CN108088715A - Moutan bark reference extract and its preparation method and application - Google Patents
Moutan bark reference extract and its preparation method and application Download PDFInfo
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- CN108088715A CN108088715A CN201711279755.XA CN201711279755A CN108088715A CN 108088715 A CN108088715 A CN 108088715A CN 201711279755 A CN201711279755 A CN 201711279755A CN 108088715 A CN108088715 A CN 108088715A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
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- 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
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- G—PHYSICS
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- 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
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- 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
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Abstract
The present invention provides a kind of moutan bark reference extracts, derive from：The moutan bark medicinal powder of different batches is repeatedly extracted, obtains the Cortex Moutan extract of different batches, then the Cortex Moutan extract of different batches is allocated, obtains moutan bark reference extract.The moutan bark reference extract of the present invention ensure that the uniformity of the moutan bark reference extract of different batches because being that the extract of different batches allocate；And its character is stable, uniform and easy to use.The moutan bark reference extract is upper in application, it is as in quality control of the control for moutan bark and medicinal material or Chinese medicine preparation containing moutan bark/moutan bark active ingredient, in this quality control procedure, it is that moutan bark 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, but also can be also used for sxemiquantitative even quantitative analysis.
Description
Technical field
The present invention relates to quality control technologies for traditional Chinese medicine fields, more particularly to a kind of moutan bark reference extract and its answer
With.
Background technology
Moutan bark is ranunculaceae peony dry root skin, has clearing heat and cooling blood, activates blood circulation and disperses blood clots, reducing the asthenic fever and other effects, main
Are produced from the ground such as Hunan, Hubei, Anhui, Sichuan, Gansu, Shaanxi, Shandong, Guizhou, wherein with the produced quality in Tongling, Anhui Province Feng huangshan Mountain
Most preferably.
Existing traditional Chinese medicine quality control pattern is substantially the development along Natural Medicine Chemistry, a certain or several to Chinese medicine
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 uses for reference the pattern of chemicals quality control, and establishes corresponding simple physics and chemistry by document report and differentiate, then
Develop to the discriminating based on spectrum, chromatography 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 indicates that one or two using in medicinal material even several ingredients as medicinal material matter
There are significant limitations for 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 can carry out quality control, currently still to medicinal material on the whole
There is very big researching value.Chinese Pharmacopoeia is there are two types of " reference substance " in terms of quality of medicinal material is controlled at present, and chemical reference substance is in
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
Past the phenomenon that having many loopholes, adulterating, happens occasionally.Chinese medicine control medicinal material is influenced be subject to the place of production, growing environment, it is difficult to
Ensure per batch of uniform quality, and be only used for Qualitive test, can not reflect the height of medicinal ingredient content.
Chinese medicine reference extract is the character and stable components prepared with Chinese medicine, can be used for qualitative or quantitative analysis
Extract, should possess several primary conditions there are four basic demand (ASCS) and reference extract：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 traditional Chinese medicine quality control important meaning
Justice.But also just since Chinese medicine reference extract has an above-mentioned specific requirement, currently available technology does not also have or does not have ripe
Pass through the moutan bark reference extract product being prepared using moutan bark medicinal material as raw material.
The content of the invention
The technical problem to be solved by the present invention is to provide a kind of batch uniformity is good, character is stable, uniform and easy to use
Moutan bark reference extract, the present invention also provides the applications of the moutan bark reference extract, i.e., compare the moutan bark
In quality control of the extract for moutan bark and medicinal material or Chinese medicine preparation containing moutan bark/moutan bark active ingredient.
One aspect of the present invention provides a kind of moutan bark reference extract, which is characterized in that it is derived from：To different batches
Moutan bark medicinal powder repeatedly extracted, the Cortex Moutan extract of different batches is obtained, then to the tree peony of different batches
Bark extract is allocated, and obtains moutan bark reference extract.
Preferably, the moutan bark medicinal powder to different batches is repeatedly extracted, and is the Paeoniflorin for containing it
The purity and/or concentration of constituents and root bark of tree peony phenols component improve, so as to obtain the Cortex Moutan extract of different batches.
Preferably, in the moutan bark reference extract Paeoniflorin content >=1.5%, content >=4.5% of Paeonol.
Preferably, the moutan bark reference extract is obtained using thin-layered chromatography and/or high performance liquid chromatography
The corresponding raw medicinal material of collection of illustrative plates is consistent.
Preferably, the Paeoniflorin in the chromatogram for thin-layered chromatography being used to detect the moutan bark reference extract
The chromatogram detected with the fluorescence spot at Paeonol position and using high performance liquid chromatography is in Paeoniflorin and Paeonol
Chromatographic peak at position should distinguish corresponding chemical reference substance or its corresponding raw medicinal material is consistent.
