CN102680628B - Method for establishing fingerprint of An Weiyang - Google Patents
Method for establishing fingerprint of An Weiyang Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 50
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 63
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims abstract description 45
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 claims abstract description 16
- 239000000284 extract Substances 0.000 claims abstract description 13
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 12
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 claims abstract description 7
- 238000010828 elution Methods 0.000 claims abstract description 6
- 244000303040 Glycyrrhiza glabra Species 0.000 claims abstract description 5
- 208000007107 Stomach Ulcer Diseases 0.000 claims description 36
- 201000005917 gastric ulcer Diseases 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 33
- 238000012360 testing method Methods 0.000 claims description 25
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- 241000202807 Glycyrrhiza Species 0.000 claims description 11
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- 229930003944 flavone Natural products 0.000 claims description 11
- 235000011949 flavones Nutrition 0.000 claims description 11
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- 230000014759 maintenance of location Effects 0.000 claims description 8
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- 235000005513 chalcones Nutrition 0.000 claims description 6
- -1 flavone compound Chemical class 0.000 claims description 6
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- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 claims description 4
- 229960004949 glycyrrhizic acid Drugs 0.000 claims description 4
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- 239000013049 sediment Substances 0.000 claims description 4
- VTAJIXDZFCRWBR-UHFFFAOYSA-N Licoricesaponin B2 Natural products C1C(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2)C(O)=O)C)(C)CC2)(C)C2C(C)(C)CC1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O VTAJIXDZFCRWBR-UHFFFAOYSA-N 0.000 claims description 3
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- DEMKZLAVQYISIA-ONJCETCRSA-N Liquiritin Natural products O([C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1)c1ccc([C@@H]2Oc3c(C(=O)C2)ccc(O)c3)cc1 DEMKZLAVQYISIA-ONJCETCRSA-N 0.000 description 5
- DEMKZLAVQYISIA-UHFFFAOYSA-N Liquirtin Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(C2OC3=CC(O)=CC=C3C(=O)C2)C=C1 DEMKZLAVQYISIA-UHFFFAOYSA-N 0.000 description 5
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- 206010021703 Indifference Diseases 0.000 description 2
- IUCVKTHEUWACFB-UHFFFAOYSA-N Licochalcone A Natural products COC1=CC=C(C(C)(C)C=C)C=C1C=CC(=O)C1=CC=C(O)C=C1 IUCVKTHEUWACFB-UHFFFAOYSA-N 0.000 description 2
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- 229930194248 Licoflavone Natural products 0.000 description 1
- MEHHCBRCXIDGKZ-UHFFFAOYSA-N Licoflavone C Natural products CC(C)=CCC1=C(O)C=C(O)C(C(C=2)=O)=C1OC=2C1=CC=C(O)C=C1 MEHHCBRCXIDGKZ-UHFFFAOYSA-N 0.000 description 1
- ZONYXWQDUYMKFB-UHFFFAOYSA-N SJ000286395 Natural products O1C2=CC=CC=C2C(=O)CC1C1=CC=CC=C1 ZONYXWQDUYMKFB-UHFFFAOYSA-N 0.000 description 1
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- 229930003949 flavanone Natural products 0.000 description 1
- 150000002208 flavanones Chemical class 0.000 description 1
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- CJWQYWQDLBZGPD-UHFFFAOYSA-N isoflavone Natural products C1=C(OC)C(OC)=CC(OC)=C1C1=COC2=C(C=CC(C)(C)O3)C3=C(OC)C=C2C1=O CJWQYWQDLBZGPD-UHFFFAOYSA-N 0.000 description 1
- 150000002515 isoflavone derivatives Chemical class 0.000 description 1
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- Investigating Or Analysing Biological Materials (AREA)
- Medicines Containing Plant Substances (AREA)
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 Pharmaceutical Analysis detection field, relate to a kind of method for building up of licorice finger-print.
Background technology
Along with the development of modern medicines analytical technology, fingerprint pattern technology is the Quality Control pattern of current internationally recognized control traditional Chinese medicine quality, it crude drug cultivation, introduce a fine variety, the specification of Chinese patent drug production technology and optimization, the aspects such as the formulation of target level of product quality all provide omnibearing quality assurance.
