CN106501440B - The discrimination method of field pennycress in Chinese medicine compound prescription - Google Patents
The discrimination method of field pennycress in Chinese medicine compound prescription Download PDFInfo
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- CN106501440B CN106501440B CN201610936802.2A CN201610936802A CN106501440B CN 106501440 B CN106501440 B CN 106501440B CN 201610936802 A CN201610936802 A CN 201610936802A CN 106501440 B CN106501440 B CN 106501440B
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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
- G01N30/90—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
- 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
- G01N1/40—Concentrating samples
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Abstract
The invention discloses a kind of discrimination method of field pennycress in Chinese medicine compound prescription, the thin-layer identification method of field pennycress more particularly in Chinese medicine compound prescription.The discrimination method of the present invention comprises the following steps：The preparation of control medicinal material solution；The preparation of need testing solution；The preparation of negative sample solution；With capillary sample applicator on same silica gel g thin-layer plate point sample；Lamellae is placed in chromatography cylinder, deployed with solvent, takes out, dries；Chromatographic sheet is inspected, result is obtained and is differentiated, test sample chromatogram shows the principal spot of same color, negative sample is without this spot on position corresponding with control medicinal material chromatogram.The discrimination method technique of the present invention is simple, good separating effect, has extremely strong specificity, further increases the accuracy of field pennycress Components identification in Chinese medicine compound prescription, has huge popularization and application potentiality in the medicine identification field relevant with field pennycress.
Description
Technical field
The present invention relates to the discrimination method of field pennycress in Chinese medicine compound prescription, the thin layer mirror of field pennycress more particularly in Chinese medicine compound prescription
Other method.
Background technology
For field pennycress section plant patrinia scabiosaefolia Fiscs Patrinia scabiosaefolia Fisch. or patrima villosa
Patrinia villosa Juss. drying herb.Excavate before summer, the flowers are in blossom, shine to half-dried, be bundled into beam, then dry in the shade.Main product in
Jiangsu, Zhejiang, Hubei, Anhui.Field pennycress has the effect of clearing heat and detoxicating, removing blood stasis and expelling pus.Cure mainly appendicitis, dysentery, enteritis, liver
Inflammation, eye conjunctivitis, postpartum blood stasis stomachache, carbuncle swells furunculosis.Also plurality of Chinese compound product can be made with other medicinal material compatibilities in field pennycress
Kind, such as infirmity clear piece recorded in 2015, Baijiang Tablets, compound fuyanping capsules, palace of the Qing Dynasty liquid, wonderful of the seed of jog's tears six in document
Grain etc., also contains field pennycress in its prescription.The only enterprise's production at present of wherein infirmity clear piece, is exclusive kind, sales volume is considerable.
The Chinese medicine compound prescription kind containing field pennycress only has infirmity clear piece a kind of in Chinese Pharmacopoeia, and field pennycress is not yet established in its standard
Discrimination method.
Kind Baijiang Tablets (document 1 in document：Tang's Yi, Dong Lin, remaining dawn qin Baijiang Tablets quality standard research Chinese patent drugs
.2008,30 (2):223~226), compound fuyanping capsules (document 2：The compounds woman such as Luo Yuhong, beam Feihua, yellow good force are scorching flat
Capsule quality standard controls Journal of Chinese Hospital Pharmacy .2009,29 (1)：73~75), Yiren Liumiao granule (document 3：Cao Ming
Into the Yiren Liumiao granules quality standard research R＆D of modern TCM such as Chen Bin, Li Liubing is with putting into practice .2004,18 (5)：50~
52) discriminating of field pennycress thin layer is established.Applicant was once lost in dysentery oral liquid using the discrimination method dialogue hardship in document
Field pennycress carries out indentification by TLC, as a result shows that these methods can't check, separating effect is also bad.At present, domestic and international centering
The quality control of medicine compound kind is more and more stricter, therefore is badly in need of finding a kind of stabilization, reliable, easy thin-layered chromatography, energy
Accurate and effective differentiates to field pennycress composition in Chinese medicine compound prescription.