Another aspect of the present invention provides a kind of preparation method of moutan bark reference extract, comprises the following steps：
Step 1: extraction：The moutan bark medicinal powder of different batches is taken to be mixed respectively with ethyl alcohol, is filtered after homogenate extraction,
Obtain filtrate 1 and filter residue 1；
Step 2: cross column：It will concentrate and/or the filtrate 1 that does not concentrate by macroreticular resin and collected the extracting solution after column,
It is evaporated to obtain moutan bark dry cream；
Step 3: prepare Cortex Moutan extract：By gained moutan bark dry cream, ethyl alcohol is dissolved in, obtains moutan bark dry cream
Ethanol solution adds auxiliary material, is evaporated sieving and obtains Cortex Moutan extract；
Step 4: allotment：The Cortex Moutan extract of different batches is allocated, obtains moutan bark reference extract.
Preferably, the filter residue 1 described in the step 1 is extracted according to the extracting method of step 1 by n times, and by n times
The filtrate that extraction is collected merges with filtrate 1 Ji Wei extracting solution, and extracting solution is evaporated to obtain moutan bark dry cream；Wherein 8 >=N >=0, and
N is 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 60% that solution ethanol concentration is extracted in the step 1.
Preferably, the w/v of the moutan bark medicinal powder in the step 1 and ethyl alcohol is 1:1~1:20；
It is highly preferred that the w/v of the moutan bark medicinal powder and ethyl alcohol in the step 1 is 1：5；
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 filtered with Medium speed filter paper.
Preferably, in the step 2, concentration or the filtrate 1 not concentrated and the volume ratio of macroreticular resin are 10:1~1:
10, extracting solution is evaporated to obtain moutan bark dry cream；
It is highly preferred that the volume ratio of the filtrate 1 and macroreticular resin in the step 2 is 1:1；
It is highly preferred that the filtrate 1 is without concentration.
Preferably, the w/v of moutan bark dry cream and ethyl alcohol is 1 in the step 3:2~1:10；
Preferably, auxiliary material used is superfine silica gel powder and/or medical starch in the step 3；
Preferably, the step 3 be added in the ethanol solution of moutan bark dry cream its weight 10%~50% it is micro-
Powder silica gel；
Preferably, the step 3 is its weight is added in the ethanol solution of moutan bark dry cream 40% micro mist silicon
Glue；
Preferably, the step 3 is that 10%~30% medicine of its weight is added in the ethanol solution of moutan bark dry cream
Use starch；
Preferably, the step 3 is that 20% medicinal shallow lake of its weight is added in the ethanol solution of moutan bark dry cream
Powder；
Preferably, it was 90~200 mesh sieve net filtrations after the step 3 is evaporated；
Preferably, it was 200 mesh sieve net filtrations after the step 3 is evaporated；
Preferably, further included between the step 3 and step 4 with thin-layered chromatography and/or high performance liquid chromatography pair
The step of Paeoniflorin and Paeonol of the Cortex Moutan extract of different batches are detected.
Preferably, the standard allocated in the step 4 is：It should make containing for Paeoniflorin in the reference extract finally obtained
Amount >=1.5%, content >=4.5% of Paeonol.
Preferably, the moutan bark reference extract is obtained using thin-layered chromatography and/or high performance liquid chromatography
The corresponding raw medicinal material of collection of illustrative plates is consistent.
Preferably, the Paeoniflorin in the chromatogram for thin-layered chromatography being used to detect the moutan bark reference extract
The chromatogram detected with the fluorescence spot at Paeonol position and using high performance liquid chromatography is in Paeoniflorin and Paeonol
Chromatographic peak at position should distinguish corresponding chemical reference substance or its corresponding raw medicinal material is consistent.
Another aspect of the invention provides discriminating or tree peony of a kind of moutan bark reference extract in medicinal material or Chinese medicine preparation
Application in the quality control of skin or medicinal material or Chinese medicine preparation containing moutan bark/moutan bark active ingredient.
Preferably, the discriminating of the medicinal material or Chinese medicine preparation or moutan bark and containing in moutan bark/moutan bark active ingredient
The method of the quality control of medicine preparation is：By moutan bark reference extract, medicinal material or the Chinese medicine preparation with thin-layered chromatography
And/or high performance liquid chromatography is detected, comparison differentiates.
Preferably, the thin-layered chromatography and/or high performance liquid chromatography be to moutan bark reference extract, medicinal material or in
Paeoniflorin and Paeonol in medicine preparation are detected.
