CN102841154A - Quality testing method of Ganshao Xiaoke tablets - Google Patents
Quality testing method of Ganshao Xiaoke tablets Download PDFInfo
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Abstract
The invention relates to the field of traditional Chinese medicine detection, in particular to a quality testing method of Ganshao Xiaoke tablets. An HPLC (high performance liquid chromatography) fingerprint method is utilized to detect. The special steps are as follows: 1) after precisely weighing the Ganshao Xiaoke tablet powder, dissolving with methanol or ethanol as a solvent, and carrying out the constant volume to obtain a sample solution; 2) after precisely weighing paeoniflorin, dissolving with methanol as a solvent, and carrying out the constant volume, and obtaining a reference solution; and 3) precisely absorbing a test sample solution or injecting a reference solution into a high performance liquid chromatograph for analysis. The quality testing method of Ganshao Xiaoke tablets provided by the invention is convenient, feasible and good in repeatability, and is capable of comprehensively analyzing the pharmaceutical taste components in an analysis formula, giving out the special fingerprint of the Ganshao Xiaoke tablets for effectively controlling the quality of the Ganshao Xiaoke tablets.
Description
Technical field
The present invention relates to the Chinese medicine detection range, be specifically related to the quench one's thirst quality determining method of sheet of a kind of sweet Chinese herbaceous peony.
Background technology
Traditional Chinese medicine fingerprint is a kind of comprehensive, quantifiable identification of means, and it is to be based upon on the basis of chemical composition of Chinese materia medica systematic study, is mainly used in to estimate Chinese crude drug and the authenticity of Chinese medicine preparation semi-manufactured goods quality, good property and stability.Chinese medicine and preparation thereof are the multi-component complex system; Therefore estimating its quality should adopt and adapt with it; The detection method of enriching authentication information can be provided; Set up kind and quantity that traditional Chinese medicine fingerprint can reflect contained chemical constitution in Chinese medicine and the preparation thereof comparatively all sidedly, and then drug quality is carried out integral body describe and estimate.The research of traditional Chinese medicine fingerprint and foundation, significant for the quality of effective control Chinese crude drug or Chinese patent drug.
The sweet Chinese herbaceous peony sheet of quenching one's thirst is produced without competition by Hehuang Pharmaceutical Co., Ltd., Shanghai, and it is made up of Radix Glycyrrhizae, the root of herbaceous peony two flavor medicinal materials, and beneficial the moon nourishes blood, and is used for the levis diabetes of adult's the moon deficiency of blood disease.Through modern pharmacology research, the application that it can be used to treat the IGR of prediabetes also can be used for can reducing the acarbose spinoff at diabetes Combined application acarbose, strengthens the curative effect of hypoglycemic.The said preparation quality standard is recorded the ministerial standard in the Ministry of Public Health, tentative standard numbering: WS-11389 (ZD1389)-2002.The present sweet Chinese herbaceous peony tablet quality control method of quenching one's thirst is that the thin layer of two control medicinal materials differentiates that the HPLC with a Paeoniflorin measures, and does not control on the homogeneity of product total quality.For reduce product batch with batch between mass discrepancy, control the stability of each composition of its inherence with finger-print, guarantee the stable homogeneous of product.For manufacturer and detection department, press for a kind of method that is directed against the quality monitoring of this medicine.
In order to remedy above-mentioned deficiency; Make that its Quality Control Technology is more perfect, science and a kind of utilizable quality control pattern is provided to its standardization from now on; Need study the quench one's thirst finger-print of sheet of sweet Chinese herbaceous peony; Setting up the finger-print HPLC method of this product, and finally confirm the quench one's thirst standard diagram of sheet of sweet Chinese herbaceous peony, lay the foundation for product quality is controlled better.
Summary of the invention
The objective of the invention is to overcome the defective of prior art, the quality determining method that provides a kind of sweet Chinese herbaceous peony to quench one's thirst sheet can comprehensively be analyzed the flavour of a drug composition in the prescription, provides the sweet Chinese herbaceous peony unique finger-print of sheet of quenching one's thirst, in order to the quench one's thirst quality of sheet of the sweet Chinese herbaceous peony of effective control.
