CN107843677A - Radix paeoniae rubrathe reference extract and its preparation method and application - Google Patents
Radix paeoniae rubrathe reference extract and its preparation method and application Download PDFInfo
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- CN107843677A CN107843677A CN201711277318.4A CN201711277318A CN107843677A CN 107843677 A CN107843677 A CN 107843677A CN 201711277318 A CN201711277318 A CN 201711277318A CN 107843677 A CN107843677 A CN 107843677A
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- radix paeoniae
- paeoniae rubrathe
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
Abstract
The invention provides a kind of radix paeoniae rubrathe reference extract, it is derived from：The radix paeoniae rubrathe medicinal powder of different batches is repeatedly extracted, obtains the red paeonia extract of different batches, then the red paeonia extract of different batches is allocated, obtains radix paeoniae rubrathe reference extract.The radix paeoniae rubrathe reference extract of the present invention ensure that the uniformity of the radix paeoniae rubrathe reference extract of different batches because being that the extract of different batches carries out allotment and formed；And its character is stable, uniform and easy to use.The radix paeoniae rubrathe reference extract is upper in application, it is as in quality control of the control for the radix paeoniae rubrathe and medicinal material or Chinese medicine preparation containing the radix paeoniae rubrathe/radix paeoniae rubrathe active ingredient, in this quality control procedure, it is that radix paeoniae rubrathe reference extract progress simple process can be used directly, it is easy to operate, can not only Qualitive test be carried out to medicinal material or Chinese medicine preparation, and can be also used for sxemiquantitative even quantitative analysis.
Description
Technical field
The present invention relates to quality control technologies for traditional Chinese medicine field, more particularly to a kind of radix paeoniae rubrathe reference extract and its preparation side
Method and application.
Background technology
The radix paeoniae rubrathe is the dry root for the ranunculaceae plant radix paeoniae rubrathe or the river radix paeoniae rubrathe, and property is bitter, is slightly cold, return liver warp, there is clearing heat and cooling blood, living
The effect of blood and dissolving stasis.
Existing traditional Chinese medicine quality control model is substantially the development along Natural Medicine Chemistry, a certain to Chinese medicine or several
Analysis method and the not only design of difinite quality but also the quality standard that can quantify of the active ingredient for target, with reference to the matter of external autonomic drug
Amount control method, the pattern of chemicals quality control is used for reference, and establish corresponding simple physics and chemistry by document report and differentiate, then
Develop into the discriminating based on spectrum, chromatogram and the quality standard of assay.All it is multicomponent synthesis per Chinese medicine simply
Body, which dictates that its distinctive globality and ambiguity, also indicate that one or two using in medicinal material even several compositions are used as medicinal material matter
Significant limitation be present in the evaluation method of amount.
1990 editions《Chinese Pharmacopoeia》Add the indentification by TLC of control medicinal material so that the discriminating of Chinese medicine and Chinese patent drug has
Very big progress.Chinese medicine and external herbal medicine increasingly pay attention to multicomponent or multi-component detection, such as German ginkgo at present
The quality control of leaf extract.The analysis method of finger-print, quality control can be carried out to medicinal material on the whole, currently still
There is very big researching value.Chinese Pharmacopoeia has two kinds " reference substances " in terms of quality of medicinal material is controlled at present, and chemical reference substance is with
Medicine control medicinal material.Wherein chemical reference substance can be used for Qualitive test and the quantitative analysis of medicinal material, and Chinese medicine control medicinal material is then used to show
Micro- discriminating and thin layer differentiate.However, chemical reference substance and Chinese medicine control medicinal material have its limitation in traditional Chinese medicine quality control.It is first
First, chemical composition variation in Chinese medicine, single or several compounds can not reflect the overall picture of medicinal material, and existing standard is past
Toward there is many leaks, shoddy phenomenon happens occasionally.Chinese medicine control medicinal material is influenceed by the place of production, growing environment, it is difficult to
Ensure per batch of uniform quality, and be only used for Qualitive test, the height of medicinal ingredient content can not be reflected.
Chinese medicine reference extract is the character and stable components prepared with Chinese medicine, can be used for qualitative or quantitative analysis
Extract, have four basic demands (ASCS), and reference extract should possess several primary conditions：Authenticity,
Crude drug source is reliable, representative；Specificity, the detection method specificity used；Con-sistency, difference batch
Secondary reference extract should be consistent；Stability, character are stable, uniform, easy to use.With TLC Fingerprints
And the methods of high-efficiency liquid-phase fingerprint, it can be used for the Qualitive test of medicinal material, by the reference extract of external standard method mark,
Sxemiquantitative and quantitative analysis detection can further be carried out.Chinese medicine reference extract will have important meaning to Chinese medicine quality control
Justice.But also just due to Chinese medicine reference extract have it is above-mentioned it is specific require, currently available technology does not have also or does not have maturation
Pass through the radix paeoniae rubrathe reference extract product being prepared using radix paeoniae rubrathe medicinal material as raw material.
The content of the invention
Present invention solves the technical problem that being to provide, a kind of batch uniformity is good, character is stable, uniform and easy to use
Radix paeoniae rubrathe reference extract, will the radix paeoniae rubrathe reference extract present invention also offers the application of the radix paeoniae rubrathe reference extract
For the radix paeoniae rubrathe and in the quality control of medicinal material or Chinese medicine preparation containing the radix paeoniae rubrathe/radix paeoniae rubrathe active ingredient.
One aspect of the present invention provides a kind of radix paeoniae rubrathe reference extract, it is characterised in that it is derived from：To different batches
Radix paeoniae rubrathe medicinal powder is repeatedly extracted, and obtains the red paeonia extract of different batches, then to the red paeonia extract of different batches
Allocated, obtain radix paeoniae rubrathe reference extract.