Preferably, it is detected when by moutan bark reference extract, medicinal material or the Chinese medicine preparation with thin-layered chromatography
When, it is necessary to which moutan bark reference extract, medicinal material or Chinese medicine preparation are configured to solution carries out thin-layered chromatography detection again；
The preparation method of wherein moutan bark reference extract solution is：The moutan bark reference extract is added in into its matter
The ethyl alcohol of 10-500 times of volume is measured, is ultrasonically treated, shakes up, crosses 0.12-0.32 μm of filter membrane up to moutan bark reference extract solution.
Preferably, the moutan bark reference extract is added in the ethyl alcohol of its 200 times of volume of quality, ultrasonic 500w processing
It 30 minutes, shakes up, crosses 0.22 μm of filter membrane up to moutan bark reference extract solution；
The preparation method of its Chinese medicine or Chinese medicine preparation solution is：It gets it filled material or Chinese medicine preparation adds in 10-150 times of its quality
The ethyl alcohol of volume centrifuges after supersound process, supernatant is taken to cross 0.12-0.32 μm of filter membrane up to medicinal material or Chinese medicine preparation solution.
Preferably, getting it filled material or Chinese medicine preparation adds in the ethyl alcohol of its 100 times of volume of quality, ultrasonic 500w is handled 15 minutes,
3200 revs/min centrifuge 3 minutes, and supernatant is taken to cross 0.22 μm of filter membrane up to medicinal material or Chinese medicine preparation solution.
Preferably, the thin-layered chromatography testing conditions are：
Lamellae：HPTLC F254 prefabricated boards；
Point sample：0.5 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 be placed in phosphorus pentoxide vacuum desiccator 2 it is small when, ensure lamellae
It is dry；
It inspects:Spray is first placed under 254nm fluorescence and inspected, then be placed in white with -10% sulfuric acid ethyl alcohol color developing agent of 5% vanillic aldehyde
It is inspected under vehement light.
Preferably, carried out when by moutan bark reference extract, medicinal material or the Chinese medicine preparation with high performance liquid chromatography
, it is necessary to which moutan bark reference extract, medicinal material or Chinese medicine preparation are configured to solution carries out high performance liquid chromatography inspection again during detection
It surveys；
The preparation method of wherein moutan bark reference extract solution is：Precision weighs the moutan bark reference extract, adds
Enter 50% EtOH Sonicate to extract 30 minutes, constant volume, be configured to the solution of 5mg/ml concentration, cross 0.22 μm of filter membrane, take subsequent filtrate
As extract reference substance solution.
The preparation method of its Chinese medicine or Chinese medicine preparation solution is：It gets it filled material or Chinese medicine preparation crosses weighed 2g after No. two sieves,
It puts in 50ml conical flask with cover, precision adds in ethanol solution 45ml, after water-bath reflux 1h, lets cool, and adds ethyl alcohol at scale 50ml,
It shakes up, crosses 0.22 μm of filter membrane, take subsequent filtrate up to medicinal material or Chinese medicine preparation solution.
Preferably, the high performance liquid chromatography testing conditions：
Chromatographic apparatus：1260 series high performance liquid chromatographs of Agilent, 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, 280nm (DAD detectors)；Flow velocity 0.8ml/min；10 μ l of sample size；25 DEG C of column temperature, operation
Time：65min.
Advantageous effect
The moutan bark reference extract of the present invention is overcome because being that the extract of different batches allocate because of Chinese medicine
Control medicinal material is influenced be subject to 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 difference
The uniformity of the moutan bark reference extract of batch；And its character is stable, uniform and easy to use.The moutan bark control carries
Take object upper in application, be by moutan bark reference extract after quantitative analysis, as control for moutan bark and containing moutan bark/
It is to compare moutan bark in this quality control procedure in the quality control of the medicinal material or Chinese medicine preparation of moutan bark active ingredient
Extract carries out simple process and can be used directly, easy to operate, especially in multicomponent assay, reference extract solution
Preparation it is easier than the preparation of chemical reference substance solution, Qualitive test can be not only carried out to medicinal material or Chinese medicine preparation, and
And it can be also used for sxemiquantitative even quantitative analysis.