The present invention at first discloses the quench one's thirst quality determining method of sheet of a kind of sweet Chinese herbaceous peony, adopts the HPLC finger print method to detect, and concrete steps are following:
1) get the sweet Chinese herbaceous peony sheet powder of quenching one's thirst, accurate claim fixed and be dissolution with solvents, constant volume with methyl alcohol or ethanol after, need testing solution;
2) get Paeoniflorin, accurate claim fixed and be dissolution with solvents, constant volume with methyl alcohol after, object of reference solution;
3) accurate need testing solution or the object of reference solution injection high performance liquid chromatograph drawn; Adopting reverse-phase chromatographic column to carry out HPLC analyzes; The condition of HPLC finger print method is: 20～30 ℃ of column temperatures, moving phase are acetonitrile-water-phosphoric acid system, gradient elution; Flow velocity is 0.7～1.5ml/mim, and the detection wavelength is 230nm.
The said sweet Chinese herbaceous peony of the step 1) of the present invention sheet powder of quenching one's thirst is to remove sweet Chinese herbaceous peony to quench one's thirst behind the film coating of sheet outside surface inner medicine powder.
More excellent, solvent described in the step 1) is 30～100v/v% methanol aqueous solution or 50v/v% ethanol water; Step 2) solvent described in is the 100v/v% methanol solution.
Optimum, solvent described in the step 1) is the 50v/v% methanol aqueous solution; Step 2) solvent described in is the 100v/v% methanol solution.
More excellent, every milliliter of the said need testing solution of step 1) contains the sweet Chinese herbaceous peony of the 6～10mg sheet powder of quenching one's thirst.
More excellent, every milliliter of the said need testing solution of step 1) contains the sweet Chinese herbaceous peony of the 8mg sheet powder of quenching one's thirst.
More excellent, the said ultrasonic dissolution that is dissolved as of step 1).More excellent, the time of step 1) ultrasonic dissolution is 5～30min.Optimum, the time of step 1) ultrasonic dissolution is 10min.
More excellent, the step 1) need testing solution also need be through 0.22 μ m filtering with microporous membrane.
More excellent, step 2) said object of reference solution contains 0.2～0.6mg Paeoniflorin for every milliliter.
More excellent, step 2) said object of reference solution contains the 0.4mg Paeoniflorin for every milliliter.
More excellent, the said reverse-phase chromatographic column of step 3) is an Agilent ZORBAX SB-C18 chromatographic column.
More excellent, in the said acetonitrile-water of step 3)-phosphoric acid system, mobile phase A is an acetonitrile, Mobile phase B is the 0.05v/v% phosphoric acid solution.
More excellent, the composition of said gradient elution program of step 3) and moving phase is following:
Preferably, accurate need testing solution or the object of reference solution 5～15ul of drawing of step 3), preferred 10ul injects high performance liquid chromatograph, measures.Record 90～100min, preferred 90 minutes chromatogram.
More excellent, said finger-print is as shown in Figure 1, and 8 characteristic peaks are wherein arranged, and the relative retention time of characteristic peak is following: No. 1 peak 0.108; No. 2 peaks 0.378; No. 3 peaks 0.867; No. 4 peaks 1.000; No. 5 peaks 1.174; No. 6 peaks 1.462; No. 7 peaks 1.546; No. 8 peaks 2.987.
More excellent, said finger-print is as shown in Figure 1, and 8 characteristic peaks are wherein arranged, and the characteristic peak relative peak area is following: No. 1 peak 0.437; No. 2 peaks 1.119; No. 3 peaks 0.391; No. 4 peaks 1.000; No. 5 peaks 0.190; No. 6 peaks 0.155; No. 7 peaks 0.392; No. 8 peaks 0.364.
The sweet Chinese herbaceous peony of the present invention sheet high-efficiency liquid-phase fingerprint of quenching one's thirst has 8 characteristic peaks, is that reference peak calculates relative retention time and relative peak area with No. 4 peaks (Paeoniflorin peak).