The content of the invention
For prior art, the unused ethyl acetate of test sample preparation method, solvent used is mixed solution, but is ground
Study carefully and find that these preparation methods and solvent, separation degree do not reach preferable identification result.It is an object of the invention to provide
A kind of test sample preparation method and solvent, the need testing solution preparation method are to use ethyl acetate solvent is adopted for solvent
With ammonia vapo(u)rous, the technical scheme of the field pennycress thin-layer chromatography, have simple and efficient to handle, good separating effect, specificity it is strong,
The advantages that being widely used, solve the problems, such as that prior art is present, the present invention contributes to improve the medicine relevant with field pennycress simultaneously
Quality standard.
The present invention relates to a kind of discrimination method of field pennycress in Chinese medicine compound prescription, the discrimination method comprises the following steps：
(1) preparation of control medicinal material solution：Field pennycress control medicinal material is taken, adds water, is decocted, filtering, filtrate concentration, with for examination
Prepared by product solution manufacturing method, as control medicinal material solution；
(2) preparation of need testing solution：Testing sample liquid is taken, adds ethyl acetate to extract, combined ethyl acetate liquid, is steamed
Dry, residue adds methanol to make dissolving, as need testing solution；
When field pennycress technique is former powder in testing sample, testing sample is taken, is added water to cook, filtered, filtrate concentration, add second
Acetoacetic ester extracts, and combined ethyl acetate liquid, is evaporated, residue adds methanol to make dissolving, as need testing solution；
When testing sample is solid, and field pennycress technique is extracts, testing sample is taken, adds hot water dissolving, filters, takes filter
Liquid, add ethyl acetate to extract, combined ethyl acetate liquid, be evaporated, residue adds methanol to make dissolving, as need testing solution；
(3) preparation of negative sample solution：Other medicinal materials of scarce field pennycress are taken in testing sample prescription ratio, preparation is free of
The compound Chinese medicinal preparation of field pennycress, take with testing sample equal amount, according still further in step (2) after " taking testing sample ",
Operated with method, gained methanol lysate is negative sample solution；
(4) with capillary sample applicator draw respectively control medicinal material solution, need testing solution and negative sample solution each 0.1~
50 μ L, put successively on same silica gel g thin-layer plate；
(5) toluene, ethyl acetate mixing are taken, another groove puts isometric ammoniacal liquor saturation, as solvent, is placed in dried and clean
In chromatography cylinder, the lamellae that step (4) obtains is placed in chromatography cylinder, deployed, takes out, dries；
(6) chromatographic sheet is inspected, is differentiated to obtaining result；
The testing sample is the compound Chinese medicinal preparation containing field pennycress.
Preferably, the amount that water is added in the step (1) is 1~500 times of control medicinal material quality；Filtrate is concentrated into control
1~50 times of quality of medicinal material；The amount for adding ethyl acetate twice is 0.1~10 times of concentrate quality.
Preferably, the amount that ethyl acetate is added in the step (2) is 1~100 times of testing sample volume.
Preferably, toluene, the volume ratio of ethyl acetate are 10 in the solvent in the step (5):1, with isometric ammonia
Water saturation.
Preferably, after chromatographic sheet is inspected in the step (6) as spray developer heating, inspect in the sunlight.
