CN106226451A - The discrimination method of Rhizoma Chuanxiong in ostealgia medicated wine - Google Patents
The discrimination method of Rhizoma Chuanxiong in ostealgia medicated wine Download PDFInfo
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- 206010006002 Bone pain Diseases 0.000 title claims abstract description 37
- 238000012850 discrimination method Methods 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 67
- OAYLNYINCPYISS-UHFFFAOYSA-N ethyl acetate;hexane Chemical compound CCCCCC.CCOC(C)=O OAYLNYINCPYISS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 16
- 238000012360 testing method Methods 0.000 claims description 78
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 68
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 64
- 238000002360 preparation method Methods 0.000 claims description 22
- 239000000047 product Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000284 extract Substances 0.000 claims description 14
- 239000000741 silica gel Substances 0.000 claims description 14
- 229910002027 silica gel Inorganic materials 0.000 claims description 14
- 239000003814 drug Substances 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 3
- -1 filters Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 239000002893 slag Substances 0.000 claims 1
- 238000001228 spectrum Methods 0.000 claims 1
- 239000002023 wood Substances 0.000 claims 1
- 239000013642 negative control Substances 0.000 abstract description 9
- 230000002349 favourable effect Effects 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000007689 inspection Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 31
- 229940093499 ethyl acetate Drugs 0.000 description 16
- 239000007788 liquid Substances 0.000 description 13
- 239000003795 chemical substances by application Substances 0.000 description 8
- 239000008280 blood Substances 0.000 description 7
- 210000004369 blood Anatomy 0.000 description 7
- 208000002193 Pain Diseases 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 238000011835 investigation Methods 0.000 description 3
- 239000012567 medical material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000903946 Clematidis Species 0.000 description 2
- 241000628997 Flos Species 0.000 description 2
- 241000244365 Ligusticum sinense Species 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 2
- 235000011613 Pinus brutia Nutrition 0.000 description 2
- 241000018646 Pinus brutia Species 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005325 percolation Methods 0.000 description 2
- 239000013558 reference substance Substances 0.000 description 2
- 208000006820 Arthralgia Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010020880 Hypertrophy Diseases 0.000 description 1
- 235000011158 Prunus mume Nutrition 0.000 description 1
- 244000018795 Prunus mume Species 0.000 description 1
- 208000025747 Rheumatic disease Diseases 0.000 description 1
- 241000209051 Saccharum Species 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 230000002308 calcification Effects 0.000 description 1
- 210000000845 cartilage Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000552 rheumatic effect Effects 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 210000002435 tendon Anatomy 0.000 description 1
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- General Health & Medical Sciences (AREA)
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- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
Abstract
The invention discloses the discrimination method of Rhizoma Chuanxiong in a kind of ostealgia medicated wine, be with Rhizoma Chuanxiong control medicinal material for comparison, with ethyl acetate hexane=8～12 1～2 thin layer chromatography as developing solvent.The discrimination method of Rhizoma Chuanxiong in a kind of ostealgia medicated wine that the present invention provides, it is capable of the Rhizoma Chuanxiong differentiating in ostealgia medicated wine efficiently and accurately, simple to operate, controllability is high, and separating degree is high, highly sensitive, precision, good stability, favorable reproducibility, and negative control is noiseless, and different manufacturers lamellae and temperature, damp condition do not affect.Discrimination method of the present invention can carry out effective discriminating accurate, comprehensive, scientifical to Rhizoma Chuanxiong composition in ostealgia medicated wine, improves quality inspection standard, further ensure that the stable, safely, effectively of product quality.
Description
Technical field
The present invention relates to the discrimination method of Rhizoma Chuanxiong in ostealgia medicated wine, particularly belong to Chinese medicine detection technique field.
