CN102841154B - Quality testing method of Ganshao Xiaoke tablets - Google Patents
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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 Chinese medicine detection field, be specifically related to a kind of quality determining method of sweet Chinese herbaceous peony Xiaoke Tablets.
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 evaluating authenticity, Optimality and the stability of Chinese crude drug and Chinese medicine preparation semi-manufactured goods quality.Chinese medicine and preparation thereof are multi-component complex system, therefore evaluating 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 composition in Chinese medicine and preparation thereof comparatively all sidedly, and then drug quality is carried out to integral body and describe and evaluate.The research of traditional Chinese medicine fingerprint and foundation, significant for the quality of effective control Chinese crude drug or Chinese patent drug.
Sweet Chinese herbaceous peony Xiaoke Tablets, is produced without competition by Hehuang Pharmaceutical Co., Ltd., Shanghai, and it is comprised of Radix Glycyrrhizae, the root of herbaceous peony two taste medicinal materials, and beneficial the moon nourishes blood, for the levis diabetes of the cloudy deficiency of blood disease of adult.Through modern pharmacology research, it can be used for the treatment of the application of the IGR of prediabetes, also can reduce acarbose spinoff at diabetes use in conjunction acarbose, strengthens the curative effect of hypoglycemic.Said preparation quality standard is recorded the ministerial standard in the Ministry of Public Health, tentative standard numbering: WS-11389(ZD1389)-2002.The thin layer that current sweet Chinese herbaceous peony Xiaoke Tablets method of quality control is two control medicinal materials is differentiated and the HPLC of a Paeoniflorin measures, and in the homogeneity of product total quality, does not control.In order to reduce the mass discrepancy between batches of product, with finger-print, control the stability of each composition of its inherence, guarantee the stable homogeneous of product.For manufacturer and detection department, in the urgent need to a kind of method of the quality monitoring for this medicine.
In order to make up above-mentioned deficiency, make that its Quality Control Technology is more perfect, science provide a kind of utilizable quality control model to its standardization from now on, need to study the finger-print of sweet Chinese herbaceous peony Xiaoke Tablets, to set up the finger-print HPLC method of this product, and finally determine and the standard diagram of sweet Chinese herbaceous peony Xiaoke Tablets lay the foundation for product quality is controlled better.
Summary of the invention
The object of the invention is to overcome the defect of prior art, a kind of quality determining method of sweet Chinese herbaceous peony Xiaoke Tablets is provided, can comprehensively analyze the flavour of a drug composition in prescription, provide the finger-print of sweet Chinese herbaceous peony Xiaoke Tablets uniqueness, in order to the quality of the sweet Chinese herbaceous peony Xiaoke Tablets of effective control.
First the present invention discloses a kind of quality determining method of sweet Chinese herbaceous peony Xiaoke Tablets, adopts HPLC finger print method to detect, and concrete steps are as follows:
1) get sweet Chinese herbaceous peony Xiaoke Tablets powder, accurately weighed and take methyl alcohol or ethanol after dissolution with solvents, constant volume, obtain need testing solution;
2) get Paeoniflorin, accurately weighed and take methyl alcohol after dissolution with solvents, constant volume, obtain object of reference solution;
3) accurate need testing solution or the object of reference solution injection high performance liquid chromatograph drawn, adopt reverse-phase chromatographic column to carry out HPLC analysis, the condition of HPLC finger print method is: 20～30 ℃ of column temperatures, mobile phase is acetonitrile-water-phosphoric acid system, gradient elution, flow velocity is 0.7～1.5ml/mim, and detection wavelength is 230nm.
Described in step 1) of the present invention, sweet Chinese herbaceous peony Xiaoke Tablets powder is to remove after the film coating of sweet Chinese herbaceous peony Xiaoke Tablets outside surface, inner medicine powder.
Preferably, solvent described in step 1) is 30～100v/v% methanol aqueous solution or 50v/v% ethanol water; Step 2) solvent described in is 100v/v% methanol solution.