In recent years, also finger-print is being advocated to the quality assessment of herbal product abroad.Along with the innovation of various analytical technology and the development of raising and Computer Applied Technology, countries in the world are deepening continuously to the understanding of natural drug and research, traditional Chinese medicine fingerprint technology has become a kind of development trend at home and abroad, Method and Technology of its research is more ripe perfect, becomes the most effective method of internationally recognized control Chinese medicine and crude drug quality and means.Japanese Kampo medicine just adopts high-efficiency liquid-phase fingerprint Mass Control in the eighties in 20th century.Finger-print monitoring technique is also applied to autonomic drug quality control by the European Community, FDA (Food and Drug Adminstration) (FDA) allows to provide chromatographic fingerprint figure during herb supplement declaration material, require that autonomic drug is in quality control, must work out the examination criteria of finger-print.The World Health Organization (WHO) evaluates in governing principle at herbal medicine in 1996 and also specifies: if the active component of herbal medicine is failed to understand, chromatographic fingerprint figure can be provided to prove the consistance of product quality.The country such as Britain, India, Canada, in the research of autonomic drug, also attaches great importance to finger-print.In the pharmacopeia of many countries, chromatographic fingerprinting has become main method for separating and analyzing.At present, the research of external many research institutions to traditional Chinese medicine fingerprint is mainly the correlation research setting up finger-print and drug effect, is the pattern based on 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 and solve Chinese crude drug quality normalization problem.2000, National Drug Administration promulgated " technical requirement (provisional) of traditional Chinese medicine finger-print research ", requires that traditional Chinese medicine must carry out the research of finger-print, and sets up its relevant standard.The specification research of traditional Chinese medicine fingerprint, thus facilitate domestic in recent years to the research boom of finger-print.The research of China to traditional Chinese medicine fingerprint is still in the junior stage, and has certain gap compared with developed countries.Be mainly the finger-print using various method establishment Chinese crude drug and preparation at present, and digitized processing is carried out to corresponding information, can evaluate and control the quality of Chinese crude drug and preparation.
Affecting one of most important reason of Chinese medicine and ethnic drug development is the quality and quantity cannot determining its effective constituent, since finger-print is found this field of quality control being applied to Chinese medicine and ethnic drug, obtain support energetically and the popularization of country, domestic many universities and research institute are all carrying out the work of this respect, and obtain certain success, as ginkgo leaf, Radix Isatidis etc.More domestic well-known pharmacy corporations begin one's study and use the quality control standard of chromatographic technique raising Chinese crude drug and products thereof, along with the development of detection technique and instrument is through the effort of more than ten years, the finger-print of existing several herbal species (injection) succeeds, but utilize fingerprint pattern technology also not popularize at the study on the industrialization in solid preparation of traditional Chinese medicine field, the strong pharmacy corporation only having several family famous obtains the finger-print of several tcm product and is applied to production (the isatis root particle of White Cloud Mountain medicine company).
It is high that high performance liquid chromatography (HPLC) high performance liquid chromatography has separation efficiency, and analysis speed is fast, and quantitative precision is high, and detecting device kind is many, the features such as good stability.Be not subject to the restriction of sample volatile grade and thermal stability, in sample, most of composition all can carry out analysis detection on high performance liquid chromatograph, is one of main method building finger-print.
Peace stomach ulcer is 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 maintaining treatment after ulcer healing.Current quality standard is the total content checking tens kinds of Flavonoids in peace stomach ulcer, cannot embody the feature of various flavones, and quality does not obtain real effective control, and the existing quality standard of such as pacifying stomach ulcer (bulk drug) is numbered WS
3-001-(Z-001)-98-(Z), wherein the method for regulation determination of total flavonoids is gravimetric method, and because gravimetric method operate miss is comparatively large, the impact by human factor is comparatively large, therefore reappearance is poor.
Summary of the invention
The present invention utilizes HPLC-TOF-MS technology, points out several flavones monomeric compounds by different chromatographic processes, finds out the characteristic fingerprint characteristic of its tool, establishes the high performance liquid chromatography characteristic spectrum of flavones ingredient in 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, for the raising of peace stomach ulcer quality standard provides technical support, also for the controlled of its product reliably provides foundation.
Therefore, the object of the invention is, a kind of licorice is provided, such as, pacify the fingerprint of stomach ulcer.
Another object of the present invention is, provides a kind of licorice, such as, pacify the detection method of stomach ulcer.
The object of the invention is to be achieved through the following technical solutions.