Background technology
Ostealgia medicated wine be by Radix Aconiti Kusnezoffii Preparata, Herba Taxilli, Radix Schefflerae Arboricolae (Caulis et Folium Schefflerae Arboricolae), Radix Clematidis, Rhizoma Polygoni Cuspidati, Caulis Trachelospermi, Rhizoma Smilacis Chinensis, Rhizoma Atractylodis (parched with bran),
Pine Nodular Branch, Radix Polygoni Multiflori Preparata, Caulis Sargentodoxae, Radix Salviae Miltiorrhizae, Ramulus Sambuci Williamsii, Herba Lycopodii, Fructus Chaenomelis, Rhizoma Chuanxiong, Radix Achyranthis Bidentatae, Herba Ephedrae, Cortex Periplocae, Flos Carthami, Radix Dipsaci
Make with Rhizoma Zingiberis.Ostealgia medicated wine has dispelling wind and relieving pain, relaxing muscles and tendons and activating QI and blood in the collateral effect, efficacy enhanced by wine, and wine helps medicine prestige, can quickly get through more
Resistance, unimpeded blood vessel, meridians, dissolve the blood stasis on cartilage, split adhesion organization, just as dissolving ice cube, gradually decompose calcification
The hypertrophy bony spur of deformation.In the quality standard of existing ostealgia medicated wine, its content only has medicated wine routine examination project, it is difficult to effectively
Ground controls drug quality.In ostealgia medicated wine side, Rhizoma Chuanxiong is principal agent, differentiates it, beneficially the quality control of ostealgia medicated wine.
Therefore, study and a kind of differentiate the method for Rhizoma Chuanxiong in ostealgia medicated wine, it appears be particularly necessary.
Summary of the invention
For solving the deficiencies in the prior art, it is an object of the invention to provide the discriminating side of Rhizoma Chuanxiong in a kind of ostealgia medicated wine
Method, it is possible to differentiating the Rhizoma Chuanxiong in ostealgia medicated wine efficiently, accurately, separating degree is good.
Ostealgia medicated wine in the present invention, be by Radix Aconiti Kusnezoffii Preparata 50g, Herba Taxilli 50g, Radix Schefflerae Arboricolae (Caulis et Folium Schefflerae Arboricolae) 50g, Caulis Trachelospermi 25g, Radix Salviae Miltiorrhizae 25g,
Pine Nodular Branch 37.5g, Fructus Chaenomelis 25g, Herba Ephedrae 12.5g, Radix Clematidis 25g, Rhizoma Polygoni Cuspidati 37.5g, Rhizoma Smilacis Chinensis 25g, Rhizoma Zingiberis 6.25g, Radix Polygoni Multiflori Preparata
25g, Caulis Sargentodoxae 37.5g, Ramulus Sambuci Williamsii 50g, Herba Lycopodii 12.5g, Rhizoma Chuanxiong 12.5g, Radix Achyranthis Bidentatae 50g, Cortex Periplocae 50g, Flos Carthami 12.5g,
Radix Dipsaci 50g and Rhizoma Atractylodis (parched with bran) 12.5g makes.Above 22 tastes, are ground into coarse powder, according under fluid extract and extractum item
Percolation (" Chinese Pharmacopoeia " version general rule 0189 in 2015), make solvent by wine sugar liquid and (take Saccharum Sinensis Roxb. 430g, be dissolved in Chinese liquor
In 4300g), after impregnating 48 hours, with the speed slowly percolation of per kilogram crude drug 1～3mL per minute, collect percolate, stand,
Filter, to obtain final product.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that:
The discrimination method of Rhizoma Chuanxiong in ostealgia medicated wine, is with Rhizoma Chuanxiong control medicinal material for comparison, with n-hexane-ethyl acetate=8
～12 1～2 be the thin layer chromatography of developing solvent.
The discrimination method of Rhizoma Chuanxiong in aforementioned ostealgia medicated wine, comprises the following steps:
(1) preparation of need testing solution: take this product add diethyl ether shaking extract, obtain ether solution, volatilize, residue adds ethyl acetate
It is made to dissolve, as need testing solution；
(2) preparation of control medicinal material solution: taking Rhizoma Chuanxiong control medicinal material 0.5g, add diethyl ether reflux, extract, filters, and filtrate is waved
Dry, residue adds ethyl acetate 1mL makes it dissolve, as control medicinal material solution；
(3) differentiate: according to four the general rule 0502 thin layer chromatography tests of " Chinese Pharmacopoeia " version in 2015, draw control medicinal material molten
Liquid, need testing solution, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate=8～12 1～2 for launching
Agent, launch, take out, dry, put and inspect under 365nm ultra-violet lamp, in test sample chromatograph, with control medicinal material chromatograph relevant position
On, the fluorescence principal spot of aobvious same color.