Optimum, solvent described in step 1) is 50v/v% methanol aqueous solution; Step 2) solvent described in is 100v/v% methanol solution.
Preferably, described in step 1) every milliliter of need testing solution containing the sweet Chinese herbaceous peony Xiaoke Tablets of 6～10mg powder.
More excellent, every milliliter of need testing solution is containing the sweet Chinese herbaceous peony Xiaoke Tablets of 8mg powder described in step 1).
Preferably, described in step 1), be dissolved as ultrasonic dissolution.More excellent, the time of step 1) ultrasonic dissolution is 5～30min.Optimum, the time of step 1) ultrasonic dissolution is 10min.
Preferably, step 1) need testing solution also needs through 0.22 μ m filtering with microporous membrane.
Preferably, step 2) every milliliter of described object of reference solution is containing 0.2～0.6mg Paeoniflorin.
More excellent, step 2) every milliliter of described object of reference solution is containing 0.4mg Paeoniflorin.
Preferably, described in step 3), reverse-phase chromatographic column is Agilent ZORBAX SB-C18 chromatographic column.
Preferably, in acetonitrile-water-phosphoric acid system, mobile phase A is acetonitrile described in step 3), and Mobile phase B is 0.05v/v% phosphoric acid solution.
More excellent, gradient elution program and mobile phase is composed as follows described in step 3):
Preferably, accurate need testing solution or the object of reference solution 5～15ul of drawing of step 3), preferably 10ul injects high performance liquid chromatograph, measures.Record 90～100min, the preferably chromatogram of 90 minutes.
Preferably, described finger-print as shown in Figure 1, wherein has 8 characteristic peaks, and the relative retention time of characteristic peak is as follows: 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.
Preferably, described finger-print as shown in Figure 1, wherein has 8 characteristic peaks, and characteristic peak relative peak area is as follows: 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 Xiaoke Tablets of the present invention high-efficiency liquid-phase fingerprint has 8 characteristic peaks, take No. 4 peaks (Paeoniflorin peak) as reference peak calculating relative retention time and relative peak area.
The quality inspection standard of the sweet Chinese herbaceous peony Xiaoke Tablets of the present invention is: the finger-print that product to be tested obtains by HPLC finger print method should (containing 8 characteristic peaks, the relative retention time of characteristic peak be: peak 2.987, No. 1.546,8, peak, No. 1.462,7, peak, No. 1.174,6, peak, No. 1.000,5, peak, No. 0.867,4, peak, No. 0.378,3, peak, No. 1 No. 0.108,2, peak with the finger-print shown in Fig. 1; Characteristic peak relative peak area is: peak 0.364, No. 0.392,8, peak, No. 0.155,7, peak, No. 0.190,6, peak, No. 1.000,5, peak, No. 0.391,4, peak, No. 1.119,3, peak, No. 1 No. 0.437,2, peak) have good similarity, similarity reaches more than 0.8.
The application of the quality determining method that second aspect present invention discloses aforementioned sweet Chinese herbaceous peony Xiaoke Tablets in the quality testing of sweet Chinese herbaceous peony Xiaoke Tablets.
The quality determining method of sweet Chinese herbaceous peony Xiaoke Tablets of the present invention has been filled up the blank of sweet Chinese herbaceous peony Xiaoke Tablets quality testing, make more easy, the easy row of its detection method, reproducible, by HPLC finger-print, detect the quality of sweet Chinese herbaceous peony Xiaoke Tablets, be more conducive to its quality control, contribute to improve the safety and stability of medicament.