The quench one's thirst quality inspection standard of sheet of the sweet Chinese herbaceous peony of the present invention is: product to be tested through the HPLC finger print method obtain finger-print should (contain 8 characteristic peaks, the relative retention time of characteristic peak be: 1.546, No. 8 peaks 2.987,1.462, No. 7 peaks, 1.174, No. 6 peaks, 1.000, No. 5 peaks, 0.867, No. 4 peaks, 0.378, No. 3 peaks, 0.108, No. 2 peaks, No. 1 peak with finger-print shown in Figure 1; The characteristic peak relative peak area is: 0.392, No. 8 peaks 0.364,0.155, No. 7 peaks, 0.190, No. 6 peaks, 1.000, No. 5 peaks, 0.391, No. 4 peaks, 1.119, No. 3 peaks, 0.437, No. 2 peaks, No. 1 peak) good similarity is arranged, similarity reaches more than 0.8.
Second aspect present invention discloses aforementioned sweet Chinese herbaceous peony and has quenched one's thirst the quality determining method of sheet in the application of tablet quality in detecting of quenching one's thirst of sweet Chinese herbaceous peony.
The quench one's thirst quality determining method of sheet of sweet Chinese herbaceous peony of the present invention has been filled up the sweet Chinese herbaceous peony blank that tablet quality detects of quenching one's thirst; Make more easy, the easy row of its detection method, good reproducibility; Detect the quench one's thirst quality of sheet of sweet Chinese herbaceous peony through the HPLC finger-print; Be more conducive to its quality control, help to improve the security and the stability of medicament.
Description of drawings
Fig. 1: the sweet Chinese herbaceous peony sheet finger-print of quenching one's thirst
Fig. 2: different the quench one's thirst HPLC chromatograms (230nm) of sheet of sweet Chinese herbaceous peony under the wavelength that detect
Fig. 3: different the quench one's thirst HPLC chromatograms (254nm) of sheet of sweet Chinese herbaceous peony under the wavelength that detect
Fig. 4: different the quench one's thirst HPLC chromatograms (263nm) of sheet of sweet Chinese herbaceous peony under the wavelength that detect
Fig. 5: the quench one's thirst HPLC chromatogram (50% methyl alcohol) of sheet of the different sweet Chinese herbaceous peonies that extract the solvents preparation
Fig. 6: the quench one's thirst HPLC chromatogram (50% ethanol) of sheet of the different sweet Chinese herbaceous peonies that extract the solvents preparation
Fig. 7: the quench one's thirst HPLC chromatogram (30% methyl alcohol) of sheet of the different sweet Chinese herbaceous peonies that extract the solvents preparation
Fig. 8: the quench one's thirst HPLC chromatogram (70% methyl alcohol) of sheet of the different sweet Chinese herbaceous peonies that extract the solvents preparation
Fig. 9: the quench one's thirst HPLC chromatogram (100% methyl alcohol) of sheet of the different sweet Chinese herbaceous peonies that extract the solvents preparation
Figure 10: the quench one's thirst selection of sheet sample ultrasonic time of sweet Chinese herbaceous peony
Figure 11: the HPLC chromatogram of epicatechin, Paeoniflorin, liquiritin, ammonium glycyrrhetate mixing reference substance
Figure 12: the finger-print of root of herbaceous peony extract
Figure 13: the finger-print of licorice extract
Figure 14: the quench one's thirst finger-print of sheet sample of ten sweet Chinese herbaceous peonies of lot number
Embodiment
Further set forth the present invention below in conjunction with embodiment.Should be understood that embodiment only is used to explain the present invention, and unrestricted scope of the present invention.
The quench one's thirst preparation of sheet of embodiment 1 sweet Chinese herbaceous peony
1. material
Radix Glycyrrhizae: these article are the dry root and rhizome of glycyrrhizic legume Glycyrrhiza uralensis Fisch., glycyrrhiza inflate bat Glycyrrhiza inflata Bat. or glycyrrhiza glabra Glycyrrhiza glabra L..