Specifically, the discrimination method of Rhizoma Chuanxiong in aforementioned ostealgia medicated wine, comprise the following steps:
(1) preparation of need testing solution: take this product 20mL～25mL, adds diethyl ether 20～30mL every time, and shaking extracts 2～3
Secondary, merge ether solution, volatilize, residue adds 1～3mL ethyl acetate makes it dissolve, as need testing solution；
(2) preparation of control medicinal material solution: take Rhizoma Chuanxiong control medicinal material 0.5g, add 15mL～20mL aether backflow extract 1～
2h, filters, and filtrate volatilizes, and residue adds ethyl acetate 1mL makes it dissolve, as control medicinal material solution；
(3) differentiate: according to four the general rule 0502 thin layer chromatography tests of " Chinese Pharmacopoeia " version in 2015, draw control medicinal material molten
Liquid 8～12 μ L, need testing solution 8 μ L～12 μ L, put on same silica gel g thin-layer plate, respectively with n-hexane-ethyl acetate=8
～12 1～2 for developing solvent, launch, take out, dry, put and inspect under 365nm ultra-violet lamp, in test sample chromatograph, with compare
On medical material chromatograph relevant position, the fluorescence principal spot of aobvious same color.
Further, the discrimination method of Rhizoma Chuanxiong in aforementioned ostealgia medicated wine, comprise the following steps:
(1) preparation of need testing solution: take this product 20mL, add diethyl ether 20mL every time, and shaking is extracted 2 times, merges ether solution,
Volatilizing, residue adds 1mL ethyl acetate makes it dissolve, as need testing solution；
(2) preparation of control medicinal material solution: take Rhizoma Chuanxiong control medicinal material 0.5g, adds 20mL aether backflow and extracts 1h, filter, filter
Liquid volatilizes, and residue adds ethyl acetate 1mL makes it dissolve, as control medicinal material solution；
(3) differentiate: according to four the general rule 0502 thin layer chromatography tests of " Chinese Pharmacopoeia " version in 2015, draw control medicinal material molten
Liquid 10 μ L, need testing solution 10 μ L, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate=9 1 for launching
Agent, launch, take out, dry, put and inspect under 365nm ultra-violet lamp, in test sample chromatograph, with control medicinal material chromatograph relevant position
On, the fluorescence principal spot of aobvious same color.
In order to ensure discrimination method science of the present invention, reasonable, feasible, the discrimination method of the present invention is studied and examined
Examine.
Rhizoma Chuanxiong, is usually used in blood-activating and qi-promoting, wind-expelling pain-stopping, and the pungent temperature of Rhizoma Chuanxiong is fragrant dry, walks and does not keeps, can go scattered, up up to
Mountain peak is pushed up；Enter again blood system, descending up to the sea of blood.Blood circulation promoting and blood stasis dispelling effect is extensive, the various disease of suitable stagnation of blood stasis；Wind-expelling pain-stopping, effect
With favourable, the diseases such as wind syndrome of head headache, rheumatic arthralgia can be controlled.It is the gas medicine in blood that former times people calls Rhizoma Chuanxiong, and its residence of dangerous speech is pungent to be dissipated, resolving depression, logical
Reach, the function such as pain relieving.As the principal agent of this product, this experiment will choose Rhizoma Chuanxiong control medicinal material as comparison, by ether extraction this
Rhizoma Chuanxiong composition in product, carries out thin layer discriminating to Ligusticum chuanxiong Hort, and investigate different point sample amount, different manufacturers lamellae, different temperatures,
Different humidity is on the impact of Ligusticum chuanxiong Hort thin layer chromatography in this product.Result of the test shows: with Rhizoma Chuanxiong control medicinal material for comparison, with just
Hexane-ethylacetate=8～12 1～2 are developing solvent, and the thin layer chromatography feature differentiating Rhizoma Chuanxiong is obvious, specificity
By force, can be as the discrimination method of Rhizoma Chuanxiong in this product.