On the one hand, the invention provides a kind of licorice, be preferably the fingerprint of peace stomach ulcer, described method comprises employing high performance liquid chromatography and detects licorice, be preferably the content of flavone compound in peace stomach ulcer, the condition of wherein said high performance liquid chromatography is as follows: chromatographic column is fill phase with octadecylsilane chemically bonded silica; Acetonitrile and 0.01 ~ 0.1%(volume ratio of mobile phase to be volume ratio be 22:78 ~ 75:25) trifluoroacetic acid aqueous solution carry out gradient elution; Flow velocity is 0.5 ~ 1.5 mL/min; Column temperature is 25 ~ 40 DEG C; UV detect wavelength is 270nm; Theoretical cam curve is pressed chalcone A peak and is calculated, and should be not less than 3000.
Preferably, described method also comprises and prepares reference substance solution by the following method: extracting Radix Glycyrrhizae chalcone A reference substance, adds 70%(volume ratio) ethanol water makes every 1ml containing the solution of 0.8mg, product solution in contrast.
Preferably, described method also comprises and prepares need testing solution by the following method: extracting Radix Glycyrrhizae extract content 0.1g, put in 25ml measuring bottle, add 70%(volume ratio) ethanol water 20ml, ultrasonic extraction 5 minutes, take out, let cool, be settled to scale with 70% ethanol water, shake up, filter, as need testing solution with 0.2 μm of miillpore filter.
In a preferred embodiment, method provided by the invention comprises the steps:
(1) preparation of reference substance solution: extracting Radix Glycyrrhizae chalcone A reference substance, adds 70%(volume ratio) ethanol water makes every 1ml containing the solution of 0.8mg, product solution in contrast;
(2) preparation of need testing solution: extracting Radix Glycyrrhizae extract content 0.1g, put in 25ml measuring bottle, add 70%(volume ratio) ethanol water 20ml, ultrasonic extraction 5 minutes, takes out, lets cool, with 70%(volume ratio) ethanol water is settled to scale, shake up, filter, as need testing solution with 0.2 μm of miillpore filter; And
(3) measure: accurate absorption reference substance solution and each 10 μ l of need testing solution, inject high performance liquid chromatograph, measure according to following chromatographic condition, obtain finger-print:
Chromatographic column: Agela Venusil MP 5 μm of C
18-100 4.6 × 250mm;
Mobile phase: volume ratio is acetonitrile and the 0.01%(volume ratio of 22:78 ~ 75:25) trifluoroacetic acid aqueous solution, carry out gradient elution;
Flow velocity: 1.0 mL/min;
Column temperature: 30 DEG C;
UV detect wavelength: 270 nm.
Preferably, described gradient elution program arranges by following volume ratio and carries out:
When 0 minute, mobile phase is the acetonitrile of 22% and the 0.01%(volume ratio of 78%) trifluoroacetic acid aqueous solution;
When 10 minutes, mobile phase is the acetonitrile of 25% and the 0.01%(volume ratio of 75%) trifluoroacetic acid aqueous solution;
When 15 minutes, mobile phase is the acetonitrile of 30% and the 0.01%(volume ratio of 70%) trifluoroacetic acid aqueous solution;
When 25 minutes, mobile phase is the acetonitrile of 35% and the 0.01%(volume ratio of 65%) trifluoroacetic acid aqueous solution;
When 40 minutes, mobile phase is the acetonitrile of 45% and the 0.01%(volume ratio of 55%) trifluoroacetic acid aqueous solution;
When 80 minutes, mobile phase is the acetonitrile of 60% and the 0.01%(volume ratio of 40%) trifluoroacetic acid aqueous solution;
When 90 minutes, mobile phase is the acetonitrile of 75% and the 0.01%(volume ratio of 25%) trifluoroacetic acid aqueous solution;
When 100 minutes, mobile phase is the acetonitrile of 75% and the 0.01%(volume ratio of 25%) trifluoroacetic acid aqueous solution.
Preferably, the finger-print of described foundation comprises 7 characteristic peaks, and the relative retention time of described 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 peak), 1.07 ± 0.05(peak 6), 1.15 ± 0.05(peak 7).
On the other hand, the invention provides a kind of detection licorice, such as pacify the method for flavone compound in stomach ulcer, the finger-print that described method adopts said method to set up detects licorice, such as, pacify the flavone compound in stomach ulcer.