Preferably, the radix paeoniae rubrathe medicinal powder to different batches is repeatedly extracted, and is the Chinese herbaceous peony glycoside for containing it
The purity and/or concentration of composition improve, so as to obtain the red paeonia extract of different batches.
Preferably, in the radix paeoniae rubrathe reference extract Paeoniflorin content >=5.0%.
Preferably, the figure for using thin-layered chromatography and/or high performance liquid chromatography to obtain to the radix paeoniae rubrathe reference extract
It is consistent to compose corresponding raw medicinal material.
Preferably, the radix paeoniae rubrathe reference extract is detected using thin-layered chromatography at the Paeoniflorin in obtained chromatogram
Fluorescence spot and using high performance liquid chromatography detect obtained chromatogram Paeoniflorin opening position chromatographic peak should respectively with
Its corresponding chemical reference substance or its corresponding raw medicinal material are consistent.
Another aspect of the present invention provides a kind of preparation method of radix paeoniae rubrathe reference extract, comprises the following steps：
Step 1: extraction：Take the radix paeoniae rubrathe medicinal powder of different batches to be mixed respectively with ethanol, filter, obtain after homogenate extraction
To filtrate 1 and filter residue 1, and filtrate 1 is evaporated to obtain radix paeoniae rubrathe dry cream；
Step 2: prepare red paeonia extract：By gained radix paeoniae rubrathe dry cream, ethanol is dissolved in, the ethanol for obtaining radix paeoniae rubrathe dry cream is molten
Liquid, auxiliary material is added, be evaporated sieving and obtain red paeonia extract；
Step 3: allotment：The red paeonia extract of different batches is allocated, obtains radix paeoniae rubrathe reference extract.
Preferably, the filter residue 1 described in the step 1 extracts according to the extracting method of step 1 by n times, and by n times
The filtrate that extraction is collected merges Ji Wei extract solution with filtrate 1, and extract solution is evaporated to obtain radix paeoniae rubrathe dry cream；Wherein 6 >=N >=0, and N
For integer；
It is highly preferred that the N is 3.
Preferably, the extraction solution ethanol concentration described in the step 1 is 30%~95%；
It is highly preferred that it is 50% that solution ethanol concentration is extracted in the step 1.
Preferably, the w/v of the radix paeoniae rubrathe medicinal powder in the step 1 and ethanol is 1:5~1:45；
It is highly preferred that the w/v of the radix paeoniae rubrathe medicinal powder and ethanol in the step 1 is 1：10；
Preferably, the homogenate extraction time in the step 1 is 1~5min；
It is highly preferred that the homogenate extraction time in the step 1 is 1min；
Preferably, the filtering in the step 1 is with Medium speed filter paper or 2000 mesh sieve net filtrations；
It is highly preferred that the filtering in the step 1 is to use Medium speed filter paper.
Preferably, the w/v of radix paeoniae rubrathe dry cream and ethanol is 1 in the step 2:2~1:10；
Preferably, auxiliary material used is superfine silica gel powder and/or medical starch in the step 2；
Preferably, the step 2 is that 10%~50% micro mist of its weight is added in the ethanol solution of radix paeoniae rubrathe dry cream
Silica gel；
Preferably, the step 2 is that 40% superfine silica gel powder of its weight is added in the ethanol solution of radix paeoniae rubrathe dry cream；
Preferably, the step 2 be added in the ethanol solution of radix paeoniae rubrathe dry cream its weight 10%~30% it is medicinal
Starch；
Preferably, the step 2 is that 20% medical starch of its weight is added in the ethanol solution of radix paeoniae rubrathe dry cream；
Preferably, it was 90~200 mesh sieve net filtrations after the step 2 is evaporated；
Preferably, it was 200 mesh sieve net filtrations after the step 2 is evaporated；
Preferably, also include between the step 2 and step 3 with thin-layered chromatography and/or high performance liquid chromatography pair
The step of Paeoniflorin of the red paeonia extract of different batches is detected.
Preferably, the standard allocated in the step 3 is：Make the content of Paeoniflorin in the reference extract that finally gives
>=5.0%.
Preferably, the figure for using thin-layered chromatography and/or high performance liquid chromatography to obtain to the radix paeoniae rubrathe reference extract
It is consistent to compose corresponding raw medicinal material.
Preferably, the Paeoniflorin position in obtained chromatogram is detected using thin-layered chromatography to the radix paeoniae rubrathe reference extract
The fluorescence spot at the place of putting and the chromatogram for detecting to obtain using high performance liquid chromatography should divide in the chromatographic peak of Paeoniflorin opening position
Not corresponding chemical reference substance or its corresponding raw medicinal material are consistent.
Another aspect of the invention provides a kind of discriminating of radix paeoniae rubrathe reference extract in medicinal material or Chinese medicine preparation, or the radix paeoniae rubrathe or
Application in the quality control of medicinal material or Chinese medicine preparation containing the radix paeoniae rubrathe/radix paeoniae rubrathe active ingredient.
Preferably, the discriminating of the medicinal material or Chinese medicine preparation, or the radix paeoniae rubrathe and the Chinese medicine preparation containing the radix paeoniae rubrathe/radix paeoniae rubrathe active ingredient
The method of quality control be：By described radix paeoniae rubrathe reference extract, medicinal material or Chinese medicine preparation with thin-layered chromatography and/or efficiently
Liquid chromatography is detected, and contrast differentiates.
Preferably, the thin-layered chromatography and/or high performance liquid chromatography are to radix paeoniae rubrathe reference extract, medicinal material or Chinese medicine
Paeoniflorin in preparation is detected.