Preferably, the discrimination method is carried out according to the following steps：
(1) preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, adds water 150ml, decocts half an hour, is filtered, filter
Liquid is concentrated into 30ml, is prepared with need testing solution preparation method, as field pennycress control medicinal material solution；
(2) preparation of need testing solution：
When testing sample is liquid, the testing sample liquid equivalent to the 2g of medicinal material containing field pennycress is taken, dilutes or is concentrated into
30ml, adding ethyl acetate to extract 2 times, each 20ml, combined ethyl acetate liquid, be evaporated, residue adds methanol 1ml to make dissolving, as
Need testing solution；
When field pennycress technique is former powder, the testing sample powder equivalent to the 2g of medicinal material containing field pennycress is taken, adds 150ml water,
Decoct, filtering, be concentrated into 30ml, add ethyl acetate to extract 2 times, each 20ml, combined ethyl acetate liquid, be evaporated, residue adds first
Alcohol 1ml makes dissolving, as need testing solution；
When field pennycress technique is extracts, the testing sample powder equivalent to the 2g of medicinal material containing field pennycress is taken, with 50ml hot water
Dissolving, filtering, takes filtrate, adds ethyl acetate to extract 2 times, each 20ml, combined ethyl acetate liquid, is evaporated, residue adds methanol 1ml
Make dissolving, as need testing solution；
(3) preparation of negative sample solution：Other medicinal materials of scarce field pennycress are taken in testing sample prescription ratio, preparation is free of
The compound Chinese medicinal preparation of field pennycress, according still further in step (2) from " take testing sample liquid equivalent to the 2g of medicinal material containing field pennycress/
Rise, operated with method, gained methanol lysate is negative sample solution after powder "；
(4) control medicinal material solution, need testing solution and each 1-20 μ of negative sample solution are drawn respectively with capillary sample applicator
L, put successively on same silica gel g thin-layer plate；
(5) it is 10 according to volume ratio by toluene, ethyl acetate:1 is well mixed, and another groove puts isometric ammoniacal liquor, as expansion
Agent, it is placed in the chromatography cylinder of dried and clean, the lamellae that step (4) obtains is placed in chromatography cylinder, deploy, takes out, dry；
(6) lamellae after step (5) is dried is sprayed with 5% vanillin-sulfuric acid solution, and it is clear to be heated to spot development, day
Inspected under light, obtain thin-layer chromatogram, judged whether to contain field pennycress according to gained thin-layer chromatogram.
The testing sample is that white hardship loses dysentery oral liquid, infirmity piece, QianLieping jiaonang, Golden Horse liver Thailand particle, hemorrhoid clearly are comfortably washed
Liquid or white sauce cold granules.
The discrimination method of field pennycress has the following advantages that in Chinese medicine compound prescription of the present invention：
1. for the thin-layer identification method of field pennycress in compound Chinese medicinal preparation, solvent system is more, such as：Toluene-acetic acid
Ethyl ester-formic acid, n-hexane-ethyl acetate-methanol-acetic acid, n-hexane-ethyl acetate-methanol, chloroform-methanol-water etc., with reference to
Chromatogram is by technical scheme of the present invention compared with the discrimination method in field pennycress document.Discriminating side in above-mentioned document
Method separating effect is bad, is not suitable for the discriminating of field pennycress in this preparation, the technical scheme that the present invention is established, separating effect is than upper
It is more preferable to state method, RfValue is more moderate, and feminine gender is noiseless, specificity is strong, and method is simple.
2. having carried out indentification by TLC inspection to oneself the several Chinese medicine compound prescription kinds of listing using the method for the present invention, obtain
To the results are shown in Table 1, as a result prove technical solutions according to the invention can be widely applied to Chinese medicine of the in the market containing field pennycress
Compound kind indentification by TLC, and positive effect is better than prior art.
Brief description of the drawings
The present invention is further detailed below in conjunction with the accompanying drawings.
Fig. 1 is according to the field pennycress thin-layer chromatography photo obtained by document 1；Wherein, μ l of 1. field pennycress control medicinal material 5,2.
μ l of field pennycress control medicinal material 10, μ l of 3. test sample 2, μ l of 4. test sample 3, μ l of 5. test sample 4, μ l of 6. test sample 4,7. feminine genders (lack
Field pennycress) 2 μ l；Development system：Toluene ﹣ ethyl acetate ﹣ formic acid (15: 2: 0.5), inspection system：10% ethanol solution of sulfuric acid is sprayed,
It is clear to be heated to spot development, is inspected under ultraviolet lamp (365nm).
Fig. 2 is that the field pennycress thin-layer chromatography photo obtained by solvent ratio is adjusted on the basis of document 1；Wherein, 1. bear
μ l of tartaric acid reference substance 2, μ l of 2. field pennycress control medicinal material 2,3. feminine gender (scarce field pennycress) 2 μ l, the μ l of 4~8. test sample 1~5；Expansion
System：N-hexane ﹣ ethyl acetate ﹣ formic acid (30: 10: 0.5), inspection system：10% ethanol solution of sulfuric acid, is heated to spot development
Clearly, inspected under ultraviolet lamp (365nm).