The root of herbaceous peony: these article are the dry root of ranunculaceae plant Chinese herbaceous peony Paeonia lacti flora Pall..
2. preparation method
Extracting liquorice 400g, root of herbaceous peony 2000g, by 6.5 water extraordinarily of inventory, heating decocted 2 hours, emitted decoction liquor, filtered; Concentrate, add water by 4 times of amounts of inventory again in the dregs of a decoction, heating decocted 1.5 hours, emitted decoction liquor; Filter, concentrate, merge concentrate, be concentrated into more than the relative density 1.13-1.20 (50-70 ℃); Add 95% ethanol, make medicinal extract contain alcohol amount and reach 50%, stir, leave standstill and be no less than 12 hours; Filter, filtrate recycling ethanol is concentrated into the thick paste that does not have the alcohol flavor, and drying under reduced pressure becomes dry extract.
Extract powder 160g, microcrystalline cellulose 32g, talcum powder 32g, lime carbonate 56g, dolomol (particle weight 1%).The dried particle that obtains with one-step palletizing sieves whole grain with 14 wood.Dried particle through arrangement adds dolomol by 1% of particle weight, puts to mix in the mixing tank to get final product in 10 minutes.With the flat fat punch die of 9.5mm, plain sheet sheet is heavily by per 1 heavy 0.27g ± 5% control.Plain sheet hardness is not less than the 3.5kg. dressing and adopts Xin Feier, gets 1 part of coating agent and mixes stirring with 6 parts of pure water more than 40 minutes; The coating agent consumption is controlled at the 6-6.25% of plain sheet weight; The finished product sheet weighs 0.28 ± 5% behind the dressing.
Embodiment 2HPLC detects and finger-print
1. instrument and reagent
Instrument: Agilent 1100 type high performance liquid chromatographs, quaternary pump, full-automatic sample introduction appearance; PDAD (DAD); Chromatographic column: Agilent ZORBAX SB-C18 Stable BondAnalytical 4.6*150mm 5-Micron.
Reagent: epicatechin standard items (lot number: 110878); Paeoniflorin standard items (lot number: 110736); Liquiritin standard items (lot number: 111610-200604); Ammonium glycyrrhetate standard items (lot number: 110731-200614); 4 reference substances are all available from Nat'l Pharmaceutical & Biological Products Control Institute; Acetonitrile is a chromatographically pure; Water is double distilled water; It is pure that all the other reagent are analysis; The sweet Chinese herbaceous peony sheet of quenching one's thirst, available from the xanthate industry, lot number is: 110601,110602,110603,111201,111202,120510,120515,120620,120622,120625; The sample lot number of experimental methodology research is 111202.
2. experimental technique
2.1 the preparation of sample solution
1) preparation of need testing solution: remove except that the sweet Chinese herbaceous peony of the film-coating sheet powder 0.2g that quenches one's thirst, accurately claim surely, put in the tool plug 25ml volumetric flask; It is an amount of to add 50% methyl alcohol; Ultrasonic Extraction 10min adds 50% methanol constant volume to scale after the cooling, with 0.22 μ m filtering with microporous membrane; Get subsequent filtrate as need testing solution, promptly get.
2) preparation of object of reference solution: get the about 10mg of Paeoniflorin standard items, place the 25ml volumetric flask, add 100% dissolve with methanol and be diluted to scale, promptly get.
3) mix the preparation of contrast solution: it is an amount of to get epicatechin, Paeoniflorin, liquiritin, ammonium glycyrrhetate reference substance; Add 100% methyl alcohol ultrasonic dissolution, process the mixing reference substance that every 1ml contains epicatechin 0.059mg, Paeoniflorin 0.200mg, liquiritin 0.150mg, ammonium glycyrrhetate 0.150mg.