1, instrument and reagent
MS304s/01 electronic balance (METTLER TOLEDO (prunus mume (sieb.) sieb.et zucc. Teller-torr benefit)), P-1 type thin layer chromatograph developing cylinder
(company limited of Xinyi Instrument Factory, Shanghai), silica gel g thin-layer plate (Qingdao Haiyang chemical industry), 5ul point sample capillary tube (Tianjin Si Lida
Science and Technology Ltd.), SLD-1 thin layer chromatography photographic apparatus (Tianjin Si Lida chromatographic technique development company).
Ostealgia medicated wine (20141201,20141202,20141203, Jiangsu Xin Bang pharmaceutical Co. Ltd), Rhizoma Chuanxiong comparison medicine
Material (Nat'l Pharmaceutical & Biological Products Control Institute), ether (Xilong Chemical Co., Ltd, analytical pure), normal hexane (western Gansu Province chemical industry
Limited company, analytical pure), ethyl acetate (Xilong Chemical Co., Ltd, analytical pure).
2, the investigation of discrimination method
2.1, the preparation method of need testing solution
In prior art, when Rhizoma Chuanxiong differentiates, need testing solution is to extract by the way of being heated to reflux.With existing skill
Art is compared, the preparation method of need testing solution in the present invention, and extraction time is short, and extraction effect is good.Two kinds of methods are used to make respectively
Available test sample solution, under equal conditions differentiates, the one group of separating degree using prior art is relatively poor, and uses this
One group of separating degree of bright method is high, favorable reproducibility.
2.2, the investigation of optimal point sample amount
Need testing solution and control medicinal material solution 4,6,8,10,12,16 μ L in difference aspiration step (1) and step (2), point
Other point, on different silica gel g thin-layer plates, is investigated, and launches, and takes out, dries, put and inspect under 365nm ultra-violet lamp.Wherein, supply
Test product 10 μ L point sample amount best results, when point sample amount is more than 12 μ L, there is conditions of streaking, point sample in need testing solution position speckle
When amount is less than 8 μ L, need testing solution position speckle is inconspicuous；During reference substance solution point sample amount 8～12 μ L effective, especially exist
Best results during 10 μ L, therefore selecting need testing solution point sample amount is 8～12 μ L, optimal point sample amount 10 μ L；Reference substance solution point sample
Amount 8～12 μ L, optimal point sample amount 10 μ L.
2.3, the investigation of developing solvent
Using n-hexane-ethyl acetate=3 1 in prior art is developing solvent；And the application uses normal hexane-
Ethyl acetate=8～12 1～2 are developing solvent, it is preferred to use n-hexane-ethyl acetate=9 1 are developing solvent.Use two kinds of exhibitions
Open agent to launch respectively, differentiate.Result shows, compared with prior art, when differentiating Rhizoma Chuanxiong in ostealgia medicated wine, uses the present invention
Developing solvent, separating degree is higher, and controllability is higher.
3, specificity is investigated
Control medicinal material solution 10 μ L in need testing solution 10 μ L, step (2) in aspiration step (1), Rhizoma Chuanxiong negative control are molten
Liquid 10 μ L, is put on same silica gel g thin-layer plate respectively by need testing solution, control medicinal material solution, negative control solution, with just own
Alkane-ethyl acetate=9 1 are developing solvent, launch, and take out, dry, put and inspect under 365nm ultra-violet lamp, in test sample chromatograph,
With on control medicinal material chromatograph relevant position, show the fluorescence principal spot of same color.Without speckle on relevant position in negative control chromatograph
Point, shows that the specificity of the method is good.As shown in Figure 1.