Fig. 3 is that the field pennycress thin-layer chromatography photo obtained by solvent ratio is adjusted on the basis of document 1；Wherein, 1. lose
μ l of sauce grass control medicinal material 5, μ l of 2. test sample 2, μ l of 3. test sample 2, μ l of 4. test sample 2,5. feminine gender (scarce field pennycress) 2 μ l；Expansion
System：N-hexane ﹣ ethyl acetate ﹣ formic acid (15: 5: 0.5)；Wherein Fig. 3-1 inspection system：10% ethanol solution of sulfuric acid is sprayed, is added
Heat is clear to spot development, is inspected under ultraviolet lamp (365nm)；Wherein Fig. 3-2 inspection system：It is molten to spray 5% vanillin-sulfuric acid
Liquid, it is clear to be heated to spot development, is inspected under daylight.
Fig. 4 is that the field pennycress thin-layer chromatography photo obtained by solvent ratio is adjusted on the basis of document 1；Wherein, 1. lose
μ l of sauce grass control medicinal material 5, μ l of 2. test sample 2, μ l of 3. test sample 2, μ l of 4. test sample 2,5. feminine gender (scarce field pennycress) 2 μ l；Expansion
System：N-hexane ﹣ ethyl acetate ﹣ formic acid (15: 5: 1), inspection system：5% vanillin-sulfuric acid solution is sprayed, is heated to spot development
Clearly, inspected under daylight.
Fig. 5 is that the field pennycress thin-layer chromatography photo obtained by solvent ratio is adjusted on the basis of document 1；Wherein, wherein,
1. μ l of field pennycress control medicinal material 5, μ l of 2. test sample 2, μ l of 3. test sample 2, μ l of 4. test sample 2,5. feminine gender (scarce field pennycress) 2 μ l；
Development system：Toluene ﹣ ethyl acetate ﹣ formic acid (15: 2: 0.5), inspection system：5% vanillin-sulfuric acid solution is sprayed, is heated to spot
Colour developing is clear, is inspected under daylight.
Fig. 6 is that the field pennycress thin-layer chromatography photo obtained by solvent ratio is adjusted on the basis of document 1；Wherein, wherein,
1. μ l of field pennycress control medicinal material 5, μ l of 2. test sample 2, μ l of 3. test sample 2, μ l of 4. test sample 2,5. feminine gender (scarce field pennycress) 2 μ l；
Development system：Toluene ﹣ ethyl acetate ﹣ formic acid (10: 1: 0.5), inspection system：5% vanillin-sulfuric acid solution is sprayed, is heated to spot
Colour developing is clear, is inspected under daylight.
Fig. 7 is that the field pennycress thin-layer chromatography photo obtained by solvent ratio is adjusted on the basis of document 1；Wherein, wherein,
1. μ l of field pennycress control medicinal material 5, μ l of 2. test sample 2, μ l of 3. test sample 2, μ l of 4. test sample 2,5. feminine gender (scarce field pennycress) 2 μ l；
Development system：Toluene ﹣ ethyl acetate ﹣ formic acid (5: 1: 0.5), inspection system：5% vanillin-sulfuric acid solution is sprayed, is heated to spot
Colour developing is clear, is inspected under daylight.
Fig. 8 is field pennycress thin layer photo in the infirmity clear piece obtained by the present invention；Wherein, 1. field pennycress control medicinal materials, 2~
4.20130226,5. negative (scarce field pennycress)；
Fig. 9 is field pennycress thin layer photo in the QianLieping jiaonang obtained by the present invention；Wherein, 1. field pennycress control medicinal materials, 2
~4.20140702,5. negative (scarce field pennycress)；
Figure 10 is field pennycress thin layer photo in the Golden Horse liver Thailand particle obtained by the present invention；Wherein, 1. field pennycress comparison medicine
Material, 2~4.20160301,5. negative (scarce field pennycress)；
Figure 11 is field pennycress thin layer photo in the comfortable wash liquid for hemorrhoids obtained by the present invention；Wherein, 1. field pennycress control medicinal materials,
2~4.20160401,5. negative (scarce field pennycress)；
Figure 12 is that the white hardship obtained by the present invention loses field pennycress thin-layer chromatography photo in dysentery oral liquid；Wherein, 1. field pennycress
Control medicinal material, 2.20120501,3.20120502,4.20120503,5. negative (scarce field pennycress)；Development system：Toluene ﹣ acetic acid
Ethyl ester (10: 1), another groove put isometric ammoniacal liquor saturation；Inspection system：5% vanillin-sulfuric acid solution, it is clear to be heated to spot development
It is clear, inspected under daylight.