Accompanying drawing explanation
Fig. 1: sweet Chinese herbaceous peony Xiaoke Tablets finger-print
Fig. 2: the different HPLC chromatograms (230nm) that detect sweet Chinese herbaceous peony Xiaoke Tablets under wavelength
Fig. 3: the different HPLC chromatograms (254nm) that detect sweet Chinese herbaceous peony Xiaoke Tablets under wavelength
Fig. 4: the different HPLC chromatograms (263nm) that detect sweet Chinese herbaceous peony Xiaoke Tablets under wavelength
Fig. 5: the HPLC chromatogram of sweet Chinese herbaceous peony Xiaoke Tablets prepared by different solvents (50% methyl alcohol)
Fig. 6: the HPLC chromatogram of sweet Chinese herbaceous peony Xiaoke Tablets prepared by different solvents (50% ethanol)
Fig. 7: the HPLC chromatogram of sweet Chinese herbaceous peony Xiaoke Tablets prepared by different solvents (30% methyl alcohol)
Fig. 8: the HPLC chromatogram of sweet Chinese herbaceous peony Xiaoke Tablets prepared by different solvents (70% methyl alcohol)
Fig. 9: the HPLC chromatogram of sweet Chinese herbaceous peony Xiaoke Tablets prepared by different solvents (100% methyl alcohol)
Figure 10: the selection of sweet Chinese herbaceous peony Xiaoke Tablets sample ultrasonic time
Figure 11: the HPLC chromatogram of epicatechin, Paeoniflorin, liquiritin, ammonium glycyrrhetate mixing reference substance
Figure 12: the finger-print of white paeony root extract
Figure 13: the finger-print of licorice extract
Figure 14: the finger-print of ten the sweet Chinese herbaceous peony Xiaoke Tablets of lot number samples
Embodiment
Below in conjunction with embodiment, further set forth the present invention.Should be understood that embodiment is only for the present invention is described, but not limit the scope of the invention.
The preparation of the sweet Chinese herbaceous peony Xiaoke Tablets of embodiment 1
1. material
Radix Glycyrrhizae: this product is 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: this product is the dry root of ranunculaceae plant Chinese herbaceous peony Paeonia lacti flora Pall..
2. preparation method
Extracting Radix Glycyrrhizae 400g, root of herbaceous peony 2000g, by 6.5 water extraordinarily of inventory, heating decocts 2 hours, emit decoction liquor, filter, concentrated, in the dregs of a decoction, 4 times of amounts by inventory add water again, heating decocts 1.5 hours, emit decoction liquor, filter, concentrated, merge concentrate, be concentrated into relative density 1.13-1.20(50-70 ℃) more than, add 95% ethanol, make medicinal extract contain alcohol amount and reach 50%, stir evenly, standingly be no less than 12 hours, filter filtrate recycling ethanol, be concentrated into the thick paste without alcohol taste, drying under reduced pressure becomes dry extract.
Extract powder 160g, microcrystalline cellulose 32g, talcum powder 32g, calcium carbonate 56g, dolomol (particle weight 1%).The whole grain of 14 wood sieve for the dry particle obtaining with one-step palletizing.By the dry particle arranging, by 1% of particle weight, add dolomol, put in mixing tank and mix 10 minutes.With the flat fat punch die of 9.5mm, plain sheet sheet is heavily controlled by every 1 heavy 0.27g ± 5%.Element sheet hardness is not less than 3.5kg. dressing and adopts Xin Feier, gets 1 part of coating agent and 6 parts of pure water mix and blends more than 40 minutes; Coating agent consumption is controlled at the 6-6.25% of plain sheet weight; After dressing, finished product sheet weighs 0.28 ± 5%.
Embodiment 2HPLC detects and finger-print
1. instrument and reagent
Instrument: Agilent 1100 type high performance liquid chromatographs, quaternary pump, full-automatic sample introduction instrument; Diode array detector (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 purchased from Nat'l Pharmaceutical & Biological Products Control Institute; Acetonitrile is chromatographically pure; Water is double distilled water; It is pure that all the other reagent are analysis; Sweet Chinese herbaceous peony Xiaoke Tablets, purchased from 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
The preparation of 2.1 sample solutions
1) preparation of need testing solution: remove the sweet Chinese herbaceous peony Xiaoke Tablets powder 0.2g except film-coating, accurately weighed, put in tool plug 25ml volumetric flask, add 50% methyl alcohol appropriate, ultrasonic extraction 10min, adds 50% methanol constant volume to scale after cooling, with 0.22 μ m filtering with microporous membrane, get subsequent filtrate as need testing solution, obtain.
