (scheming not shown) of comprehensive each chromatographic peak confirms to use acetonitrile-0.01% trifluoracetic acid water as finger-print chromatography eluant system, carries out follow-up chromatographic condition and gropes.
6, the investigation of column flow rate
According to the HPLC chromatographic condition, investigated different column flow rate (1.1 ml/min, 1.0 ml/min, 0.9 ml/min) respectively.
The result shows that the influence of each component separating effect of column flow rate is not obvious, and the flow velocity separating effect of only indivedual chromatographic peak 1.0 ml/min is (scheme not shown) better, so to select column flow rate for use be 1.0ml/min.
7, column temperature is investigated
According to the HPLC chromatographic condition, 3 kinds of column temperatures (25 ℃, 30 ℃, 35 ℃) have been investigated respectively.
The result shows that the influence of each chromatographic peak component separating effect of column temperature is not obvious, slightly variant (scheming not shown), the chromatographic peak separating effect of 50 ~ 60min is little good in the time of 30 ℃, and therefore selecting column temperature for use is 30 ℃.
8,2 times of chromatographic peak acquisition times of finger-print chromatographic condition are investigated
Behind the need testing solution sample introduction, the chromatogram of record 200min investigates whether go out peak (scheming not shown) fully.
The result shows, under this chromatographic condition, do not detect chromatographic peak in 100 minutes later on.
9, moving phase is blank investigates
Under the HPLC chromatographic condition, sample introduction list working procedure is investigated 100 minutes chromatogram, does not detect any chromatographic peak (scheming not shown), and the result shows that the moving phase blank detects the nothing influence to finger-print.
10, the investigation of blank solvent influence
100 minutes chromatogram of record blank solvent (70% ethanol water) does not detect any chromatographic peak (scheming not shown) under the HPLC chromatographic condition, and the result shows that blank solvent detects the nothing influence to finger-print.
Embodiment 3The detection of licoflavone class material in the peace stomach ulcer
1. chromatographic column: model is Agela Venusil MP 5 μ m C
18-100 4.6 * 250mm;
2. moving phase: with the acetonitrile is mobile phase A, is Mobile phase B with 0.01% trifluoracetic acid (TFA) solution, and the regulation in the according to the form below is carried out gradient elution;
3. flow velocity: 1.0mL/ minute;
4. detection wavelength: 270nm;
5. column temperature is 30 ℃;
6. the preparation of reference substance solution: extracting liquorice chalcone A reference substance is an amount of, adds 70% ethanol water and processes the solution that every 1ml contains 0.8mg, promptly gets.
7. the preparation of need testing solution: take by weighing peace stomach ulcer content 0.1g, put in the 25ml measuring bottle, add 70% ethanol 20ml, ultrasonic Extraction 5 minutes is taken out, and puts coldly, is settled to scale with 70% ethanol, shakes up, and with the filtration of 0.2 μ m miillpore filter, promptly gets.
8. determination method: accurate respectively each the 10 μ l of reference substance solution and need testing solution that draw, inject liquid chromatograph, mensuration writes down 100 minutes chromatogram.
Embodiment 4Methodological study
1, precision is investigated
The preparation need testing solution, with reference to the method for embodiment 3, continuous sample introduction 6 times is measured characteristic spectrum, and the stacking diagram sees Fig. 3, utilizes finger-print software evaluation similarity, and the result shows that instrument precision is good.
2, study on the stability
The preparation need testing solution is with reference to the method for embodiment 3, respectively near 0,3.5,7,11,15,24 hour sample introduction; Measure characteristic spectrum, the stacking diagram sees Fig. 4, adopts its similarity of finger-print computed in software; The result shows, measures in 24 hours, and need testing solution is stable.
3, repeatability is investigated
6 parts of need testing solutions of parallel preparation are measured characteristic spectrum with reference to the method for embodiment 3, and the characteristic spectrum stacking diagram sees Fig. 5, utilizes its similarity of finger-print computed in software, and the result shows that method repeatability is good.
Embodiment 5The foundation of characteristic spectrum common pattern
With reference to the method for embodiment 3, detected the peace stomach ulcer of 2008 (4 batches), 2009 (16 batches) production." chromatographic fingerprints of Chinese materia medica similarity evaluation system, the 2004A version " software that uses pharmacopoeia commission to recommend utilizes 20 batches of peace stomach ulcer characteristic spectrums to generate common pattern figure, specifically describes as follows:
1, characteristic spectrum mark: combine 20 batches of peace stomach ulcer characteristic spectrum characteristics, the total chromatographic peak of mark is 15 altogether, and is as shown in Figure 2; The liquiritin composition chromatographic peak that marks in the collection of illustrative plates only 08 is being produced four batches and 09 per year and is being produced per year lot number and be 20090210 ~ 20090313 seven batches and totally ten a collection ofly obviously detect in 20 batches of peace stomach ulcer samples; Other all do not detect; Therefore the liquiritin composition is defined as non-total peak, and No. 2 peaks are the acromion that contains the onocerin composition.
2, the characteristic spectrum similarity is calculated: 20 batches of peace stomach ulcers are calculated similarity jointly, and the result sees table 1, and the result shows; 20 batches of similarities of pacifying stomach ulcer and common pattern are between 0.929 ~ 0.985; Mean value reaches 0.963, explains that each batch sample room homogeneity is fine, and sample is stable.