Visible, the present inventor's research finds out the characteristic fingerprint characteristic of its tool by different chromatographic processes, obtains the chromatographic condition of this compounds, sets up fingerprint file, the quality of this compounds is made to be able to real control, for the raising of peace stomach ulcer quality standard provides technical support.Particularly, by document retrieval and methodology demonstration, chromatographic condition (peak kind, peak area, retention time) is groped, relatively kind and content, utilize high-efficient liquid phase technique foundation to be applicable to pacify the finger-print of stomach ulcer, improve the quality standard of peace stomach ulcer and preparation thereof, make product quality reliably controlled; According to finger-print, Selection utilization raw material, improves product yield, increases economic benefit.
Method provided by the invention is easy, stable, precision is high, favorable reproducibility, and the quality of energy Efficient Characterization licorice (such as pacifying stomach ulcer), has the quality being used in monitoring product.
Accompanying drawing explanation
Below, describe embodiment of the present invention in detail by reference to the accompanying drawings, wherein:
Figure 1A is that in embodiment 2, collection of illustrative plates is pointed out at sample peak;
Figure 1B is superposition collection of illustrative plates in reference substance peak in embodiment 2;
Fig. 2 is the finger-print of peace stomach ulcer provided by the invention;
Fig. 3 is the chromatographic results figure that in embodiment 4, precision is investigated;
Fig. 4 is the chromatographic results figure of study on the stability in embodiment 4;
Fig. 5 is the chromatographic results figure that in embodiment 4, repeatability is investigated.
Embodiment
Referring to specific embodiment, the present invention is described.It will be appreciated by those skilled in the art that these embodiments are only for illustration of the present invention, its scope do not limited the present invention in any way.
The reference substance source used in following embodiment is as follows:
Liquiritin, purchased from Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 111610-200604; Ammonium glycyrrhetate, purchased from Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 111731-200614; Licochalcone A, purchased from Tongtian Biochemical Technology Co., Ltd., Shanghai, lot number: 10091421.
The test sample used in following embodiment can purchased from Xinjiang Quanan Pharmaceutical Co., Ltd., its preparation method is as follows: the glycyrrhiza residue of learning from else's experience after extracting extract of licorice root or glycyrrhizic acid powder, ethanol water with more than 93% extracts twice, often all over 1 hour, merge extract and be concentrated into paste, the sodium carbonate liquor adding 2.0% dissolves, precipitate 24 hours, get supernatant with 10.0% hydrochloric acid be neutralized to pH value 2-3, filter, sediment is with purified water washing to pH value 6, and sediment, after 40-50 DEG C of drying, obtains licorice.
The chromatograph used in following embodiment is U.S. Agilent 1100 series (the online vacuum degassing machine of G1322A, G1311A quaternary gradient pump, G1313A automatic sampler, G1316A column oven, G1315B diode array detector).
embodiment 1the preparation of need testing solution
The present embodiment is investigated from the preparation method of following several respects to need testing solution.
1, Extraction solvent
With water, 30% ethanol water, 50% ethanol water, 70% ethanol water, absolute ethyl alcohol for Extraction solvent, adopt ultrasonic extracting method, carried out Extraction solvent investigation to a collection of test sample.
Result shows (scheming not shown), water and 30% ethanol water extraction ratio too low, and chromatographic peak composition does not almost extract after 40min, 50% ethanol water is suitable with 70% ethanol water extraction effect, absolute ethyl alcohol extraction ratio, lower than 50% ethanol water and 70% ethanol water, therefore selects 70% ethanol water identical with content assaying method in pharmacopeia as test sample Extraction solvent.
2, test sample sampling amount
Precision takes peace stomach ulcer content 0.02g, 0.05g, 0.1g, 0.2g and puts in 25ml measuring bottle respectively, and with 70% ethanol water for solvent, ultrasonic extraction 30 minutes, prepares test sample.
Result shows, sampling amount 0.02 ~ 0.05g, and in collection of illustrative plates (not shown), more chromatographic peak response is corresponding lower, and sample 0.1,0.2g each chromatogram cutting edge of a knife or a sword composition all can obviously show in collection of illustrative plates, considers the protection of chromatographic column, select then 0.1g as test sample sampling amount.
3, extraction time is investigated
When sampling amount is investigated, find that content is more soluble, when therefore investigating extraction time, investigated the ultrasonic time extraction effect of 15,30,45 minutes respectively, and a test sample that simultaneously used the method for artificial jolting to prepare.