2) preparation of object of reference solution: get the about 10mg of Paeoniflorin standard items, be placed in 25ml volumetric flask, add 100% methyl alcohol dissolved dilution to scale, obtain.
3) mix the preparation of contrast solution: get epicatechin, Paeoniflorin, liquiritin, ammonium glycyrrhetate reference substance appropriate, add 100% methyl alcohol ultrasonic dissolution, make every 1ml containing the mixing reference substance of 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; Detection wavelength is 230nm; Column temperature is 25 ℃; Elution flow rate and eluent gradient are as following table 1, and 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 determining of mobile phase
4 kinds of flow phase system in experimentation, have been selected: 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.
Result shows, with acetonitrile-0.05% phosphoric acid system, condition of gradient elution as shown in table 1 is best, on spectrogram, the degree of separation of each chromatographic peak is better, chromatographic peak is many, and retention time is moderate, therefore select acetonitrile-water-phosphoric acid system to detect mobile phase as the HPLC finger-print of sweet Chinese herbaceous peony Xiaoke Tablets.
2.2.2 detect the selection of wavelength
Adopt diode array detector, choose principal ingredient Paeoniflorin maximum absorption wavelength 230nm and the root of herbaceous peony in said preparation, detection wavelength 254nm, 263nm that Radix Glycyrrhizae two taste medicinal materials are conventional carry out chromatogram comparison, under 230nm wavelength testing conditions, chromatographic peak separation case is good, each component all has larger absorption, response sample chemical composition information that can be more, and detection collection of illustrative plates under 254nm, 263nm, sample peak disappearance is more.Therefore preferably 230nm is the different sample HPLC chromatograms that detect under wavelength of detection analysis condition of sample finger-print, sees Fig. 2-4.
2.3 extract the investigation of solvent
Remove the outer dressing of sweet Chinese herbaceous peony Xiaoke Tablets, 5 parts, the powder of accurately weighed sweet Chinese herbaceous peony Xiaoke Tablets inside, every part of 0.2g, puts respectively in tool plug 25ml volumetric flask; To above-mentioned 5 minutes powder, use respectively appropriate 100% methyl alcohol, 70% methyl alcohol, 50% methyl alcohol, 30% methyl alcohol, five kinds of solvents of 50% ethanol (aqueous solution of organic solvent) to carry out ultrasonic extraction 10min, the identical solvent of cooling rear use is settled to scale, with 0.22 μ m filtering with microporous membrane, obtain the filtrate of different solvents extraction as need testing solution.
The HPLC chromatic graph spectrum of sweet Chinese herbaceous peony Xiaoke Tablets sample prepared by different solvents is shown in Figure of description 5-9; From HPLC result, after above-mentioned solvent extraction, all can obtain correct separated HPLC collection of illustrative plates; Wherein, in 50% methanol extract liquid chromatogram chromatographic peak separation best, and the Paeoniflorin chromatographic peak area of equivalent sample is maximum; Therefore select 50% methyl alcohol as sample preparation preferred solvent.
The investigation of 2.4 extracting modes
Get 5 parts, glycosides Chinese herbaceous peony Xiaoke Tablets powder, every part of 0.2g, accurately weighed, put in tool plug 25ml volumetric flask, adopt 50% methyl alcohol as solvent to sweet Chinese herbaceous peony Xiaoke Tablets ultrasonic extraction dissolve, check respectively ultrasonic processing 5min, 10min, 15min, 20min, the extraction effect of 30min to sweet Chinese herbaceous peony Xiaoke Tablets, ultrasonic rear cooling, constant volume, sample introduction analysis after 0.22 μ m filtering with microporous membrane.