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 purposes,
Feature and other advantages, wherein,
Fig. 1 is moutan bark reference extract preparation flow figure；
Fig. 2 is to be directed to carry out thin layer color to commercially available medicinal material as reference substance using chemical reference substance and moutan bark reference extract
The high performance thin layer chromatography figure that spectrometry obtains, the wherein chromatographic band of label 1 are corresponding in turn to from lower to upper as reference substance Paeoniflorin, catechu
Element, benzoyl oxypaeoniflorin, benzoylpaeoniflorin and Paeonol, 2-9 be corresponding in turn to moutan bark 1, moutan bark 2, moutan bark 3,
Moutan bark 4, moutan bark 5, moutan bark 6, the medicinal material of moutan bark 7 and moutan bark 8,10 correspond to moutan bark reference extract；
Fig. 3 is to be directed to carry out efficient liquid to commercially available medicinal material as reference substance using chemical reference substance and moutan bark reference extract
The HPLC finger-print stacking charts that phase chromatography obtains, from top to bottom, R correspond to common pattern, and S corresponds to moutan bark control extraction
Object, 1-8 correspond to moutan bark 1, moutan bark 2, moutan bark 3, moutan bark 4, moutan bark 5, moutan bark 6, moutan bark 7 and moutan bark respectively
8 medicinal materials；
Fig. 4 is the finger-print common pattern collection of illustrative plates for the moutan bark medicinal material established, wherein No. 15 chromatographic peaks are gallic acid,
No. 48 chromatographic peaks are Paeoniflorin, and No. 64 chromatographic peaks are Penta-O-galloyl-D-glucopyranose, and No. 99 chromatographic peaks are benzoylpaeoniflorin, 107
Number chromatographic peak is Paeonol.
Specific embodiment
The embodiment of the present invention is described below in detail.The embodiments described below is exemplary, and is only used for explaining this hair
It is bright, and be not considered as limiting the invention.Particular technique or condition are not specified in embodiment, according to text in the art
It offers described technology or condition or is carried out according to product description.Reagents or instruments used without specified manufacturer,
For can be with conventional products that are commercially available.Term as used herein "and/or" includes one or more relevant listed
The arbitrary and all combination of project.
The instrument used in following embodiment and the source of material are as follows：
It is envisaged for preparing the medicinal material of reference extract:Moutan bark (Anhui).
The semi-automatic point sample instrument of 5 thin-layer chromatographys of Linomat, the full-automatic point sample instrument of 4 thin-layer chromatographys of ATS, thin-layer chromatography double flute
Expansion cylinder, Chromatogram Immersion Device III chromatography colour developing dipping tanks and TLC visualizer thin layers
Chromatography video camera (Switzerland, CAMAG).
1260 series high performance liquid chromatographs of Agilent, 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 chromatographically pure (Merck KGaA).
Paeoniflorin, Paeonol indicate purity >=98%, (Baoji time bio tech ltd).
Test medicinal material moutan bark：
The 8 batches of buyings of moutan bark medicinal material are in Guangzhou medicinal material market.
Embodiment 1：The preparation of moutan bark reference extract
The preparation method of moutan bark reference extract of the present invention is present embodiments provided, method flow diagram is as shown in Figure 1.
One：Extraction
Choose moutan bark medicinal material (Anhui, genunie medicinal materials), be made powder, medicinal powder cross No. two sieves (850 ± 29 μm, 24
Mesh), then add in its 3.5 times of volume of quality ethyl alcohol (i.e. solid-to-liquid ratio be 1：3.5 (w/V)), ultrasonic (power 500w, room temperature) carries
Middling speed qualitative filter paper after 30min is taken to filter, collects filter residue 1 and filtrate 1, filter residue 1 extracted again by same procedure it is secondary, and will again
The filtrate of the secondary secondary collection of extraction merges with filtrate 1 Ji Wei extracting solution, and extracting solution solvent evaporated is got dry extract；
Two：Prepare Cortex Moutan 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 Cortex Moutan extract.
4 batches of Cortex Moutan extracts are prepared, high effective liquid chromatography for measuring, testing result such as 1 institute of table are utilized by reference substance
Show：
Table 1
Three：Allotment
The Cortex Moutan extract of 4 batches of step 2 is pressed 1:1 mixing blends to obtain moutan bark reference extract, finally
It is about 1 that product, which corresponds to crude drug ratio,：2 (g/g), by reference substance using high effective liquid chromatography for measuring, wherein each ingredient
Content measurement result it is as shown in Figure 2.
Table 2
Allotment standard is：Should make content >=1.5% of Paeoniflorin, Paeonol in final moutan bark reference extract >=
4.5% (content is in terms of wt%).The scope of the content of each ingredient in this allotment standard is also by repeatedly experiment integrates repeatedly
The optimum data that stability, uniformity and application below etc. is kept to draw.
The character analysis of 2 moutan bark reference extract of embodiment
1. apparent state：The moutan bark reference extract that embodiment 1 obtains is yellowish-white powder.
2. determination of moisture：It is carried out according to 2015 editions Chinese Pharmacopoeia annex IX G (hypobaric drying method).Testing result is tree peony
Skin reference extract water content is 3.1%.
3. uniformity test：14 batch moutan bark reference extracts are prepared according to the method for embodiment 1, after measured each batch
Between for Paeoniflorin, the thin-layer chromatography testing result difference very little of Paeonol, the fluorescence spot of Paeoniflorin and Paeonol has
Apparent display, and be distributed very consistent；Through its Paeoniflorin of high performance liquid chromatography detection and paeonol content in allotment standard
Within the scope of.Therefore the moutan bark reference extract being prepared using the preparation method of the moutan bark reference extract of the present invention
Uniformity is very good.