Embodiment
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.
Embodiment 1
The discrimination method of field pennycress is the indentification by TLC to field pennycress in infirmity clear piece in the Chinese medicine compound prescription of the present embodiment：
1. instrument and reagent
Field pennycress control medicinal material (Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number：121271-201201)；The medication of prescription institute
Material (is purchased from Hebei Anguo Chinese Medicinal Materials Markets)；Infirmity clear piece (Longshunrong Pharmaceutical Factory, Tianjin Zhongxin Pharmaceutical Group Co., Ltd, rule
Lattice：Every 0.6 gram of weight, lot number are：20130226)；Silica G plate (100mm × 100mm, Haiyang Chemical Plant, Qingdao)；Other reagents
It is that analysis is pure.
2. method and result
(1) preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, adds water 150ml, decocts half an hour, is filtered, filter
Liquid is concentrated into 30ml, is prepared with need testing solution preparation method, as field pennycress control medicinal material solution；
(2) preparation of need testing solution：
Infirmity clear piece 8 is taken, film-coating removes coating, finely ground, the 150ml dissolvings of heating water, centrifugation, takes supernatant, adds acetic acid
Ethyl ester extracts 2 times, each 20ml, combined ethyl acetate liquid, is evaporated, residue adds methanol 1ml to make dissolving, as need testing solution；
(3) preparation of negative sample solution：Other medicinal materials of scarce field pennycress are taken in testing sample prescription ratio, preparation is free of
The Chinese medicine compound prescription piece of field pennycress, according still further to from after " finely ground ", being operated in step (2) with method, gained methanol lysate is
Negative sample solution；
(4) μ L of control medicinal material solution 2, need testing solution and each 1- of negative sample solution are drawn respectively with capillary sample applicator
10 μ L, put successively on same silica gel g thin-layer plate；
(5) it is 10 according to volume ratio by toluene, ethyl acetate:1 is well mixed, and another groove puts isometric ammoniacal liquor, as expansion
Agent, it is placed in the chromatography cylinder of dried and clean, the lamellae that step (4) obtains is placed in chromatography cylinder, deploy, takes out, dry；
(6) lamellae after step (5) is dried is sprayed with 5% vanillin-sulfuric acid solution, and it is clear to be heated to spot development, day
Inspected under light, obtain thin-layer chromatogram, test sample chromatogram shows the master of same color on position corresponding with control medicinal material chromatogram
Spot, negative sample is without this spot；Its result is as shown in Figure 8.
Embodiment 2
The discrimination method of field pennycress is the thin-layer chromatography to field pennycress in QianLieping jiaonang in the Chinese medicine compound prescription of the present embodiment
Differentiate：
1. instrument and reagent
Field pennycress control medicinal material (Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number：121271-201201)；The medication of prescription institute
Material (is purchased from Hebei Anguo Chinese Medicinal Materials Markets)；QianLieping jiaonang (Xi'an Qianhe Pharmaceutical Co., Ltd, specification：0.4g/ grains,
Lot number is：20140702)；Silica G plate (100mm × 100mm, Haiyang Chemical Plant, Qingdao)；Other reagents are that analysis is pure.
2. method and result
(1) preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, adds water 150ml, decocts half an hour, is filtered, filter
Liquid is concentrated into 30ml, is prepared with need testing solution preparation method, as field pennycress control medicinal material solution；
(2) preparation of need testing solution：
QianLieping jiaonang 3 is taken, pours out content, heating water 30ml makes dissolving, centrifuges, take supernatant, add ethyl acetate
Extraction 2 times, each 20ml, combined ethyl acetate liquid, is evaporated, residue adds methanol 1ml to make dissolving, as need testing solution；
(3) preparation of negative sample solution：Other medicinal materials of scarce field pennycress are taken in testing sample prescription ratio, preparation is free of
The Chinese medicine compound prescription liquid of field pennycress, according still further to from after " pouring out content ", being operated in step (2) with method, gained methanol is molten
It is negative sample solution to solve liquid；
(4) μ L of control medicinal material solution 2, need testing solution and each 1 μ of negative sample solution are drawn respectively with capillary sample applicator
L, put successively on same silica gel g thin-layer plate；
(5) it is 10 according to volume ratio by toluene, ethyl acetate:1 is well mixed, and another groove puts isometric ammoniacal liquor, as expansion
Agent, it is placed in the chromatography cylinder of dried and clean, the lamellae that step (4) obtains is placed in chromatography cylinder, deploy, takes out, dry；
(6) lamellae after step (5) is dried is sprayed with 5% vanillin-sulfuric acid solution, and it is clear to be heated to spot development, day
Inspected under light, obtain thin-layer chromatogram, test sample chromatogram shows the master of same color on position corresponding with control medicinal material chromatogram
Spot, negative sample is without this spot；Its result is as shown in Figure 9.