4, ruggedness is investigated
4.1, different manufacturers lamellae
Control medicinal material solution 10 μ L in need testing solution 10 μ L, step (2) in aspiration step (1), Rhizoma Chuanxiong negative control are molten
Liquid 10 μ L, by need testing solution, control medicinal material solution, negative control solution point sample respectively, changes the lamellae of different manufacturers, with
N-hexane-ethyl acetate=9 1 are developing solvent, launch, and take out, dry, put and inspect under 365nm ultra-violet lamp.Test sample chromatograph
In, with on control medicinal material chromatograph relevant position, the fluorescence principal spot of aobvious same color, in negative control chromatograph on relevant position
After immaculate, and replacing different manufacturers lamellae, without significant difference between each lamellae, show to change different manufacturers lamellae pair
The thin layer of Rhizoma Chuanxiong differentiates without impact.As shown in Figure 2.
4.2, humidity
Control medicinal material solution 10 μ L in need testing solution 10 μ L, step (2) in aspiration step (1), by need testing solution, right
According to medical material solution point sample respectively, convert different humidity condition, with n-hexane-ethyl acetate=9 1 as developing solvent, launch, take out,
Dry, put and inspect under 365nm ultra-violet lamp.In test sample chromatograph, with on control medicinal material chromatograph relevant position, show same color
Fluorescence principal spot, and conversion different humidity condition after, without significant difference between each lamellae, show conversion different humidity to river
The thin layer of rhizome of chuanxiong differentiates without impact.As shown in Figure 3.
4.3, temperature
Control medicinal material solution 10 μ L in need testing solution 10 μ L, step (2) in aspiration step (1), by need testing solution, right
According to medical material solution point sample respectively, convert condition of different temperatures, with n-hexane-ethyl acetate=9 1 as developing solvent, launch, take out,
Dry, put and inspect under 365nm ultra-violet lamp.In test sample chromatograph, with on control medicinal material chromatograph relevant position, show same color
Fluorescence principal spot, and conversion condition of different temperatures after, without significant difference between each lamellae, show conversion different temperatures to river
The thin layer of rhizome of chuanxiong differentiates without impact.As shown in Figure 4.
The invention have benefit that: the discrimination method of Rhizoma Chuanxiong in a kind of ostealgia medicated wine that the present invention provides, it is possible to real
Differentiating the Rhizoma Chuanxiong in ostealgia medicated wine the most efficiently and accurately, simple to operate, controllability is high, and separating degree is high, highly sensitive, precision,
Good stability, favorable reproducibility, and negative control are noiseless, and different manufacturers lamellae and temperature, damp condition do not affect.This
Invention discrimination method can carry out effective discriminating accurate, comprehensive, scientifical to Rhizoma Chuanxiong composition in ostealgia medicated wine, improves quality inspection
Mark is accurate, further ensure that the stable, safely, effectively of product quality.
Accompanying drawing explanation
Fig. 1 be the present invention ostealgia medicated wine in the specificity identification color spectrogram of Rhizoma Chuanxiong；
Fig. 2 is the chromatogram that in ostealgia medicated wine, Rhizoma Chuanxiong uses different lamellae when differentiating；
Fig. 3 be in ostealgia medicated wine Rhizoma Chuanxiong differentiate time different humidity under the conditions of chromatogram；
Chromatogram under condition of different temperatures when Fig. 4 is that in ostealgia medicated wine, Rhizoma Chuanxiong differentiates；
The implication of reference in figure: Fig. 1: 1-negative control, 2-test sample lot number 20141201,3-test sample lot number
20141202,4-test sample lot number 20141203,5-Rhizoma Chuanxiong control medicinal material；Fig. 2-Fig. 4: 1-test sample lot number 20141201,2-
Test sample lot number 20141202,3-test sample lot number 20141203,4-Rhizoma Chuanxiong control medicinal material；Fig. 2: A-Qingdao Haiyang silica gel G is thin
Laminate (specification: 100 × 200mm), B-Yantai Chemical Industry Research Inst. silica gel g thin-layer plate (specification: 100 × 200mm)；Fig. 3:
A-humidity 32%, B-humidity 72%；Fig. 4: A-temperature 25 DEG C, B-temperature 8 DEG C.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further introduced.