4. stability test：
The test sample of the moutan bark reference extract of the method preparation according to embodiment 1 of 4 different batches is taken, according to state
Family pharmacopoeia commission work out " requirement of national drug standards substance Development Techniques " relevant regulations, inspection target include character with
Dissolubility.
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,
It is detected by stability high spot reviews project.
The results show that 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, and result of calculation P ＞ 0.05 illustrate no conspicuousness
Difference.
Comparative example 1
With embodiment 1 difference lies in：
To in the step one in embodiment 1 methanol being used to be carried out instead of ethyl alcohol, the content of the moutan bark dry cream finally obtained
Significantly lower than embodiment 1, it can be seen that, yield of the value substantially than ethyl alcohol extraction is much lower, only increases extracted amount or secondary
Number is possible to reach within allotment critical field.
Embodiment 3
Present embodiments provide the application for the moutan bark reference extract that embodiment 1 is prepared.
With thin-layered chromatography and high performance liquid chromatography respectively using chemical reference substance and moutan bark reference extract as ginseng
Commercially available medicinal material is analyzed according to substance.
1 thin-layer chromatography
1.1 sample preparation
Chemical reference substance solution：Precision weighs Paeoniflorin and Paeonol respectively, is configured to the molten of 1mg/ml respectively with methanol
Liquid.
Moutan bark reference extract solution：Precision weighs the moutan bark reference extract 0.2g that embodiment 1 is prepared, and adds
Enter ethyl alcohol 10ml, ultrasonic (500w) is handled 15 minutes, shaken up, and crosses 0.22 μm of filter membrane up to moutan bark reference extract solution.
Medicinal material test solution：Get it filled each 1g of shop medicinal material, adds in ethyl alcohol 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 0.22 μm of filter membrane up to medicinal material test solution.Pharmacy's medicinal material is equal
It buys from Guangzhou, is respectively：Moutan bark 1, moutan bark 2, moutan bark 3, moutan bark 4, moutan bark 5, moutan bark 6, moutan bark 7 and tree peony
Skin 8.
1.2 thin-layer chromatographys detect
Testing conditions are as follows：
Lamellae：HPTLC F254 prefabricated boards (Merck)；
Point sample：2 μ l and 5 μ l, the long 8mm of ribbon point sample；
Solvent：Jia Ben ︰ Yi Suan Yi Zhi ︰ Jia Chun ︰ Shui ︰ glacial acetic acid=10 ︰, 7 ︰, 5 ︰, 0.5 ︰ 0.1；
Expansion mode：Add solvent 12ml, common pre-equilibration 15 minutes in one side in double flute expansion cylinder (20cm × 10cm)；
The drying of lamellae：Lamellae after point sample be placed in phosphorus pentoxide vacuum desiccator 2 it is small when, ensure lamellae
It is dry；
It inspects:It is first placed under 254nm fluorescence and inspects, then spray with -10% sulfuric acid ethyl alcohol of 5% vanillic aldehyde, be placed under incandescence
It inspects.
Testing result under incandescence as shown in Fig. 2, to inspect thin-layer chromatogram (T：27 DEG C, RH：66%).The color of label 1
Bands of a spectrum are arranged from lower to upper to be corresponding in turn to as reference substance Paeoniflorin, catechin, benzoyl oxypaeoniflorin, benzoylpaeoniflorin and pellet
Skin phenol, 2-9 are corresponding in turn to moutan bark 1, moutan bark 2, moutan bark 3, moutan bark 4, moutan bark 5, moutan bark 6, moutan bark 7 and tree peony
The medicinal material of skin 8,10 correspond to moutan bark reference extract.
Interpretation of result：As shown in Figure 2, Paeoniflorin, catechin, benzoyl oxypaeoniflorin, benzoylpaeoniflorin, Paeonol
Separation situation is preferable, and moutan bark reference extract and medicinal material (moutan bark 1- moutan barks 8) can show identical in same position
Spot, find out that moutan bark reference extract and medicinal material (moutan bark 1- moutan barks 8) have the uniformity of height from collection of illustrative plates.
2 high performance liquid chromatography
2.1 sample preparation
Chemical reference substance solution：Precision weighs Paeoniflorin 5mg, Paeonol 5mg reference substances, is configured to respectively with methanol
The solution of 0.5mg/ml, 1.0mg/ml concentration.