Preferably, when described radix paeoniae rubrathe reference extract, medicinal material or Chinese medicine preparation are detected with thin-layered chromatography,
Need radix paeoniae rubrathe reference extract, medicinal material or Chinese medicine preparation being configured to solution to carry out thin-layered chromatography detection again；
The compound method of wherein radix paeoniae rubrathe reference extract solution is：The radix paeoniae rubrathe reference extract adds its quality 100-
The ethanol of 400 times of volumes, it is ultrasonically treated, shakes up, crosses 0.12-0.32 μm of filter membrane and produce radix paeoniae rubrathe reference extract solution；
Preferably, the radix paeoniae rubrathe reference extract is added to the ethanol of its 330 times of volume of quality, ultrasonic 500w handles 30 points
Clock, shake up, cross 0.22 μm of filter membrane and produce radix paeoniae rubrathe reference extract solution；
The compound method of its Chinese medicine or Chinese medicine preparation solution is：Get it filled material or Chinese medicine preparation adds 50-150 times of its quality
The ethanol of volume, centrifuge after supersound process, take supernatant to cross 0.12-0.32 μm of filter membrane and produce medicinal material or Chinese medicine preparation solution.
Preferably, getting it filled material or Chinese medicine preparation adds the ethanol of its 100 times of volume of quality, ultrasonic 500w is handled 15 minutes,
3200 revs/min centrifuge 3 minutes, take supernatant to cross 0.22um filter membranes and produce medicinal material or Chinese medicine preparation solution.
Preferably, the thin-layered chromatography testing conditions are：
Lamellae：HPTLC G60 prefabricated boards；
Point sample：2 μ l, the long 8mm of ribbon point sample；
Solvent：Toluene：Ethyl acetate：Methanol：Water：Glacial acetic acid=10:7:5:0.5:0.1；
The drying of lamellae：Lamellae after point sample is placed in phosphorus pentoxide vacuum desiccator 2 hours, ensures lamellae
Dry；
Inspect:Spray is placed under incandescence and inspected with the sulfuric acid ethanol developer of 5% vanillic aldehyde -10%.
Preferably, examined when by described radix paeoniae rubrathe reference extract, medicinal material or Chinese medicine preparation with high performance liquid chromatography
, it is necessary to which radix paeoniae rubrathe reference extract, medicinal material or Chinese medicine preparation are configured into solution carries out high performance liquid chromatography detection again during survey；
The compound method of wherein radix paeoniae rubrathe reference extract solution is：Precision weighs the radix paeoniae rubrathe reference extract 0.2g, adds
Enter ethanol solution 10ml, ultrasonic 500w processing 30 minutes, let cool, be configured to the solution that concentration is 20mg/ml with ethanol, cross 0.22
μm filter membrane, take subsequent filtrate, produce radix paeoniae rubrathe reference extract solution；
The compound method of its Chinese medicine or Chinese medicine preparation solution is：Get it filled material or Chinese medicine preparation cross weighed 2g after No. two sieves,
To put in 50ml conical flask with cover, precision adds ethanol solution 45ml, after water-bath backflow 1h, lets cool, and adds ethanol at scale 50ml,
Shake up, cross 0.22 μm of filter membrane, take subsequent filtrate to produce medicinal material or Chinese medicine preparation solution.
Preferably, described high performance liquid chromatography testing conditions：
Chromatographic apparatus：Agilent 1100series high performance liquid chromatographs, equipped with DAD detectors (U.S., Agilent
Technologies)
Chromatographic column：Waters Symmetry C18column (250mm × 4.6mm I.D, 5 μm)；
Mobile phase：A- acetonitriles, B-0.1% phosphate aqueous solutions；
Gradient elution program：0-5min：10%A → 15%A, 5-30min：15%A → 22%A, 30-60min：22%A
→ 49%A, 60-65min：49%A → 80%A；
0-5min：90%B → 85%B, 5-30min：85%B → 78%B, 30-60min：78%B → 51%B, 60-
65min：51%B → 20%B；
Detection wavelength 230nm (DAD detectors)；Flow velocity 0.8ml/min；The μ l of sample size 10；25 DEG C of column temperature, run time：
65min。
Beneficial effect
The radix paeoniae rubrathe reference extract of the present invention is overcome because of Chinese medicine pair because being that the extract of different batches carries out allotment and formed
Influenceed according to medicinal material by the place of production, growing environment, it is difficult to ensure that the defects of every batch of uniform quality, so as to ensure that different batches
The uniformity of secondary radix paeoniae rubrathe reference extract；And its character is stable, uniform and easy to use.The radix paeoniae rubrathe reference extract exists
It is by radix paeoniae rubrathe reference extract after quantitative analysis, as control for the radix paeoniae rubrathe and containing the radix paeoniae rubrathe/radix paeoniae rubrathe active ingredient using upper
Medicinal material or Chinese medicine preparation quality control in, be simply to be located radix paeoniae rubrathe reference extract in this quality control procedure
Reason can be used directly, and easy to operate, especially in multicomponent assay, the preparation of reference extract solution is more molten than reference substance
The preparation of liquid is easier, not only can carry out Qualitive test to medicinal material or Chinese medicine preparation, and can be also used for sxemiquantitative very
To quantitative analysis.