Embodiment 1
The discrimination method of Rhizoma Chuanxiong in ostealgia medicated wine, comprises the following steps:
(1) preparation of need testing solution: take this product 22mL, add diethyl ether 25mL every time, and shaking is extracted 1 time, obtains ether solution, waves
Dry, residue adds 2mL ethyl acetate makes it dissolve, as need testing solution；
(2) preparation of control medicinal material solution: take Rhizoma Chuanxiong control medicinal material 0.5g, adds 15mL aether backflow and extracts 1.5h, filter,
Filtrate volatilizes, and residue adds ethyl acetate 1mL makes it dissolve, as control medicinal material solution；
(3) differentiate: according to four the general rule 0502 thin layer chromatography tests of " Chinese Pharmacopoeia " version in 2015, draw control medicinal material molten
Liquid 8 μ L, need testing solution 8 μ L, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate=8 1 as developing solvent,
Launch, take out, dry, put and inspect under 365nm ultra-violet lamp, in test sample chromatograph, with on control medicinal material chromatograph relevant position,
The fluorescence principal spot of aobvious same color.
Embodiment 2
The discrimination method of Rhizoma Chuanxiong in ostealgia medicated wine, comprises the following steps:
(1) preparation of need testing solution: take this product 25mL, add diethyl ether 30mL every time, and shaking is extracted 3 times, merges ether solution,
Volatilizing, residue adds 3mL ethyl acetate makes it dissolve, as need testing solution；
(2) preparation of control medicinal material solution: take Rhizoma Chuanxiong control medicinal material 0.5g, adds 18mL aether backflow and extracts 2h, filter, filter
Liquid volatilizes, and residue adds ethyl acetate 1mL makes it dissolve, as control medicinal material solution；
(3) differentiate: according to four the general rule 0502 thin layer chromatography tests of " Chinese Pharmacopoeia " version in 2015, draw control medicinal material molten
Liquid 12 μ L, need testing solution 12 μ L, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate=12 2 for launching
Agent, launch, take out, dry, put and inspect under 365nm ultra-violet lamp, in test sample chromatograph, with control medicinal material chromatograph relevant position
On, the fluorescence principal spot of aobvious same color.
Embodiment 3
The discrimination method of Rhizoma Chuanxiong in ostealgia medicated wine, comprises the following steps:
(1) preparation of need testing solution: take this product 20mL, add diethyl ether 20mL every time, and shaking is extracted 2 times, merges ether solution,
Volatilizing, residue adds 1mL ethyl acetate makes it dissolve, as need testing solution；
(2) preparation of control medicinal material solution: take Rhizoma Chuanxiong control medicinal material 0.5g, adds 20mL aether backflow and extracts 1h, filter, filter
Liquid volatilizes, and residue adds ethyl acetate 1mL makes it dissolve, as control medicinal material solution；
(3) differentiate: according to four the general rule 0502 thin layer chromatography tests of " Chinese Pharmacopoeia " version in 2015, draw control medicinal material molten
Liquid 10 μ L, need testing solution 10 μ L, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate=9 1 for launching
Agent, launch, take out, dry, put and inspect under 365nm ultra-violet lamp, in test sample chromatograph, with control medicinal material chromatograph relevant position
On, the fluorescence principal spot of aobvious same color.
Embodiment 4
The discrimination method of Rhizoma Chuanxiong in ostealgia medicated wine, comprises the following steps:
(1) preparation of need testing solution: take this product 23mL, add diethyl ether 28mL every time, and shaking is extracted 2 times, merges ether solution,
Volatilizing, residue adds 2mL ethyl acetate makes it dissolve, as need testing solution；
(2) preparation of control medicinal material solution: take Rhizoma Chuanxiong control medicinal material 0.5g, adds 16mL aether backflow and extracts 1.8h, filter,
Filtrate volatilizes, and residue adds ethyl acetate 1mL makes it dissolve, as control medicinal material solution；
(3) differentiate: according to four the general rule 0502 thin layer chromatography tests of " Chinese Pharmacopoeia " version in 2015, draw control medicinal material molten
Liquid 11 μ L, need testing solution 9 μ L, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate=11 2 for launching
Agent, launch, take out, dry, put and inspect under 365nm ultra-violet lamp, in test sample chromatograph, with control medicinal material chromatograph relevant position
On, the fluorescence principal spot of aobvious same color.