Embodiment 3
The discrimination method of field pennycress is the thin layer color to field pennycress in Golden Horse liver Thailand particle in the Chinese medicine compound prescription of the present embodiment
Spectrum differentiates：
1. instrument and reagent
Field pennycress control medicinal material (Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number：121271-201201)；The medication of prescription institute
Material (is purchased from Hebei Anguo Chinese Medicinal Materials Markets)；Golden Horse liver Thailand particle (the long-lived permanently happy pharmaceutical factory in Guizhou, specification：Per packed 2g (no sugarcanes
Sugar), lot number is：20160301)；Silica G plate (100mm × 100mm, Haiyang Chemical Plant, Qingdao)；Other reagents are that analysis is pure.
2. method and result
(1) preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, adds water 150ml, decocts half an hour, is filtered, filter
Liquid is concentrated into 30ml, is prepared with need testing solution preparation method, as field pennycress control medicinal material solution；
(2) preparation of need testing solution：
Take Golden Horse liver Thailand particle 18g, heating water 30ml to make dissolving, centrifuge, take supernatant, add ethyl acetate extraction 2 times, often
Secondary 20ml, combined ethyl acetate liquid, is evaporated, and residue adds methanol 1ml to make dissolving, as need testing solution；
(3) preparation of negative sample solution：Other medicinal materials of scarce field pennycress are taken in testing sample prescription ratio, preparation is free of
The compound Chinese medicinal preparation of field pennycress, according still further to from after " pouring out content ", being operated in step (2) with method, gained methanol is molten
It is negative sample solution to solve liquid；
(4) μ L of control medicinal material solution 5, need testing solution and each 5 μ of negative sample solution are drawn respectively with capillary sample applicator
L, put successively on same silica gel g thin-layer plate；
(5) it is 10 according to volume ratio by toluene, ethyl acetate:1 is well mixed, and another groove puts isometric ammoniacal liquor, as expansion
Agent, it is placed in the chromatography cylinder of dried and clean, the lamellae that step (4) obtains is placed in chromatography cylinder, deploy, takes out, dry；
(6) lamellae after step (5) is dried is sprayed with 5% vanillin-sulfuric acid solution, and it is clear to be heated to spot development, day
Inspected under light, obtain thin-layer chromatogram, test sample chromatogram shows the master of same color on position corresponding with control medicinal material chromatogram
Spot, negative sample is without this spot；Its result is as shown in Figure 10.
Embodiment 4
The discrimination method of field pennycress is the thin-layer chromatography to field pennycress in comfortable wash liquid for hemorrhoids in the Chinese medicine compound prescription of the present embodiment
Differentiate：
1. instrument and reagent
Field pennycress control medicinal material (Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number：121271-201201)；The medication of prescription institute
Material (is purchased from Hebei Anguo Chinese Medicinal Materials Markets)；Comfortable wash liquid for hemorrhoids (Yunnan Mingyang Pharmaceutical Co., Ltd., specification：Per bottled 300 millis
Rise, lot number is：20160401)；Silica G plate (100mm × 100mm, Yantai Chemical Industry Research Inst.)；Other reagents are point
Analyse pure.