Brief description of the drawings
From detailed description below in conjunction with the accompanying drawings, it will be more clearly understood the present invention above-mentioned and other purpose,
Feature and other advantages, wherein,
Fig. 1 is radix paeoniae rubrathe reference extract preparation flow figure；
Fig. 2 is to be directed to carry out thin-layer chromatography to commercially available medicinal material as reference substance using chemical reference substance and radix paeoniae rubrathe reference extract
The high performance thin layer chromatography figure that method obtains, wherein label 1 correspond to radix paeoniae rubrathe reference extract, 2-7 be corresponding in turn to the radix paeoniae rubrathe 1, the radix paeoniae rubrathe 2,
The radix paeoniae rubrathe 3, the radix paeoniae rubrathe 4, the medicinal material of the radix paeoniae rubrathe 5 and the radix paeoniae rubrathe 6,8 chromatographic band are corresponding in turn to as reference substance Paeoniflorin, catechu from lower to upper
Element, benzoyl oxypaeoniflorin, benzoylpaeoniflorin；
Fig. 3 is to be directed to carry out efficient liquid phase to commercially available medicinal material as reference substance using chemical reference substance and radix paeoniae rubrathe reference extract
The HPLC finger-print stacking charts that chromatography obtains, from top to bottom, R corresponds to common pattern, and S corresponds to radix paeoniae rubrathe reference extract, 1-6
The radix paeoniae rubrathe 1, the radix paeoniae rubrathe 2, the radix paeoniae rubrathe 3, the radix paeoniae rubrathe 4, the radix paeoniae rubrathe 5 and the medicinal material of the radix paeoniae rubrathe 6 are corresponded to respectively；
Fig. 4 is the finger-print common pattern collection of illustrative plates for the radix paeoniae rubrathe medicinal material established, wherein No. 11 are gallic acid, No. 33 chromatograms
Peak is nutgall acyl methyl esters, and No. 48 chromatographic peaks are Paeoniflorin, and No. 62 chromatographic peaks are Penta-O-galloyl-D-glucopyranose, and No. 66 chromatographic peaks are
Benzoic acid, No. 91 chromatographic peaks are benzoylpaeoniflorin, and No. 97 chromatographic peaks are Paeonol.
Embodiment
Embodiments of the invention are described below in detail.The embodiments described below is exemplary, is only used for explaining this hair
It is bright, and be not considered as limiting the invention.Unreceipted particular technique or condition in embodiment, according to text in the art
Offer described technology or condition or carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument,
For the conventional products of acquisition purchased in market can be passed through.Term as used herein "and/or" includes the listed of one or more correlations
The arbitrary and all combination of project.
The instrument used in following examples and the source of material are as follows：
It is envisaged for preparing the medicinal material of reference extract:The radix paeoniae rubrathe (Inner Mongol).
The semi-automatic point sample instrument of the thin-layer chromatographys of Linomat 5, the full-automatic point sample instrument of the thin-layer chromatographys of ATS 4, thin-layer chromatography double flute
Expansion cylinder, Chromatogram Immersion Device III chromatogram colour developing dipping tanks and TLC visualizer thin layers
Chromatogram video camera (Switzerland, CAMAG).
The series high performance liquid chromatographs of Agilent 1100, equipped with DAD detectors (U.S., Agilent
Technologies)。
Toluene, ethyl acetate, methanol, glacial acetic acid, phosphoric acid are to analyze pure (Guangzhou Chemical Reagent Factory).
Acetonitrile is analysis pure (Merck KGaA).
Paeoniflorin, indicate purity >=98%, (Baoji time bio tech ltd)；
Test the medicinal material radix paeoniae rubrathe：
Radix paeoniae rubrathe medicinal material 6 batches is purchased in the major pharmacy in Guangzhou and medicinal material market.
Embodiment 1：The preparation of radix paeoniae rubrathe reference extract
The preparation method of radix paeoniae rubrathe reference extract of the present invention is present embodiments provided, its method flow diagram is as shown in Figure 1.
One：Extraction
Choose radix paeoniae rubrathe medicinal material (Inner Mongol, genunie medicinal materials), be made powder, medicinal powder cross No. two sieves (850 ± 29 μm, 24
Mesh), then add its 10 times of volume of quality ethanol (i.e. solid-to-liquid ratio be 1：10 (w/V)), ultrasonic (power 500w, normal temperature) extraction
Middling speed qualitative filter paper filters after 30min, collects filter residue 1 and filtrate 1, filter residue 1 extracted again by same procedure it is secondary, and will again
The filtrate for extracting secondary collection merges Ji Wei extract solution with filtrate 1, and extract solution solvent evaporated is got dry extract；
Two：Prepare red paeonia extract
After dry cream is dissolved completely with ethanol in proper amount, then add 40% superfine silica gel powder (mountains and rivers medicine is auxiliary) of dry cream quality, use
Rotary Evaporators are evaporated, and be crushed 110 mesh sieves, are obtained red paeonia extract.
3 batches of red paeonia extracts are prepared, high effective liquid chromatography for measuring are utilized by reference substance, testing result is as shown in table 1：
Table 1
Three：Allotment
The red paeonia extract of 3 batches of step 2 is pressed 1:The mixing of 1 ratio blends to obtain radix paeoniae rubrathe reference extract, finally
It is about 1 that product, which corresponds to crude drug ratio,：2 (g/g), high effective liquid chromatography for measuring is utilized by reference substance, wherein each composition
Content measurement result it is as shown in Figure 2.
Table 2
Allotment standard is：Content >=5.0% of Paeoniflorin in final radix paeoniae rubrathe reference extract should be made, and (content is with wt%
Meter).The scope of the content of each composition in this allotment standard, which is also that experiment is comprehensive repeatedly by repeatedly, keeps stability, uniformity
And the optimum data that application below etc. is drawn.
The character analysis of the radix paeoniae rubrathe reference extract of embodiment 2
1. apparent state：The radix paeoniae rubrathe reference extract that embodiment 1 obtains is yellow grey powder.
2. determination of moisture：Carried out according to 2015 editions Chinese Pharmacopoeia annex IX G (hypobaric drying method).Testing result is the radix paeoniae rubrathe
Reference extract water content is 3.9%.