Moutan bark reference extract solution：Precision weighs Cortex Moutan extract 0.2g, adds at 50% EtOH Sonicate 500w
Reason 30 minutes, constant volume are configured to the solution of 5mg/ml concentration, cross 0.22 μm of filter membrane, take subsequent filtrate molten as extract reference substance
Liquid；
Medicinal material test solution：Each batch of medicinal powder crosses No. two sieves, and accurately weighed each 2g is put in 50ml conical flask with cover,
50% ethanol solution 45ml is added in, water-bath flows back after 1h, filters into 50ml volumetric flasks, let cool by fast grade filter paper, add ethyl alcohol
It at constant volume scale 50ml, shakes up, crosses 0.22 μm of filter membrane, take subsequent filtrate up to medicinal material solution.Each batch of medicinal material is bought from Guangzhou, point
It is not：Moutan bark 1, moutan bark 2, moutan bark 3, moutan bark 4, moutan bark 5, moutan bark 6, moutan bark 7 and moutan bark 8.
2.2 high performance liquid chromatography detection
High performance liquid chromatography testing conditions are as follows：
Chromatographic apparatus：1260 series high performance liquid chromatographs of Agilent, 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, 280nm (DAD detectors)；Flow velocity 0.8ml/min；10 μ l of sample size；25 DEG C of column temperature, operation
Time：65min.
High effective liquid chromatography for detecting：Accurate absorption chemical reference substance solution, moutan bark reference extract are molten respectively
Liquid and each 10 μ l of medicinal material test solution inject liquid chromatograph.
High performance liquid chromatography testing result：
It measures, record chromatogram is to get HPLC finger-prints stacking chart shown in Fig. 3, and from top to bottom, it is right that R corresponds to chemistry
According to product, S corresponds to moutan bark reference extract, and 1-8 corresponds to moutan bark 1, moutan bark 2, moutan bark 3, moutan bark 4, moutan bark respectively
5th, moutan bark 6, moutan bark 7 and moutan bark 8.
As seen from Figure 3, the finger-print of 8 medicinal material of moutan bark 1- moutan barks has high consistency, thus in accordance with
Pharmacopoeia of People's Republic of China committee similarity evaluation (2012.130723 version) is established male
The finger-print common pattern of root bark of tree peony medicinal material, and similarity analysis is carried out to all samples.Common pattern collection of illustrative plates as shown in figure 4,
Wherein No. 15 chromatographic peaks are gallic acid, and No. 48 chromatographic peaks are Paeoniflorin, and No. 64 chromatographic peaks are Penta-O-galloyl-D-glucopyranose, No. 99
Chromatographic peak is benzoylpaeoniflorin, and No. 107 chromatographic peaks are Paeonol.
According to set moutan bark medicinal materials fingerprint common pattern, using included angle cosine algorithm according to each sample component and
Its peak area carries out similarity evaluation to 8 batches of moutan bark medicinal materials and reference extract sample, and the results are shown in Table 3.
Table 3
| Sample | Similarity |
| Moutan bark 1 | 0.999 |
| Moutan bark 2 | 0.984 |
| Moutan bark 3 | 0.999 |
| Moutan bark 4 | 0.990 |
| Moutan bark 5 | 0.999 |
| Moutan bark 6 | 0.990 |
| Moutan bark 7 | 0.999 |
| Moutan bark 8 | 0.935 |
| Moutan bark reference extract | 0.999 |
According to more than similarity analysis as a result, the similarity of 8 batches of medicinal materials and moutan bark medicinal materials fingerprint common pattern exists
In the range of 0.935-0.999, similarity is very high.The phase of moutan bark reference extract and moutan bark medicinal materials fingerprint common pattern
It is 0.999 like degree, shows that the uniformity of moutan bark reference extract of the invention and medicinal material is good.
According to the result of TLC and HPLC finger-prints, thin-layered chromatography is used to the moutan bark reference extract
It is consistent to detect the corresponding raw medicinal material of obtained chromatogram, more precisely, the moutan bark reference extract is used
Fluorescence spot at Paeoniflorin and Paeonol position in the chromatogram that thin-layered chromatography detects and using high-efficient liquid phase color
Chromatographic peak of the chromatogram that spectrometry detects at Paeoniflorin and Paeonol position distinguish corresponding chemical reference substance or
Its corresponding raw medicinal material is consistent, therefore the moutan bark reference extract of the present invention can be applied to the qualitative of medicinal material or Chinese medicine preparation
Differentiate, such as qualitative analysis is carried out to the Paeoniflorin ingredient of medicinal material or Chinese medicine preparation.