Found that, four kinds of methods almost indifference, but jolting is extracted needs jolting energetically that sample just can be made all to dissolve, relatively effort, therefore the method for ultrasonic 5 minutes hydrotropies has been investigated again, contrast collection of illustrative plates (not shown), also indifference, therefore selects the method for easy-operating ultrasonic 5 minutes hydrotropies to prepare test sample.
embodiment 2chromatographic condition and system suitability are investigated
The present embodiment from following aspect to the chromatographic condition of peace stomach ulcer finger-print and and system suitability carried out experiment investigation.
1, the selection of fingerprint atlas detection method
Literature survey shows, in glycyrrhiza residue, composition is mainly based on flavones ingredient, and specific examples of such components all has good uv absorption, therefore selects HPLC-UV detection method to carry out finger-print research.
2, the selection of finger-print determined wavelength
Literature research shows, mainly containing flavones ingredient in glycyrrhiza residue, mostly wherein is chalcone, flavanone, isoflavones etc., and still containing glycyrrhizin constituents in Radix Glycyrrhizae crude drug, it is different that its ultraviolet inhales wavelength characteristic, has bibliographical information to use wavelength gradient; Diode array detector is adopted to carry out full wavelength detecting to sample, according to collect three-dimensional collection of illustrative plates (scheming not shown), and collect 245 nm, 270 nm, 276nm(liquiritin absorption maximum simultaneously), 330nm, 360 nm wavelength places collection of illustrative plates (scheming not shown).
Integrated survey, glycyrrhiza residue is suitable at the maximum and chromatographic peak peak height of the quantity of information at 270 nm wavelength places, therefore finally determines that 270 nm are the determined wavelength of glycyrrhiza residue finger-print.
3, finger-print reference substance peak is pointed out
In research process, HPLC-MS analysis has been carried out to peace stomach ulcer sample, by HPLC-MS data, and tie bibliographical information and reference substance points out (reference substance superposition collection of illustrative plates see Figure 1B), determine to pacify in stomach ulcer sample and look into youngster's ketone A composition and chromatographic peak corresponding to each composition, specifically see Figure 1A containing liquiritin, glycyrrhizic acid, onocerin and Radix Glycyrrhizae.
4, chromatographic column is investigated
Agela, Agilent, GRACE and Kromasil tetra-kinds of chromatographic columns are investigated respectively.
Result shows, the detection collection of illustrative plates of four kinds of chromatographic columns is different, has their own characteristics each (scheming not shown) to the separation of chromatographic peak.Relatively, under similarity condition, 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 Agela Venusil MP 5 μm of C18-100 4.6 × 250mm chromatographic columns to carry out the mensuration of glycyrrhiza residue finger-print.
5, mobile phase elution system is investigated
At the experiment initial stage, when groping finger-print chromatographic condition, once list of references has investigated acetonitrile-0.4% glacial acetic acid water, acetonitrile-0.1% phosphoric acid water system respectively, comparing result, and the separating effect of phosphoric acid water to chromatographic peak is better than glacial acetic acid water; After compare again acetonitrile-0.01% trifluoracetic acid water system, found that phosphoric acid water is suitable with the separating effect of trifluoracetic acid water system to most of chromatographic peak, only has indivedual chromatographic peak slightly difference, the separating effect (scheming not shown) of comprehensive each chromatographic peak, determine to use acetonitrile-0.01% trifluoracetic acid water as finger-print chromatography eluant system, carry out follow-up chromatographic condition and grope.
6, the investigation of column flow rate
According to HPLC chromatographic condition, investigate different column flow rate (1.1 ml/min, 1.0 ml/min, 0.9 ml/min) respectively.
Result shows, the impact of column flow rate each component separating effect is not obvious, and only the velocity separation effect of indivedual chromatographic peak 1.0 ml/min better (scheming not shown), therefore selects column flow rate to be 1.0ml/min.
7, column temperature is investigated
According to HPLC chromatographic condition, 3 kinds of column temperatures (25 DEG C, 30 DEG C, 35 DEG C) are investigated respectively.
Result shows, the impact of column temperature each chromatographic peak component separating effect is not obvious, slightly difference (scheming not shown), and when 30 DEG C, the chromatographic peak separating effect of 50 ~ 60min is micro-good, therefore selects column temperature to be 30 DEG C.
8, finger-print chromatographic condition 2 times of chromatographic peak acquisition times are investigated
After need testing solution sample introduction, the chromatogram of record 200min, investigates and whether goes out peak completely (scheming not shown).
Result shows, under this chromatographic condition, within 100 minutes, does not detect chromatographic peak later.