3. uniformity test：3 batch radix paeoniae rubrathe reference extracts are prepared according to the method for embodiment 1, after measured between each batch
The thin-layer chromatography testing result difference very little for Paeoniflorin, the fluorescence spot of Paeoniflorin has obvious display, and is distributed
It is very consistent；Through high performance liquid chromatography detection, its paeoniflorin content is being allocated within critical field.Therefore utilize the present invention's
The radix paeoniae rubrathe reference extract uniformity that the preparation method of radix paeoniae rubrathe reference extract is prepared is very good.
4. stability test：
The test sample of the radix paeoniae rubrathe reference extract of the method preparation according to embodiment 1 of 3 different batches is taken, according to country
The relevant regulations of " requirements of national drug standards material Development Techniques " that pharmacopoeia commission works out, inspection target include character and molten
Xie Xing.
Test sample opening is put in suitable clean container, is placed 10 days at a temperature of 60 DEG C, is sampled in the 5th day and the 10th day,
Detected by stability high spot reviews project.
As a result show, before and after hot test test sample character without significant change, before and after hot test thin-layer chromatogram also without
Significant change, dissolution rate measurement result carry out Independent samples t-test with SPSS, result of calculation P ＞ 0.05, illustrate no conspicuousness
Difference.
Comparative example 1
Difference with embodiment 1 is：
To using methanol to be carried out instead of ethanol in the step one in embodiment 1, the content of the radix paeoniae rubrathe dry cream finally obtained is bright
It is aobvious be less than embodiment 1, it can be seen that, its value is substantially lower than the yield of ethanol extraction more, only increasing extracted amount or number
Be possible to reach within allotment critical field.
Embodiment 3
Present embodiments provide the application for the radix paeoniae rubrathe reference extract that embodiment 1 is prepared.
With thin-layered chromatography and high performance liquid chromatography respectively using chemical reference substance and radix paeoniae rubrathe reference extract as reference
Material is analyzed commercially available medicinal material.
1 thin-layer chromatography
1.1 sample preparation
Chemical reference substance solution：Precision weighs Paeoniflorin, and 1mg/ml solution is configured to methanol.
Radix paeoniae rubrathe reference extract solution：Precision weighs the radix paeoniae rubrathe reference extract 0.5g that embodiment 1 is prepared, and adds second
Alcohol 10ml, ultrasonic (500w) are handled 15 minutes, shaken up, and are crossed 0.22 μm of filter membrane and are produced radix paeoniae rubrathe reference extract solution.
Medicinal material need testing solution：Get it filled each 1g of shop medicinal material, adds ethanol 50ml, and ultrasonic (500w) takes out after 30 minutes, from
The heart 3 minutes (rotating speed is 3200 turns per minute), takes supernatant to cross 0.22um filter membranes and produces medicinal material need testing solution.Pharmacy's medicinal material is equal
Buy from Guangzhou, be respectively：The radix paeoniae rubrathe 1, the radix paeoniae rubrathe 2, the radix paeoniae rubrathe 3, the radix paeoniae rubrathe 4, the medicinal material of the radix paeoniae rubrathe 5 and the radix paeoniae rubrathe 6.
1.2 thin-layer chromatographys detect
Testing conditions are as follows：
Lamellae：HPTLC G60 prefabricated boards (Merck)；
Point sample：Medicinal material：2 μ l, ERS：6 μ l, the long 8mm of ribbon point sample；
Solvent：Toluene:Ethyl acetate:Methanol:Water:Glacial acetic acid=10:7:5:0.5:0.1；
Expansion mode：Add solvent 12ml, common pre-equilibration 15 minutes in side in double flute expansion cylinder (20cm × 10cm)；
The drying of lamellae：Lamellae after point sample is placed in phosphorus pentoxide vacuum desiccator 2 hours, ensures the drying of lamellae；
Inspect:Spray is placed under incandescence and inspected with the sulfuric acid ethanol of 5% vanillic aldehyde -10%.
Testing result under incandescence as shown in Fig. 2 to inspect thin-layer chromatogram (T：25 DEG C, RH：76%).The color of label 1
Bands of a spectrum correspond to radix paeoniae rubrathe reference extract, and 2-7 is corresponding in turn to the medicine of the radix paeoniae rubrathe 1, the radix paeoniae rubrathe 2, the radix paeoniae rubrathe 3, the radix paeoniae rubrathe 4, the radix paeoniae rubrathe 5 and the radix paeoniae rubrathe 6
Material, the chromatographic band of label 8 is arranged from lower to upper to be corresponding in turn to as reference substance Paeoniflorin, catechin, benzoyl oxypaeoniflorin, benzene first
Acyl Paeoniflorin.
Interpretation of result：As shown in Figure 2, Paeoniflorin, catechin, benzoyl oxypaeoniflorin, benzoylpaeoniflorin separation feelings
Condition is preferable, and radix paeoniae rubrathe reference extract and medicinal material (radix paeoniae rubrathe 1- radix paeoniae rubrathe 6) can show identical spot in same position, from collection of illustrative plates
Find out that radix paeoniae rubrathe reference extract and medicinal material (radix paeoniae rubrathe 1- radix paeoniae rubrathe 6) have the uniformity of height.
2 high performance liquid chromatography
2.1 sample preparation
Chemical reference substance solution：Precision weighs Paeoniflorin reference substance (by phosphorus pentoxide vacuum drying 24h), uses methanol
The solution of 1.0mg/ml concentration is configured to, as test sample.