2.2 chromatographic condition
Chromatographic column: Agilent ZORBAX SB-C18 Stable Bond Analytical 4.6*150mm 5-Micron; The detection wavelength is 230nm; Column temperature is 25 ℃; Elution flow rate and eluent gradient such as following table 1, the map record time is 90min.Reference substance Paeoniflorin retention time 24.091min under this condition, theoretical cam curve is not less than 30000 in Paeoniflorin.
Table 1 acetonitrile-0.05v/v% phosphoric acid solution gradient elution table
2.2.1 confirming of moving phase
4 kinds of flow phase system have been selected in the experimentation: 1. methanol-water (22:78) fixed mixing ratio; 2. the gradient elution of methanol-water; 3. acetonitrile-0.5% phosphoric acid gradient elution; 4. acetonitrile-0.05% phosphoric acid gradient elution.
The result shows that with acetonitrile-0.05% phosphoric acid system, condition of gradient elution promptly as shown in table 1 is best; The degree of separation of each chromatographic peak is better on the spectrogram; Chromatographic peak is many, and retention time is moderate, so select acetonitrile-water-phosphoric acid system to detect moving phase as the quench one's thirst HPLC finger-print of sheet of sweet Chinese herbaceous peony.
2.2.2 detect the selection of wavelength
Adopt PDAD; Choose principal ingredient Paeoniflorin maximum absorption wavelength 230nm and the root of herbaceous peony in the said preparation, Radix Glycyrrhizae two flavor medicinal materials detection wavelength 254nm, 263nm commonly used carries out chromatogram relatively, under the 230nm wavelength testing conditions, the chromatographic peak separation case is good; Each component all has bigger absorption; Response sample chemical constitution information that can be more, and 254nm, 263nm detection collection of illustrative plates down, the sample peak lacks more.So preferred 230nm is the different sample HPLC chromatograms that detect under the wavelength of the check and analysis condition of sample finger-print, sees Fig. 2-4.
2.3 extract the investigation of solvent
Remove the quench one's thirst outer dressing of sheet of sweet Chinese herbaceous peony, accurate quench one's thirst 5 parts in the inner powder of sheet of fixed sweet Chinese herbaceous peony of claiming, every part of 0.2g puts respectively in the tool plug 25ml volumetric flask; Use an amount of 100% methyl alcohol, 70% methyl alcohol, 50% methyl alcohol, 30% methyl alcohol, five kinds of solvents of 50% ethanol (WS of organic solvent) to carry out ultrasonic Extraction 10min respectively to above-mentioned 5 minutes powder; The cooling back is settled to scale with identical solvent; With 0.22 μ m filtering with microporous membrane, the filtrating that obtains the different solvents extraction is as need testing solution.
The quench one's thirst HPLC chromatic graph spectrum of sheet sample of the different sweet Chinese herbaceous peonies that extract the solvents preparation is seen Figure of description 5-9; Can know by HPLC result, after the above-mentioned solvent extraction, all can obtain the correct HPLC collection of illustrative plates that separates; Wherein, chromatographic peak separates preferably in the 50% methanol extract liquid chromatogram, and the Paeoniflorin chromatographic peak area of equivalent sample is maximum; So select for use 50% methyl alcohol as the specimen preparation preferred solvent.
2.4 the investigation of extracting mode
Get quench one's thirst 5 parts in sheet powder of glycosides Chinese herbaceous peony; Every part of 0.2g, the accurate title, decide, and puts in the tool plug 25ml volumetric flask; Adopt 50% methyl alcohol the sweet Chinese herbaceous peony sheet ultrasonic Extraction of quenching one's thirst to be dissolved as solvent; Check sonicated 5min, 10min, 15min, 20min, 30min to the quench one's thirst extraction effect of sheet of sweet Chinese herbaceous peony, the cooling of ultrasonic back, constant volume, sample introduction analysis behind the 0.22 μ m filtering with microporous membrane respectively.
With the ultrasonic Extraction time be horizontal ordinate; With the Paeoniflorin peak area is ordinate, investigates the relation of extraction time and extraction efficiency, and experimental result is seen Figure of description 10; The result show when extraction time greater than 10min; Extraction time reduces the influence that extraction efficiency produces, and considers the quick, easy of experiment, so the sample extraction ultrasonic time is decided to be 10min.