According to HPLC measurement results and statistical analysis, the moutan bark medicinal materials fingerprint common pattern and moutan bark of foundation
The similarity of medicinal material is high, and the present invention moutan bark reference extract and moutan bark medicinal materials fingerprint common pattern it is similar
Degree is again high, this explanation carries out Paeoniflorin and Paeonol using the moutan bark reference extract of the present invention to medicinal material or Chinese medicine preparation
Assay reliability it is high, therefore the moutan bark reference extract of the present invention can be applied to the semidefinite of medicinal material or Chinese medicine preparation
Discriminatory analysis is measured, can also be applied to the quality control of moutan bark and the medicinal material containing moutan bark/moutan bark active ingredient or Chinese medicine preparation
In system, such as sxemiquantitative discriminatory analysis is carried out or to moutan bark to the Paeoniflorin and Paeonol ingredient of medicinal material or Chinese medicine preparation
And medicinal material containing moutan bark/moutan bark active ingredient or Chinese medicine preparation carry out half-quantitative detection and then control its quality.
The foregoing is merely the better embodiments of the present invention, are not intended to limit the invention, all the present invention's
All any modification, equivalent and improvement made within spirit and principle etc., should all be included in the protection scope of the present invention.
Claims (11)
1. a kind of moutan bark reference extract, which is characterized in that it is derived from：The moutan bark medicinal powder of different batches is carried out
Repeatedly extraction, obtains the Cortex Moutan extract of different batches, then the Cortex Moutan extract of different batches is allocated, is obtained
Moutan bark reference extract；
Optional, the moutan bark medicinal powder to different batches is repeatedly extracted, be the Chinese herbaceous peony glycoside that contains it into
Divide and improved with the purity of root bark of tree peony phenols component and/or concentration, so as to obtain the Cortex Moutan extract of different batches；
Optional, content >=1.5% of Paeoniflorin, content >=4.5% of Paeonol in the moutan bark reference extract.
2. a kind of preparation method of moutan bark reference extract described in claim 1, comprises the following steps：
Step 1: extraction：The moutan bark medicinal powder of different batches is taken to be mixed respectively with ethyl alcohol, filters, obtains after homogenate extraction
Filtrate 1 and filter residue 1；
Step 2: cross column：It will concentrate and/or the filtrate 1 that does not concentrate by macroreticular resin and collected the extracting solution after column, be evaporated
Obtain moutan bark dry cream；
Step 3: prepare Cortex Moutan extract：By gained moutan bark dry cream, ethyl alcohol is dissolved in, obtains the ethyl alcohol of moutan bark dry cream
Solution adds auxiliary material, is evaporated sieving and obtains Cortex Moutan extract；
Step 4: allotment：The Cortex Moutan extract of different batches is allocated, obtains moutan bark reference extract.
3. the preparation method of moutan bark reference extract according to claim 2, which is characterized in that institute in the step 1
The filter residue 1 stated is extracted according to the extracting method of step 1 by n times, and the filtrate that n times extraction is collected merge with filtrate 1 as
Extracting solution is evaporated to obtain moutan bark dry cream by extracting solution；Wherein 8 >=N >=0, and N is integer；
Optional, the N is 3.
4. the preparation method of moutan bark reference extract according to claim 2, which is characterized in that institute in the step 1
The extraction solution ethanol concentration stated is 30%~95%；
Optional, it is 60% that solution ethanol concentration is extracted in the step 1.
5. the preparation method of moutan bark reference extract according to claim 3, which is characterized in that in the step 1
The w/v of moutan bark medicinal powder and ethyl alcohol is 1:1~1:20；
Optional, the w/v of moutan bark medicinal powder and ethyl alcohol in the step 1 is 1:5；
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 moutan bark reference extract according to claim 2, which is characterized in that in the step 2,
Concentration or the filtrate 1 not concentrated and the volume ratio of macroreticular resin are 10:1~1:10, extracting solution is evaporated to obtain moutan bark dry cream；
Optional, the volume ratio of filtrate 1 and macroreticular resin in the step 2 is 1:1；
Optional, the filtrate 1 is without concentration.
7. the preparation method of moutan bark reference extract according to claim 3, which is characterized in that male in the step 3
The w/v of root bark of tree peony dry cream and ethyl alcohol：1:2~1:10；
Optional, the auxiliary material is superfine silica gel powder and/or medical starch；
Optional, the step 3 is its weight is added in the ethanol solution of moutan bark dry cream 10%~50% micro mist silicon
Glue；
Optional, the step 3 is that 40% superfine silica gel powder of its weight is added in the ethanol solution of moutan bark dry cream；
Optional, the step 3 is that 10%~30% medicinal shallow lake of its weight is added in the ethanol solution of moutan bark dry cream
Powder；
Optional, the step 3 is that 20% medical starch of its weight is added in the ethanol solution of moutan bark dry cream；
It is optional, the step 3 be evaporated after be 90~200 mesh sieve net filtrations；
It is optional, the step 3 be evaporated after be 200 mesh sieve net filtrations；
Optional, it is further included between the step 3 and step 4 with thin-layered chromatography and/or high performance liquid chromatography to difference
The step of Paeoniflorin and Paeonol of the Cortex Moutan extract of batch are detected.