Radix paeoniae rubrathe reference extract solution：Precision weighs red paeonia extract, adds 50% EtOH Sonicate and extracts 30 minutes, fixed
Hold, be configured to the solution of 20mg/ml concentration, cross 0.22 μm of miillpore filter, take subsequent filtrate as extract reference substance solution.
Medicinal material need testing solution：Each pharmacy's medicinal powder crosses No. two sieves, accurately weighed each 2g, puts 50ml conical flask with cover
In, ethanol solution 45ml is added, water-bath flows back after 1h, filters into 50ml volumetric flasks, let cool by fast grade filter paper, add ethanol to determine
Hold at scale 50ml, shake up, cross 0.22 μm of filter membrane, take subsequent filtrate to produce medicinal material solution.
Pharmacy's medicinal material is bought from Guangzhou, is respectively：The radix paeoniae rubrathe 1, the radix paeoniae rubrathe 2, the radix paeoniae rubrathe 3, the radix paeoniae rubrathe 4, the medicinal material of the radix paeoniae rubrathe 5 and the radix paeoniae rubrathe 6
2.2 high performance liquid chromatography detection
High performance liquid chromatography testing conditions are as follows：
Chromatographic apparatus：The series high performance liquid chromatographs of Agilent 1100, equipped with DAD detectors (U.S., Agilent
Technologies)
Chromatographic column：Waters Symmetry C18 column (250mm × 4.6mm I.D, 5 μm)；
Mobile phase：A- acetonitriles, B-0.1% phosphate aqueous solutions；
Gradient elution program：0-5min：10%A → 15%A, 5-30min：15%A → 22%A, 30-60min：22%A
→ 49%A, 60-65min：49%A → 80%A；
0-5min：90%B → 85%B, 5-30min：85%B → 78%B, 30-60min：78%B → 51%B, 60-
65min：51%B → 20%B；
Detection wavelength 230nm (DAD detectors)；Flow velocity 0.8ml/min；The μ l of sample size 10；25 DEG C of column temperature, run time：
65min。
High effective liquid chromatography for detecting：It is accurate respectively to draw chemical reference substance solution, radix paeoniae rubrathe reference extract solution
With each 10 μ l of medicinal material need testing solution, liquid chromatograph is injected.
High performance liquid chromatography testing result：
Measure, chromatogram is recorded, produces the HPLC finger-print stacking charts shown in Fig. 3, from top to bottom, R correspondingly shares mould
Formula, S correspond to radix paeoniae rubrathe reference extract, and 1-6 corresponds to the radix paeoniae rubrathe 1, the radix paeoniae rubrathe 2, the radix paeoniae rubrathe 3, the radix paeoniae rubrathe 4, the radix paeoniae rubrathe 5 and the medicinal material of the radix paeoniae rubrathe 6 respectively.
As seen from Figure 3, the finger-print of the medicinal material of the radix paeoniae rubrathe 1- radix paeoniae rubrathe 6 has the uniformity of height, thus in accordance with China
Pharmacopoeia commission of people's republic similarity evaluation (2012.130723 version) establishes RADIX PAEONIAE RUBRA
The finger-print common pattern of material, and similarity analysis is carried out to all samples.Common pattern collection of illustrative plates is as shown in figure 4, wherein 11
Number it is gallic acid, No. 33 chromatographic peaks are nutgall acyl methyl esters, and No. 48 chromatographic peaks are Paeoniflorin, and No. 62 chromatographic peaks are five nutgalls
Acyl glucose, No. 66 chromatographic peaks are benzoic acid, and No. 91 chromatographic peaks are benzoylpaeoniflorin, and No. 97 chromatographic peaks are Paeonol.
According to set radix paeoniae rubrathe medicinal materials fingerprint common pattern, using included angle cosine algorithm according to each sample component and its
Peak area carries out similarity evaluation to 6 batches of radix paeoniae rubrathe medicinal materials and reference extract sample, as a result as shown in table 3.
Table 3
| Sample | Similarity |
| The radix paeoniae rubrathe 1 | 0.999 |
| The radix paeoniae rubrathe 2 | 0.999 |
| The radix paeoniae rubrathe 3 | 0.998 |
| The radix paeoniae rubrathe 4 | 0.988 |
| The radix paeoniae rubrathe 5 | 0.999 |
| The radix paeoniae rubrathe 6 | 0.994 |
| Radix paeoniae rubrathe reference extract | 0.999 |
According to above similarity analysis result, the similarity of 6 batches of medicinal materials and radix paeoniae rubrathe medicinal materials fingerprint common pattern exists
In the range of 0.988-0.999, similarity is very high.The similarity of radix paeoniae rubrathe reference extract and radix paeoniae rubrathe medicinal materials fingerprint common pattern
For 0.999, show the present invention radix paeoniae rubrathe reference extract and medicinal material uniformity it is good.
It can be seen from the result of TLC and HPLC finger-prints, the radix paeoniae rubrathe reference extract is examined using thin-layered chromatography
The corresponding raw medicinal material of the chromatogram that measures is consistent, more precisely, thin layer is used to the radix paeoniae rubrathe reference extract
The fluorescence spot and use high performance liquid chromatography of Paeoniflorin opening position in the chromatogram that chromatography detects to obtain detect to obtain
Chromatogram distinguish corresponding chemical reference substance in the chromatographic peak of Paeoniflorin opening position or its corresponding raw medicinal material is consistent,
Therefore the radix paeoniae rubrathe reference extract of the present invention can be applied to the Qualitive test of medicinal material or Chinese medicine preparation, such as to medicinal material or Chinese medicine system
The Paeoniflorin composition of agent carries out qualitative analysis.