2.5 methodological study
Prepare the quench one's thirst sample of sheet of sweet Chinese herbaceous peony and carry out the preliminary experiment of finger-print, by above-mentioned chromatographic condition (remove except that the sweet Chinese herbaceous peony of the film-coating sheet powder 0.2g that quenches one's thirst, accurate claim fixed; Put in the tool plug 25ml volumetric flask, it is an amount of to add 50% methyl alcohol, ultrasonic Extraction 10min; Add 50% methanol constant volume after the cooling to scale; With 0.22 μ m filtering with microporous membrane, get filtrating as need testing solution), can obtain degree of separation better, the finger-print of each peak distribution uniform; And reselection procedure peak area still can 8 peaks, carry out methodological investigation.
2.5.1 precision experiment
Get need testing solution, according to above-mentioned chromatographic condition, continuous sample introduction 6 times, record chromatogram.The result shows that the relative retention time at each total peak and relative peak area ratio basically identical, the RSD of each peak retention time ratio are 0.00% ~ 0.46%, and the RSD of peak area ratio is 0.20% ~ 2.83%, and RSD meets the fingerprint pattern technology requirement all less than 3%.The result shows that the precision of whole detection system such as instrument is good.
2.5.2 stability experiment
Get need testing solution, according to above-mentioned chromatographic condition, respectively at 0,2,4,6,8,22,24h detects the record chromatogram.The result shows, sample in 24h, the relative retention time at each total peak and relative peak area ratio basically identical, the RSD of each peak relative retention time ratio is 0.09% ~ 0.47%; The RSD of each peak relative area ratio is 0.28% ~ 2.81%; RSD meets the technical requirement of finger-print all less than 3%.The result shows that finger-print is stable in the test sample 24h.
2.5.3 repeated experiment
Precision takes by weighing same lot number (lot number: 111202) sample is 6 parts, and the preparation method prepares need testing solution by need testing solution, sample introduction respectively, record chromatogram respectively.The result shows, the relative retention time at each total peak and relative peak area ratio basically identical, and the RSD of the relative retention time ratio at each total peak is 0.05% ~ 0.42%; The RSD of the relative peak area ratio at each total peak is 0.39% ~ 2.73%; RSD meets the technical requirement of finger-print all less than 3%.
2.6 finger-print and technical parameter
2.6.1 medicine
Lot number is 110601,110602,110603,111201,111202,120510,120515,120620,120622,120625 the sweet Chinese herbaceous peony sheet of quenching one's thirst.
2.6.2 mixing contrast solution: it is an amount of to get epicatechin, Paeoniflorin, liquiritin, ammonium glycyrrhetate reference substance; Add the methyl alcohol ultrasonic dissolution; Process the mixing reference substance that every 1ml contains epicatechin 0.059mg, Paeoniflorin 0.200mg, liquiritin 0.150mg, ammonium glycyrrhetate 0.150mg, carry out HPLC according to the elution program of table 1 and analyze.
2.6.2 herbal extract
1) white Peony Root extract: the root of herbaceous peony (dry root of ranunculaceae plant Chinese herbaceous peony Paeonia lacti flora Pall.) is an amount of, boiling 2 times, 2 hours for the first time; The 2nd time 1.5 hours, collecting decoction filtered; Filtrate decompression is concentrated into thick paste; Get that to add 50% methyl alcohol in right amount ultrasonic,, get subsequent filtrate as need testing solution with 0.22 μ m filtering with microporous membrane.
2) licorice medicinal materials extract: Radix Glycyrrhizae (glycyrrhizic legume Glycyrrhiza uralensis Fisch.) is an amount of, boiling 2 times, 2 hours for the first time; The 2nd time 1.5 hours, collecting decoction filtered; Filtrate decompression is concentrated into thick paste; Get that to add 50% methyl alcohol in right amount ultrasonic,, get subsequent filtrate as need testing solution with 0.22 μ m filtering with microporous membrane
Get 10 lot numbers and be 110601,110602,110603,111201,111202,120510,120515,120620,120622,120625 sample; Preparation method by need testing solution prepares sample solution; Measure in accordance with the law; With 10 batches of test sample finger-prints serves as that the basis obtains " common pattern " as reference fingerprint, sees Fig. 1; Mainly contain 8 total peaks.