8. the preparation method of moutan bark reference extract according to claim 3, which is characterized in that adjusted in the step 4
The standard matched somebody with somebody is：It should make content >=4.5% of content >=1.5% of Paeoniflorin, Paeonol in the reference extract finally obtained.
9. moutan bark reference extract described in claim 1 is in the discriminating of medicinal material or Chinese medicine preparation or moutan bark or containing tree peony
Application in the quality control of the medicinal material or Chinese medicine preparation of skin/moutan bark active ingredient；
It is optional, the discriminating of the medicinal material or Chinese medicine preparation or moutan bark and the Chinese medicine system containing moutan bark/moutan bark active ingredient
The method of the quality control of agent is：By moutan bark reference extract described in claim 1, medicinal material or Chinese medicine preparation with thin layer color
Spectrometry and/or high performance liquid chromatography are detected, and comparison differentiates；
Optional, the thin-layered chromatography and/or high performance liquid chromatography are to moutan bark reference extract, medicinal material or Chinese medicine system
Paeoniflorin and Paeonol in agent are detected.
10. application according to claim 9, which is characterized in that when by moutan bark reference extract described in claim 1, medicine
, it is necessary to which moutan bark reference extract, medicinal material or Chinese medicine preparation are prepared when material or Chinese medicine preparation are detected with thin-layered chromatography
Thin-layered chromatography detection is carried out again into solution；
The preparation method of wherein moutan bark reference extract solution is：Moutan bark reference extract described in claim 1 is added
Enter the ethyl alcohol of 10-500 times of volume of its quality, be ultrasonically treated, shake up, cross 0.12-0.32 μm of filter membrane and compare extraction up to moutan bark
Object solution；
It is optional, the moutan bark reference extract is added in the ethyl alcohol of its 200 times of volume of quality, ultrasonic 500w handles 30 points
Clock shakes up, and crosses 0.22 μm of filter membrane up to moutan bark reference extract solution；
The preparation method of its Chinese medicine or Chinese medicine preparation solution is：It gets it filled material or Chinese medicine preparation adds in 10-150 times of volume of its quality
Ethyl alcohol, centrifuge after supersound process, supernatant taken to cross 0.12-0.32 μm of filter membrane up to medicinal material or Chinese medicine preparation solution；
It is optional, it gets it filled material or Chinese medicine preparation adds in the ethyl alcohol of its 100 times of volume of quality, ultrasonic 500w handles 15 minutes, and 3200
Rev/min centrifugation 3 minutes, supernatant is taken to cross 0.22 μm of filter membrane up to medicinal material or Chinese medicine preparation solution；
Optional, the thin-layered chromatography testing conditions are：
Lamellae：HPTLC F254 prefabricated boards；
Point sample：0.5 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 be placed in phosphorus pentoxide vacuum desiccator 2 it is small when, ensure the dry of lamellae
It is dry；
It inspects:Spray is first placed under 254nm fluorescence and inspected, then be placed in incandescence with -10% sulfuric acid ethyl alcohol color developing agent of 5% vanillic aldehyde
Under inspect.
11. application according to claim 9, which is characterized in that when by moutan bark reference extract described in claim 1, medicine
When material or Chinese medicine preparation are detected with high performance liquid chromatography, it is necessary to by moutan bark reference extract, medicinal material or Chinese medicine preparation
It is configured to solution and carries out high performance liquid chromatography detection again；
The preparation method of wherein moutan bark reference extract solution is：Precision weighs moutan bark control extraction described in claim 1
Object adds in 50% EtOH Sonicate and extracts 30 minutes, constant volume, is configured to the solution of 5mg/ml concentration, crosses 0.22 μm of filter membrane, takes continuous
Filtrate is as extract reference substance solution；
The preparation method of its Chinese medicine or Chinese medicine preparation solution is：It gets it filled material or Chinese medicine preparation crosses weighed 2g after No. two sieves, put
In 50ml conical flask with cover, precision adds in ethanol solution 45ml, after water-bath reflux 1h, lets cool, ethyl alcohol is added to be shaken at scale 50ml
It is even, 0.22 μm of filter membrane is crossed, takes subsequent filtrate up to medicinal material or Chinese medicine preparation solution；
Optional, described high performance liquid chromatography testing conditions：
Chromatographic apparatus：1260 series high performance liquid chromatographs of Agilent, 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, 280nm (DAD detectors)；Flow velocity 0.8ml/min；10 μ l of sample size；25 DEG C of column temperature, during operation
Between：65min.
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| CN113514596A (en) * | 2021-04-28 | 2021-10-19 | 广州科曼生物科技有限公司 | Small and medium polarity control extract of wolfberry fruit and preparation method and application thereof |
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