According to HPLC measurement results and statistical analysis, radix paeoniae rubrathe medicinal materials fingerprint common pattern and the radix paeoniae rubrathe medicinal material of foundation
Similarity it is high, and the present invention radix paeoniae rubrathe reference extract and radix paeoniae rubrathe medicinal materials fingerprint common pattern similarity pole
Height, this explanation carry out the assay reliability of Paeoniflorin using the radix paeoniae rubrathe reference extract of the present invention to medicinal material or Chinese medicine preparation
It is high, therefore the radix paeoniae rubrathe reference extract of the present invention can be applied to the sxemiquantitative discriminatory analysis of medicinal material or Chinese medicine preparation, can also answer
For the radix paeoniae rubrathe and in the quality control of medicinal material or Chinese medicine preparation containing the radix paeoniae rubrathe/radix paeoniae rubrathe active ingredient, such as to medicinal material or Chinese medicine system
The Paeoniflorin composition of agent carries out sxemiquantitative discriminatory analysis, or to the radix paeoniae rubrathe and medicinal material or Chinese medicine containing the radix paeoniae rubrathe/radix paeoniae rubrathe active ingredient
Preparation carries out half-quantitative detection and then controls its quality.
The better embodiment of the present invention is the foregoing is only, is not intended to limit the invention, it is all the present invention's
All any modification, equivalent and improvement made within spirit and principle etc., should be included in the scope of the protection.
Claims (10)
1. a kind of radix paeoniae rubrathe reference extract, it is characterised in that it is derived from：The radix paeoniae rubrathe medicinal powder of different batches is carried out repeatedly
Extraction, obtains the red paeonia extract of different batches, then the red paeonia extract of different batches is allocated, and obtains radix paeoniae rubrathe control
Extract；
Optional, the radix paeoniae rubrathe medicinal powder to different batches is repeatedly extracted, and is the Chinese herbaceous peony methods of glycosides for containing it
Purity and/or concentration improve, so as to obtain the red paeonia extract of different batches；
Optional, content >=5.0% of Paeoniflorin in the radix paeoniae rubrathe reference extract；
It is optional, to the radix paeoniae rubrathe reference extract using the collection of illustrative plates that thin-layered chromatography and/or high performance liquid chromatography obtain with
Its corresponding raw medicinal material is consistent；
It is optional, the radix paeoniae rubrathe reference extract is detected using thin-layered chromatography glimmering at the Paeoniflorin in obtained chromatogram
The chromatogram that hot spot point and use high performance liquid chromatography detect to obtain is in albiflorin, Paeoniflorin and benzoylpaeoniflorin position
The chromatographic peak at the place of putting should distinguish corresponding chemical reference substance or its corresponding raw medicinal material is consistent.
2. a kind of preparation method of the radix paeoniae rubrathe reference extract described in claim 1, comprises the following steps：
Step 1: extraction：Take the radix paeoniae rubrathe medicinal powder of different batches to be mixed respectively with ethanol, filter, filtered after homogenate extraction
Liquid 1 and filter residue 1, and filtrate 1 is evaporated to obtain radix paeoniae rubrathe dry cream；
Step 2: prepare red paeonia extract：By gained radix paeoniae rubrathe dry cream, ethanol is dissolved in, obtains the ethanol solution of radix paeoniae rubrathe dry cream, then
Auxiliary material is added, sieving is evaporated and obtains red paeonia extract；
Step 3: allotment：The red paeonia extract of different batches is allocated, obtains radix paeoniae rubrathe reference extract.
3. the preparation method of radix paeoniae rubrathe reference extract according to claim 2, it is characterised in that described in the step 1
Filter residue 1 extracted according to the extracting method of step 1 by n times, and n times are extracted to the filtrate collected and merged with filtrate 1 as carrying
Liquid is taken, extract solution is evaporated to obtain radix paeoniae rubrathe dry cream；Wherein 6 >=N >=0, and N is integer；
Optional, the N is 3.
4. the preparation method of radix paeoniae rubrathe reference extract according to claim 2, it is characterised in that described in the step 1
Extraction solution ethanol concentration be 30%~95%；
Optional, it is 50% that solution ethanol concentration is extracted in the step 1.
5. the preparation method of radix paeoniae rubrathe reference extract according to claim 3, it is characterised in that red in the step 1
The w/v of Chinese herbaceous peony medicinal powder and ethanol is 1:5~1:45；
Optional, the w/v of radix paeoniae rubrathe medicinal powder and ethanol in the step 1 is 1：10；
Optional, the homogenate extraction time in the step 1 is 1~5min；
Optional, the homogenate extraction time in the step 1 is 1min；
Optional, the filtering in the step 1 is with Medium speed filter paper or 2000 mesh sieve net filtrations；
Optional, the filtering in the step 1 is to use Medium speed filter paper.
6. the preparation method of radix paeoniae rubrathe reference extract according to claim 3, it is characterised in that the radix paeoniae rubrathe in the step 2
The w/v of dry cream and ethanol：1:2~1:10；
Optional, auxiliary material used is superfine silica gel powder and/or medical starch in the step 2；
Optional, the step 2 is its weight is added in the ethanol solution of radix paeoniae rubrathe dry cream 10%~50% micro mist silicon
Glue；
Optional, the step 2 is that 40% superfine silica gel powder of its weight is added in the ethanol solution of radix paeoniae rubrathe dry cream；
Optional, the step 2 is that 10%~30% medicinal shallow lake of its weight is added in the ethanol solution of radix paeoniae rubrathe dry cream
Powder；
Optional, the step 2 is that 20% medical starch of its weight is added in the ethanol solution of radix paeoniae rubrathe dry cream；
It is optional, the step 2 be evaporated after be 90~200 mesh sieve net filtrations；
It is optional, the step 2 be evaporated after be 200 mesh sieve net filtrations；
Optional, also include between the step 2 and step 3 with thin-layered chromatography and/or high performance liquid chromatography to difference
The step of Paeoniflorin of the red paeonia extract of batch is detected.