Sweet Chinese herbaceous peony is quenched one's thirst, and Paeoniflorin is its principal ingredient in the sheet, from finger-print, can find out i.e. No. 4 peaks (RT ≌ 24.091min), Paeoniflorin peak, and integral area is big and be main effective component, so be elected to be to reference to the peak; In addition, No. 3 peaks (RT ≌ 20.876min) are epicatechin in the sample finger-print, and No. 5 peaks (RT ≌ 35.214min) are that liquiritin, No. 7 peaks (RT ≌ 71.952min) are ammonium glycyrrhetate.
With No. 4 peaks is with reference to the peak, and each average relative retention time in total peak (peak number) is followed successively by 0.108 (1), 0.378 (2), 0.867 (3), 1.000 (4S), 1.174 (5), 1.462 (6), 1.546 (7), 2.987 (8).
From the finger-print of the root of herbaceous peony, licorice medicinal materials extract, can confirm that 1,2,3,4, No. 5 peak is from white Peony Root;
6,7, No. 8 peaks are from licorice medicinal materials.
2.6.4 finger-print
The sweet Chinese herbaceous peony sheet finger-print of quenching one's thirst is seen Fig. 1; Epicatechin, Paeoniflorin, liquiritin, ammonium glycyrrhetate mixing reference substance collection of illustrative plates are seen Figure 11; The finger-print of white Peony Root extract is seen Figure 12; The finger-print of licorice medicinal materials extract is seen Figure 13.
2.6.5 finger-print similarity
With the reference fingerprint is reference, through " traditional Chinese medicine fingerprint similarity evaluation software--2009 editions " 10 lot number sample similarities of calculating.
The similarity of table 2 sample
The similarity of 10 lot number samples is seen table 2, can know that by table 2 the sweet Chinese herbaceous peony of 10 lot numbers quenches one's thirst the similarity of sheet between 0.884-0.965, and higher consistance is arranged between each batch sample; The finger-print spectrogram of 10 lot number samples is seen Figure 14.
Claims (10)
1. the sweet Chinese herbaceous peony quality determining method of sheet of quenching one's thirst adopts the HPLC finger print method to detect, and concrete steps are following:
1) get the sweet Chinese herbaceous peony sheet powder of quenching one's thirst, accurate claim fixed and be dissolution with solvents, constant volume with methyl alcohol or ethanol after, need testing solution;
2) get Paeoniflorin, accurate claim fixed and be dissolution with solvents, constant volume with methyl alcohol after, object of reference solution;
3) accurate need testing solution or the object of reference solution injection high performance liquid chromatograph drawn; Adopting reverse-phase chromatographic column to carry out HPLC analyzes; The condition of HPLC finger print method is: 20～30 ℃ of column temperatures, moving phase are acetonitrile-water-phosphoric acid system, gradient elution; Flow velocity is 0.7～1.5ml/mim, and the detection wavelength is 230nm.
2. detection method as claimed in claim 1 is characterized in that, solvent described in the step 1) is 30～100v/v% methanol aqueous solution or 50v/v% ethanol water; Step 2) solvent described in is the 100v/v% methanol solution.
3. detection method as claimed in claim 1 is characterized in that, every milliliter of the said need testing solution of step 1) contains the sweet Chinese herbaceous peony of the 6～10mg sheet powder of quenching one's thirst.
4. detection method as claimed in claim 1 is characterized in that, the said ultrasonic dissolution that is dissolved as of step 1), and the time of ultrasonic dissolution is 5～30min.
5. detection method as claimed in claim 1 is characterized in that step 2) said object of reference solution contains 0.2～0.6mg Paeoniflorin for every milliliter.