Claims (4)
1. the discrimination method of Rhizoma Chuanxiong in ostealgia medicated wine, it is characterised in that: described discrimination method is with Rhizoma Chuanxiong control medicinal material for comparison,
With n-hexane-ethyl acetate=8～12 1～2 thin layer chromatography as developing solvent.
The discrimination method of Rhizoma Chuanxiong in ostealgia medicated wine the most according to claim 1, it is characterised in that: concrete discrimination method bag
Include following steps:
(1) preparation of need testing solution: take this product add diethyl ether shaking extract, obtain ether solution, volatilize, residue adds ethyl acetate makes it
Dissolve, as need testing solution；
(2) preparation of control medicinal material solution: taking Rhizoma Chuanxiong control medicinal material 0.5g, add diethyl ether reflux, extract, filters, and filtrate volatilizes, residual
Slag adds ethyl acetate 1mL makes it dissolve, as control medicinal material solution；
(3) differentiate: test according to four general rule 0502 thin layer chromatography of " Chinese Pharmacopoeia " version in 2015, absorption control medicinal material solution,
Need testing solution, puts respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate=8～12 1～2 as developing solvent, and exhibition
Open, take out, dry, put and inspect under 365nm ultra-violet lamp, in test sample chromatograph, with on control medicinal material chromatograph relevant position, show
The fluorescence principal spot of same color.
The discrimination method of Rhizoma Chuanxiong in ostealgia medicated wine the most according to claim 2, it is characterised in that: concrete discrimination method bag
Include following steps:
(1) preparation of need testing solution: take this product 20mL～25mL, adds diethyl ether 20～30mL every time, and shaking is extracted 2～3 times, closes
And ether solution, volatilizing, residue adds 1～3mL ethyl acetate makes it dissolve, as need testing solution；
(2) preparation of control medicinal material solution: take Rhizoma Chuanxiong control medicinal material 0.5g, adds 15mL～20mL aether backflow and extracts 1～2h, mistake
Filter, filtrate volatilizes, and residue adds ethyl acetate 1mL makes it dissolve, as control medicinal material solution；
(3) differentiate: according to four the general rule 0502 thin layer chromatography tests of " Chinese Pharmacopoeia " version in 2015, draw control medicinal material solution 8
～12 μ L, need testing solution 8 μ L～12 μ L, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate=8～
12 1～2 be developing solvent, launch, take out, dry, put and inspect under 365nm ultra-violet lamp, in test sample chromatograph, with compare medicine
On wood color spectrum relevant position, the fluorescence principal spot of aobvious same color.
4. according to the discrimination method of Rhizoma Chuanxiong in the ostealgia medicated wine described in Claims 2 or 3, it is characterised in that: concrete discriminating side
Method comprises the following steps:
(1) preparation of need testing solution: take this product 20mL, add diethyl ether 20mL every time, and shaking is extracted 2 times, merges ether solution, waves
Dry, residue adds 1mL ethyl acetate makes it dissolve, as need testing solution；
(2) preparation of control medicinal material solution: take Rhizoma Chuanxiong control medicinal material 0.5g, adds 20mL aether backflow and extracts 1h, filter, and filtrate is waved
Dry, residue adds ethyl acetate 1mL makes it dissolve, as control medicinal material solution；
(3) differentiate: according to four the general rule 0502 thin layer chromatography tests of " Chinese Pharmacopoeia " version in 2015, draw control medicinal material solution 10
μ L, need testing solution 10 μ L, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate=9 1 as developing solvent, and exhibition
Open, take out, dry, put and inspect under 365nm ultra-violet lamp, in test sample chromatograph, with on control medicinal material chromatograph relevant position, show
The fluorescence principal spot of same color.
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Application publication date: 20161214 |