7. the preparation method of radix paeoniae rubrathe reference extract according to claim 2, it is characterised in that allocated in the step 3
Standard be：Make content >=5.0% of Paeoniflorin in the reference extract that finally gives.
8. radix paeoniae rubrathe reference extract described in claim 1 is in the discriminating of medicinal material or Chinese medicine preparation, or the radix paeoniae rubrathe or containing the radix paeoniae rubrathe/radix paeoniae rubrathe
Application in the quality control of the medicinal material or Chinese medicine preparation of active ingredient；
Optional, the discriminating of the medicinal material or Chinese medicine preparation, or the matter of the radix paeoniae rubrathe and the Chinese medicine preparation containing the radix paeoniae rubrathe/radix paeoniae rubrathe active ingredient
Measuring the method controlled is：By radix paeoniae rubrathe reference extract, medicinal material or the Chinese medicine preparation described in claim 1 with thin-layered chromatography and/
Or high performance liquid chromatography is detected, contrast differentiates；
Optional, the thin-layered chromatography and/or high performance liquid chromatography are to radix paeoniae rubrathe reference extract, medicinal material or Chinese medicine preparation
In Paeoniflorin detected.
9. application according to claim 8, it is characterised in that when by the radix paeoniae rubrathe reference extract described in claim 1, medicinal material or
, it is necessary to which radix paeoniae rubrathe reference extract, medicinal material or Chinese medicine preparation are configured into solution when Chinese medicine preparation is detected with thin-layered chromatography
Thin-layered chromatography detection is carried out again；
The compound method of wherein radix paeoniae rubrathe reference extract solution is：Radix paeoniae rubrathe reference extract described in claim 1 is added it
The ethanol of 100-400 times of volume of quality, it is ultrasonically treated, shakes up, it is molten produces radix paeoniae rubrathe reference extract for 0.12-0.32 μm of filter membrane excessively
Liquid；
It is optional, the radix paeoniae rubrathe reference extract described in claim 1 is added to the ethanol of its 330 times of volume of quality, ultrasonic 500w
Processing 30 minutes, shakes up, and crosses 0.22 μm of filter membrane and produces radix paeoniae rubrathe reference extract solution；
The compound method of its Chinese medicine or Chinese medicine preparation solution is：Get it filled material or Chinese medicine preparation adds 50-150 times of volume of its quality
Ethanol, centrifuge after supersound process, take supernatant to cross 0.12-0.32 μm of filter membrane and produce medicinal material or Chinese medicine preparation solution；
It is optional, get it filled material or Chinese medicine preparation adds the ethanol of its 100 times of volume of quality, ultrasonic 500w handles 15 minutes, and 3200
Rev/min centrifugation 3 minutes, take supernatant to cross 0.22um filter membranes and produce medicinal material or Chinese medicine preparation solution；
Optional, the thin-layered chromatography testing conditions are：
Lamellae：HPTLC G60 prefabricated boards；
Point sample：2 μ l, the long 8mm of ribbon point sample；
Solvent：Toluene:Ethyl acetate:Methanol:Water:Glacial acetic acid=10:7:5:0.5:0.1；
The drying of lamellae：Lamellae after point sample is placed in phosphorus pentoxide vacuum desiccator 2 hours, ensures the dry of lamellae
It is dry；
Inspect:Spray is placed under incandescence and inspected with the sulfuric acid ethanol developer of 5% vanillic aldehyde -10%.
10. application according to claim 8, it is characterised in that when by radix paeoniae rubrathe reference extract, the medicinal material described in claim 1
Or Chinese medicine preparation when being detected with high performance liquid chromatography, it is necessary to which radix paeoniae rubrathe reference extract, medicinal material or Chinese medicine preparation are prepared
High performance liquid chromatography detection is carried out again into solution；
The compound method of wherein radix paeoniae rubrathe reference extract solution is：Precision weighs the radix paeoniae rubrathe reference extract described in claim 1
0.2g, ethanol solution 10ml is added, ultrasonic 500w processing 30 minutes, is let cool, it is the molten of 20mg/ml to be configured to concentration with ethanol
Liquid, 0.22 μm of filter membrane is crossed, subsequent filtrate is taken, produces radix paeoniae rubrathe reference extract solution；
The compound method of its Chinese medicine or Chinese medicine preparation solution is：Get it filled material or Chinese medicine preparation crosses weighed 2g after No. two sieves, put
In 50ml conical flask with cover, precision adds ethanol solution 45ml, after water-bath backflow 1h, lets cool, adds ethanol to be shaken at scale 50ml
It is even, 0.22 μm of filter membrane is crossed, takes subsequent filtrate to produce medicinal material or Chinese medicine preparation solution；
Optional, described high performance liquid chromatography testing conditions：
Chromatographic apparatus：Agilent 1100series high performance liquid chromatographs, equipped with DAD detectors (U.S., Agilent
Technologies)
Chromatographic column：Waters Symmetry C18 column (250mm × 4.6mm I.D, 5 μm)；
Mobile phase：A- acetonitriles, B-0.1% phosphate aqueous solutions；
Gradient elution program：0-5min：10%A → 15%A, 5-30min：15%A → 22%A, 30-60min：22%A →
49%A, 60-65min：49%A → 80%A；
0-5min：90%B → 85%B, 5-30min：85%B → 78%B, 30-60min：78%B → 51%B, 60-65min：
51%B → 20%B；
Detection wavelength 230nm (DAD detectors)；Flow velocity 0.8ml/min；The μ l of sample size 10；25 DEG C of column temperature, run time：
65min。
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