6. detection method as claimed in claim 1 is characterized in that, the said reverse-phase chromatographic column of step 3) is an Agilent ZORBAXSB-C18 chromatographic column.
7. detection method as claimed in claim 1 is characterized in that, the said acetonitrile-water of step 3)-phosphoric acid system comprises mobile phase A and Mobile phase B, and wherein mobile phase A is an acetonitrile, and Mobile phase B is the 0.05v/v% phosphoric acid solution.
8. detection method as claimed in claim 1 is characterized in that, the composition of said gradient elution program of step 3) and moving phase is following:
9. detection method as claimed in claim 1; It is characterized in that; 8 characteristic peaks are arranged in the said finger-print, and the relative retention time of characteristic peak is following: 1.546, No. 8 peaks 2.987,1.462, No. 7 peaks, 1.174, No. 6 peaks, 1.000, No. 5 peaks, 0.867, No. 4 peaks, 0.378, No. 3 peaks, 0.108, No. 2 peaks, No. 1 peak; The characteristic peak relative peak area is following: 0.392, No. 8 peaks 0.364,0.155, No. 7 peaks, 0.190, No. 6 peaks, 1.000, No. 5 peaks, 0.391, No. 4 peaks, 1.119, No. 3 peaks, 0.437, No. 2 peaks, No. 1 peak.
10. the said sweet Chinese herbaceous peony of the arbitrary claim of claim 1-9 is quenched one's thirst the quality determining method of sheet in the application of tablet quality in detecting of quenching one's thirst of sweet Chinese herbaceous peony.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107941967A (en) * | 2018-01-10 | 2018-04-20 | 广西壮族自治区食品药品检验所 | The fingerprint atlas detection method of Xiao Ke Lin piece and Xiaokelin capsule for diabetes |
| CN109917044A (en) * | 2019-04-10 | 2019-06-21 | 成都中医药大学 | The detection method of Guizhi-Shoyao-Zhimu Decoction |
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| CN101008633A (en) * | 2006-01-26 | 2007-08-01 | 黑龙江中医药大学 | Fingerprint of Sinisan decoction and establishing method therefor |
| CN101991661A (en) * | 2009-08-19 | 2011-03-30 | 中国药品生物制品检定所 | Method for detecting Chinese patent drug containing at least two of white paeony root, ginseng, salvia miltiorrhiza, sweet wormwood, liquorice and angelica sinensis |
| CN102539553A (en) * | 2011-12-15 | 2012-07-04 | 石家庄东方药业有限公司 | Method for establishing fingerprint spectrum of liver-enhancing medicine |
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| CN101008633A (en) * | 2006-01-26 | 2007-08-01 | 黑龙江中医药大学 | Fingerprint of Sinisan decoction and establishing method therefor |
| CN101991661A (en) * | 2009-08-19 | 2011-03-30 | 中国药品生物制品检定所 | Method for detecting Chinese patent drug containing at least two of white paeony root, ginseng, salvia miltiorrhiza, sweet wormwood, liquorice and angelica sinensis |
| CN102539553A (en) * | 2011-12-15 | 2012-07-04 | 石家庄东方药业有限公司 | Method for establishing fingerprint spectrum of liver-enhancing medicine |
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| 李越峰等: "四逆散指纹图谱相似度的分析研究", 《时珍国医国药》, vol. 22, no. 5, 20 May 2011 (2011-05-20) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107941967A (en) * | 2018-01-10 | 2018-04-20 | 广西壮族自治区食品药品检验所 | The fingerprint atlas detection method of Xiao Ke Lin piece and Xiaokelin capsule for diabetes |
| CN107941967B (en) * | 2018-01-10 | 2020-08-04 | 广西壮族自治区食品药品检验所 | Fingerprint detection method of xiaokeling tablets and xiaokeling capsules |
| CN109917044A (en) * | 2019-04-10 | 2019-06-21 | 成都中医药大学 | The detection method of Guizhi-Shoyao-Zhimu Decoction |
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| CN102841154B (en) | 2014-03-26 |
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