Take ultrasonic extraction time as horizontal ordinate, take Paeoniflorin peak area as ordinate, investigate the relation of extraction time and extraction efficiency, experimental result is shown in Figure of description 10, result shows to be greater than 10min when extraction time, the impact that extraction time produces extraction efficiency reduces, and considers the quick, easy of experiment, therefore sample extraction ultrasonic time is decided to be 10min.
2.5 methodological study
The sample of preparing sweet Chinese herbaceous peony Xiaoke Tablets carries out the preliminary experiment of finger-print, by above-mentioned chromatographic condition, (remove the sweet Chinese herbaceous peony Xiaoke Tablets powder 0.2g except film-coating, accurately weighed, put in tool plug 25ml volumetric flask, add 50% methyl alcohol appropriate, ultrasonic extraction 10min, after cooling, add 50% methanol constant volume to scale, with 0.22 μ m filtering with microporous membrane, get filtrate 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, records chromatogram.Result shows, the relative retention time at each total peak and relative peak area ratio are basically identical, and the RSD of each peak retention time ratio is 0.00% ~ 0.46%, and the RSD of peak area ratio is all less than 3% at 0.20% ~ 2.83%, RSD, meets fingerprint pattern technology requirement.Result shows, the precision of the 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, and records chromatogram.Result shows, sample is in 24h, and the relative retention time at each total peak and relative peak area ratio are basically identical, and 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 is all less than 3%, meets the technical requirement of finger-print.Result shows that in test sample 24h, finger-print is stable.
2.5.3 repeated experiment
Precision takes same lot number (lot number: 111202) sample is 6 parts, and preparation method prepares need testing solution by need testing solution, respectively sample introduction, records chromatogram respectively.Result shows, the relative retention time at each total peak and relative peak area ratio are 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 is all less than 3%, meets the technical requirement of finger-print.
2.6 finger-prints and technical parameter
2.6.1 medicine
Lot number is 110601,110602,110603,111201,111202,120510,120515,120620,120622,120625 sweet Chinese herbaceous peony Xiaoke Tablets.
2.6.2 mix contrast solution: get epicatechin, Paeoniflorin, liquiritin, ammonium glycyrrhetate reference substance appropriate, add methyl alcohol ultrasonic dissolution, make every 1ml containing the mixing reference substance of epicatechin 0.059mg, Paeoniflorin 0.200mg, liquiritin 0.150mg, ammonium glycyrrhetate 0.150mg, according to the elution program of table 1, carry out HPLC analysis.
2.6.2 herbal extract
1) white Peony Root extract: the root of herbaceous peony (the dry root of ranunculaceae plant Chinese herbaceous peony Paeonia lacti flora Pall.) is appropriate, 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 in right amount 50% methyl alcohol ultrasonic, with 0.22 μ m filtering with microporous membrane, get subsequent filtrate as need testing solution.
2) licorice medicinal materials extract: Radix Glycyrrhizae (glycyrrhizic legume Glycyrrhiza uralensis Fisch.) is appropriate, 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 in right amount 50% methyl alcohol ultrasonic, with 0.22 μ m filtering with microporous membrane, get subsequent filtrate as need testing solution
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, the 10 batches of test sample finger-prints of take obtain " common pattern " finger-print in contrast as basis, see Fig. 1; Mainly contain 8 total peaks.
In sweet Chinese herbaceous peony Xiaoke Tablets, Paeoniflorin is its principal ingredient, can find out i.e. No. 4 peaks (RT ≌ 24.091min), Paeoniflorin peak from finger-print, and integral area is large and be main effective component, therefore be elected to be as with reference to peak; In addition, in sample finger-print, No. 3 peaks (RT ≌ 20.876min) are epicatechin, and No. 5 peaks (RT ≌ 35.214min) are that liquiritin, No. 7 peaks (RT ≌ 71.952min) are ammonium glycyrrhetate.