9, mobile phase blank is investigated
Under HPLC chromatographic condition, sample introduction list working procedure does not investigate the chromatogram of 100 minutes, any chromatographic peak (scheming not shown) do not detected, and result shows that mobile phase is blank and detects without impact finger-print.
10, the investigation of blank solvent impact
Under HPLC chromatographic condition, record blank solvent (70% ethanol water) chromatogram of 100 minutes, any chromatographic peak (scheming not shown) do not detected, result shows that blank solvent detects without impact finger-print.
embodiment 3the detection of licoflavone class material in peace stomach ulcer
1. chromatographic column: model is Agela Venusil MP 5 μm of C
18-100 4.6 × 250mm;
2. mobile phase: take acetonitrile as mobile phase A, with 0.01% trifluoracetic acid (TFA) solution for Mobile phase B, the regulation according to the form below carries out gradient elution;
3. flow velocity: 1.0mL/ minute;
4. determined wavelength: 270nm;
5. column temperature 30 DEG C;
6. the preparation of reference substance solution: extracting Radix Glycyrrhizae chalcone A reference substance is appropriate, adds 70% ethanol water and makes the solution of every 1ml containing 0.8mg, to obtain final product.
7. the preparation of need testing solution: take peace stomach ulcer content 0.1g, put in 25ml measuring bottle, add 70% ethanol 20ml, ultrasonic extraction 5 minutes, take out, let cool, be settled to scale with 70% ethanol, shake up, filter with 0.2 μm of miillpore filter, to obtain final product.
8. determination method: accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, record the chromatogram of 100 minutes.
embodiment 4methodological study
1, precision is investigated
Prepare need testing solution, with reference to the method for embodiment 3, continuous sample introduction 6 times, measure characteristic spectrum, stacking diagram sees Fig. 3, and utilize finger-print software evaluation similarity, result shows, instrument precision is good.
2, study on the stability
Prepare need testing solution, with reference to the method for embodiment 3, respectively close to 0,3.5,7,11,15,24 hour sample introduction, measure characteristic spectrum, stacking diagram sees Fig. 4, adopts finger-print software to calculate its similarity, result shows, measures in 24 hours, and need testing solution is stablized.
3, repeatability is investigated
Parallel preparation 6 parts of need testing solutions, the method with reference to embodiment 3 measures characteristic spectrum, and characteristic spectrum stacking diagram sees Fig. 5, and utilize finger-print software to calculate its similarity, result shows, method repeatability is good.
embodiment 5the foundation of characteristic spectrum common pattern
With reference to the method for embodiment 3, have detected 2008 (4 batches), peace stomach ulcer that 2009 (16 batches) produce." similarity evaluation, the 2004A version " software using pharmacopoeia commission to recommend, utilizes 20 batches to pacify stomach ulcer characteristic spectrum and generates common pattern figure, specifically describe as follows:
1, characteristic spectrum mark: in conjunction with 20 batches of peace stomach ulcer characteristic spectrum characteristics, the total chromatographic peak 15 of mark altogether, as shown in Figure 2; The liquiritin composition chromatographic peak marked in 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 liquiritin composition is defined as non-shared peak, and No. 2 peaks are the acromion containing onocerin composition.
2, characteristic spectrum Similarity Measure: 20 batches of peace stomach ulcers calculate similarity jointly, and the results are shown in Table 1, result shows, the similarity of 20 batches of peace stomach ulcers and common pattern is between 0.929 ~ 0.985, mean value reaches 0.963, and illustrate that between each batch sample, homogeneity is fine, sample is stablized.
20 batches, table 1 peace stomach ulcer similarity result
3, pacify each characteristic peak relative retention time of stomach ulcer characteristic spectrum to calculate
Utilize 20 batches to pacify stomach ulcer characteristic spectrum each chromatographic peak retention time data, be with reference to peak S with licochalcone A, calculate the relative retention time at other 6 characteristic peaks and S peak, show that the average of 20 batch datas formulates relative retention time standard; Result obtains each chromatographic peak with as follows with reference to 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(peak 6), 1.15(peak 7); Consider error between chromatographic column and detecting instrument, tentative check limit be setting ± 5% within.