20 batches of peaces of table 1 stomach ulcer similarity result
3, each characteristic peak relative retention time of peace stomach ulcer characteristic spectrum is calculated
Utilizing 20 batches of each chromatographic peak retention time data of peace stomach ulcer characteristic spectrum, is with reference to peak S with licochalcone A, calculates the relative retention time at other 6 characteristic peaks and S peak, and the average that draws 20 batch datas is formulated the relative retention time standard; The result obtains each chromatographic peak with following with reference to the peak relative retention time: 0.52 (peak 1), 0.65 (peak 2), 0.80 (peak 3), 0.93 (peak 4), 1.00 (peak S), 1.07 (peaks 6), 1.15 (peaks 7); Error between consideration chromatographic column and detecting instrument, tentative inspection limit are within setting ± 5%.
Claims (7)
1. a licorice is preferably the method for building up of pacifying stomach ulcer finger-print, and said method comprises that the employing high performance liquid chromatography detects licorice, is preferably content of flavonoids in the peace stomach ulcer, and the condition of wherein said high performance liquid chromatography is following:
Chromatographic column: with the octadecylsilane chemically bonded silica is to fill phase;
Moving phase: volume ratio is the trifluoroacetic acid aqueous solution of the acetonitrile and 0.01 ~ 0.1% (volume ratio) of 22:78 ~ 75:25, carries out gradient elution;
Flow velocity: 0.5 ~ 1.5 mL/min;
Column temperature: 25 ~ 40 ℃;
Ultraviolet detection wavelength: 270nm;
Theoretical cam curve is pressed the chalcone A peak and is calculated, and should be not less than 3000.
2. method according to claim 1 is characterized in that, said method also comprises through following method and prepares reference substance solution: extracting liquorice chalcone A reference substance adds 70% ethanol water and processes the solution that every 1ml contains 0.8mg, as reference substance solution.
3. method according to claim 1 and 2 is characterized in that, extracting liquorice extract content 0.1g; Put in the 25ml measuring bottle, add 70% (volume ratio) ethanol water 20ml, ultrasonic Extraction 5 minutes; Take out, put coldly, be settled to scale with 70% (volume ratio) ethanol water; Shake up, filter with 0.2 μ m miillpore filter, as need testing solution.
4. according to each described method in the claim 1 to 3, it is characterized in that said method comprises the steps:
(1) preparation of reference substance solution: extracting liquorice chalcone A reference substance adds 70% ethanol water and processes the solution that every 1ml contains 0.8mg, as reference substance solution;
(2) preparation of need testing solution: extracting liquorice extract content 0.1g, put in the 25ml measuring bottle, add 70% ethanol water 20ml, ultrasonic Extraction 5 minutes; Take out, put coldly, be settled to scale with 70% ethanol water; Shake up, filter with 0.2 μ m miillpore filter, as need testing solution; And
(3) measure: accurate reference substance solution and each 10 μ l of need testing solution of drawing, inject high performance liquid chromatograph, measure according to following chromatographic condition, obtain finger-print:
Chromatographic column: Agela Venusil MP 5 μ m C
18-100 4.6 * 250mm;
Moving phase: volume ratio is the trifluoroacetic acid aqueous solution of the acetonitrile and 0.01% (volume ratio) of 22:78 ~ 75:25, carries out gradient elution;
Flow velocity: 1.0 mL/min;
Column temperature: 30 ℃;
Ultraviolet detection wavelength: 270nm.
5. according to each described method in the claim 1 to 4, it is characterized in that said gradient elution program is undertaken by following volume ratio setting:
In the time of 0 minute, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 22% acetonitrile and 78%;
In the time of 10 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 25% acetonitrile and 75%;
In the time of 15 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 30% acetonitrile and 70%;
In the time of 25 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 35% acetonitrile and 65%;
In the time of 40 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 45% acetonitrile and 55%;
In the time of 80 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 60% acetonitrile and 40%;
In the time of 90 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 75% acetonitrile and 25%;
In the time of 100 minutes, moving phase is the trifluoroacetic acid aqueous solution of 0.01% (volume ratio) of 75% acetonitrile and 25%.
6. according to each described method in the claim 1 to 5, it is characterized in that, comprise 7 characteristic peaks in the finger-print of said foundation, and the relative retention time of said characteristic peak be respectively:
Peak 1:0.52 ± 0.05; Peak 2:0.65 ± 0.05; Peak 3:0.80 ± 0.05; Peak 4:0.93 ± 0.05; S peak: 1.00 ± 0.05; Peak 6:1.07 ± 0.05; Peak 7:1.15 ± 0.05.
7. one kind is detected licorice, is preferably the method for flavone compound in the peace stomach ulcer, and said method adopts the finger-print that each said method is set up in the claim 1 to 6 to detect licorice, is preferably flavone compound in the peace stomach ulcer.
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| CN102680629A (en) * | 2012-05-18 | 2012-09-19 | 新疆全安药业有限公司 | Method for establishing Anweiyang capsule fingerprint spectrum |
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| CN104721256A (en) * | 2015-02-15 | 2015-06-24 | 新疆全安药业有限公司 | Anwei Yang extract as well as preparation method and medical application thereof |
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| CN109633006B (en) * | 2018-12-27 | 2021-07-30 | 广州白云山陈李济药厂有限公司 | Construction method and application of fingerprint of Weiyang ning |
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