Take No. 4 peaks as with reference to peak, and each total peak average relative retention time (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
Fig. 1 is shown in by sweet Chinese herbaceous peony Xiaoke Tablets finger-print; Figure 11 is shown in by epicatechin, Paeoniflorin, liquiritin, ammonium glycyrrhetate mixing reference substance collection of illustrative plates; Figure 12 is shown in by the finger-print of white Peony Root extract; Figure 13 is shown in by the finger-print of licorice medicinal materials extract.
2.6.5 fingerprint similarity
Take reference fingerprint as reference, by < < traditional Chinese medicine fingerprint similarity evaluation software--2009 editions > > calculate 10 lot number sample similarities.
The similarity of table 2 sample
The similarity of 10 lot number samples is in Table 2, and the similarity of the sweet Chinese herbaceous peony Xiaoke Tablets of 10 lot numbers, between 0.884-0.965, has higher consistance between each batch of sample as shown in Table 2; The finger-print spectrogram of 10 lot number samples is shown in Figure 14.
Claims (9)
1. a quality determining method for sweet Chinese herbaceous peony Xiaoke Tablets, adopts HPLC finger print method to detect, and concrete steps are as follows:
1) get sweet Chinese herbaceous peony Xiaoke Tablets powder, accurately weighed and take methyl alcohol or ethanol after dissolution with solvents, constant volume, obtain need testing solution;
2) get Paeoniflorin, accurately weighed and take methyl alcohol after dissolution with solvents, constant volume, obtain object of reference solution;
3) accurate need testing solution or the object of reference solution injection high performance liquid chromatograph drawn, adopt reverse-phase chromatographic column to carry out HPLC analysis, the condition of HPLC finger print method is: 20～30 ℃ of column temperatures, mobile phase is acetonitrile-water-phosphoric acid system, gradient elution, flow velocity is 0.7～1.5ml/mim, and detection wavelength is 230nm; Described gradient elution program and mobile phase composed as follows:
2. detection method as claimed in claim 1, is characterized in that, solvent described in step 1) is methanol aqueous solution, the 100v/v% methyl alcohol that concentration is more than or equal to 30v/v%, or 50v/v% ethanol water; Step 2) solvent described in is 100v/v% methyl alcohol.
3. detection method as claimed in claim 1, is characterized in that, every milliliter of need testing solution is containing the sweet Chinese herbaceous peony Xiaoke Tablets of 6～10mg powder described in step 1).
4. detection method as claimed in claim 1, is characterized in that, is dissolved as ultrasonic dissolution described in 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) every milliliter of described object of reference solution is containing 0.2～0.6mg Paeoniflorin.
6. detection method as claimed in claim 1, is characterized in that, reverse-phase chromatographic column is Agilent ZORBAX SB-C18 chromatographic column described in step 3).
7. detection method as claimed in claim 1, is characterized in that, acetonitrile-water-phosphoric acid system comprises mobile phase A and Mobile phase B described in step 3), and wherein mobile phase A is acetonitrile, and Mobile phase B is 0.05v/v% phosphoric acid solution.
8. detection method as claimed in claim 1, it is characterized in that, in described finger-print, have 8 characteristic peaks, the relative retention time of characteristic peak is as follows: peak 2.987, No. 1.546,8, peak, No. 1.462,7, peak, No. 1.174,6, peak, No. 1.000,5, peak, No. 0.867,4, peak, No. 0.378,3, peak, No. 1 No. 0.108,2, peak; Characteristic peak relative peak area is as follows: peak 0.364, No. 0.392,8, peak, No. 0.155,7, peak, No. 0.190,6, peak, No. 1.000,5, peak, No. 0.391,4, peak, No. 1.119,3, peak, No. 1 No. 0.437,2, peak.
9. the application of the quality determining method of sweet Chinese herbaceous peony Xiaoke Tablets in the quality testing of sweet Chinese herbaceous peony Xiaoke Tablets described in the arbitrary claim of claim 1-8.
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