Claims (3)
1. pacify a method for building up for stomach ulcer finger-print, described method comprises the content adopting high performance liquid chromatography to detect flavone compound in peace stomach ulcer, and described method comprises the steps:
(1) preparation of reference substance solution: extracting Radix Glycyrrhizae chalcone A reference substance, adds 70% ethanol water and makes the solution of every 1ml containing 0.8mg, product solution in contrast;
(2) preparation of need testing solution: extracting Radix Glycyrrhizae extract content 0.1g, puts in 25ml measuring bottle, adds 70% ethanol water 20ml, ultrasonic extraction 5 minutes, take out, let cool, be settled to scale with 70% ethanol water, shake up, filter, as need testing solution with 0.2 μm of miillpore filter;
Wherein, the preparation method of described licorice content is as follows: the glycyrrhiza residue of learning from else's experience after extracting extract of licorice root or glycyrrhizic acid powder, and the ethanol water with more than 93% extracts twice, often all over 1 hour, merge extract and be concentrated into paste, add 2.0% sodium carbonate liquor dissolve, precipitate 24 hours, get supernatant with 10.0% hydrochloric acid be neutralized to pH value 2-3, filter, the washing of sediment purified water is 6 to pH value, and sediment, after 40-50 DEG C of drying, to obtain final product;
And
(3) measure: accurate absorption reference substance solution and each 10 μ l of need testing solution, inject high performance liquid chromatograph, measure according to following chromatographic condition, record the chromatogram of 100 minutes, obtain finger-print:
Chromatographic column: Agela Venusil MP 5 μm
4.6 × 250mm;
Mobile phase: the trifluoroacetic acid aqueous solution of acetonitrile and 0.01% (volume ratio), carries out gradient elution;
Wherein, described gradient elution program arranges by following volume ratio and carries out:
When 0 minute, mobile phase is the trifluoroacetic acid aqueous solution of the acetonitrile of 22% and 0.01% (volume ratio) of 78%;
When 10 minutes, mobile phase is the trifluoroacetic acid aqueous solution of the acetonitrile of 25% and 0.01% (volume ratio) of 75%;
When 15 minutes, mobile phase is the trifluoroacetic acid aqueous solution of the acetonitrile of 30% and 0.01% (volume ratio) of 70%;
When 25 minutes, mobile phase is the trifluoroacetic acid aqueous solution of the acetonitrile of 35% and 0.01% (volume ratio) of 65%;
When 40 minutes, mobile phase is the trifluoroacetic acid aqueous solution of the acetonitrile of 45% and 0.01% (volume ratio) of 55%;
When 80 minutes, mobile phase is the trifluoroacetic acid aqueous solution of the acetonitrile of 60% and 0.01% (volume ratio) of 40%;
When 90 minutes, mobile phase is the trifluoroacetic acid aqueous solution of the acetonitrile of 75% and 0.01% (volume ratio) of 25%;
When 100 minutes, mobile phase is the trifluoroacetic acid aqueous solution of the acetonitrile of 75% and 0.01% (volume ratio) of 25%;
Flow velocity: 1.0mL/min;
Column temperature: 30 DEG C;
UV detect wavelength: 270nm.
2. method according to claim 1, is characterized in that, the finger-print of described foundation comprises 7 characteristic peaks, and the relative retention time of described characteristic peak is respectively:
1:0.52 ± 0.05, peak; 2:0.65 ± 0.05, peak; 3:0.80 ± 0.05, peak; 4:0.93 ± 0.05, peak; S peak: 1.00 ± 0.05; 6:1.07 ± 0.05, peak; 7:1.15 ± 0.05, peak.
3. detect a method for flavone compound in peace stomach ulcer, described method adopts the finger-print of method establishment described in claim 1 or 2 to detect flavone compound in peace stomach ulcer.
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| CN102680629B (en) * | 2012-05-18 | 2014-08-06 | 新疆全安药业有限公司 | Method for establishing Anweiyang capsule fingerprint spectrum |
| 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 |
| CN105004812A (en) * | 2015-07-27 | 2015-10-28 | 合肥伟海讴斯医药科技有限公司 | Method for distinguishing famous-region drug Huangshan gongju and counterfeit drug sunflowers by means of Chinese medicine characteristic chromatogram |
| CN106431877A (en) * | 2016-08-24 | 2017-02-22 | 天津中新药业研究中心 | Method for preparing licochalcone from licorice residues |
| 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 |
| CN110346492A (en) * | 2019-07-24 | 2019-10-18 | 新疆全泰兴药业科技有限公司 | A kind of glycyrrhiza extract fingerprint atlas detection method |
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