2. method and result
(1) preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, adds water 150ml, decocts half an hour, is filtered, filter
Liquid is concentrated into 30ml, is prepared with need testing solution preparation method, as field pennycress control medicinal material solution；
(2) preparation of need testing solution：
Comfortable wash liquid for hemorrhoids 20ml is taken, adds water 10ml to dilute, adds ethyl acetate to extract 2 times, each 20ml, combined ethyl acetate
Liquid, it is evaporated, residue adds methanol 1ml to make dissolving, as need testing solution；
(3) preparation of negative sample solution：Other medicinal materials of scarce field pennycress are taken in testing sample prescription ratio, preparation is free of
The Chinese medicine compound prescription liquid of field pennycress, according still further to from " addition ethyl acetate ", being operated in step (2) with method, gained methanol dissolves
Liquid is negative sample solution；
(4) control medicinal material solution, need testing solution and each 2 μ L of negative sample solution are drawn respectively with capillary sample applicator,
Put successively on same silica gel g thin-layer plate；
(5) it is 10 according to volume ratio by toluene, ethyl acetate:1 is well mixed, and another groove puts isometric ammoniacal liquor, as expansion
Agent, it is placed in the chromatography cylinder of dried and clean, the lamellae that step (4) obtains is placed in chromatography cylinder, deploy, takes out, dry；
(6) lamellae after step (5) is dried is sprayed with 5% vanillin-sulfuric acid solution, and it is clear to be heated to spot development, day
Inspected under light, obtain thin-layer chromatogram, test sample chromatogram shows the master of same color on position corresponding with control medicinal material chromatogram
Spot, negative sample is without this spot；Its result is as shown in Figure 11.
Embodiment 5
The discrimination method of field pennycress is the thin layer that dialogue hardship loses field pennycress in dysentery oral liquid in the Chinese medicine compound prescription of the present embodiment
Chromatographic identification：
1. instrument and reagent
Field pennycress control medicinal material (Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number：121271-201201)；The medication of prescription institute
Material (is purchased from Hebei Anguo Chinese Medicinal Materials Markets)；White hardship loses dysentery oral liquid, and (for my company's production, prescription is the Chinese bulbul, kuh-seng, Patrinia scaniosaefolia
Grass etc., specification：It is equivalent to primary crude drug 0.5g, lot number per 1g：20120501、20120502、20120503)；Silica G plate
(100mm × 100mm, Yantai Chemical Industry Research Inst.)；Other reagents are that analysis is pure.
2. method and result
(1) preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, adds water 150ml, decocts half an hour, is filtered, filter
Liquid is concentrated into 30ml, is prepared with need testing solution preparation method, as field pennycress control medicinal material solution；
(2) preparation of need testing solution：
Take white hardship to lose dysentery oral liquid 30ml, add ethyl acetate to extract 2 times, each 20ml, combined ethyl acetate liquid, be evaporated,
Residue adds methanol 1ml to make dissolving, as need testing solution；
(3) preparation of negative sample solution：Other medicinal materials of scarce field pennycress are taken in testing sample prescription ratio, preparation is free of
The Chinese medicine compound prescription liquid of field pennycress, according still further to from " addition ethyl acetate ", being operated in step (2) with method, gained methanol dissolves
Liquid is negative sample solution；
(4) control medicinal material solution, need testing solution and each 2 μ L of negative sample solution are drawn respectively with capillary sample applicator,
Put successively on same silica gel g thin-layer plate；
(5) it is 10 according to volume ratio by toluene, ethyl acetate:1 is well mixed, and another groove puts isometric ammoniacal liquor, as expansion
Agent, it is placed in the chromatography cylinder of dried and clean, the lamellae that step (4) obtains is placed in chromatography cylinder, deploy, takes out, dry；
(6) lamellae after step (5) is dried is sprayed with 5% vanillin-sulfuric acid solution, and it is clear to be heated to spot development, day
Inspected under light, obtain thin-layer chromatogram, test sample chromatogram shows the master of same color on position corresponding with control medicinal material chromatogram
Spot, negative sample is without this spot；Its result is as shown in Figure 12.
Contrast test 1
For the thin-layer identification method of field pennycress in compound Chinese medicinal preparation, national standard for traditional Chinese medicines compilation internal medicine lung system (one)
In fascicle, in white sauce cold granules standard, its thin-layer identification method is established, the present invention studies early stage, respectively according to above-mentioned side
The development system of method is tested, and is compared according to experiment, and the technical scheme that the present invention is established, separating effect is than the above method more
It is good, RfValue is more moderate, and spot is apparent.
Contrast test 2
White hardship is taken to lose dysentery oral liquid sample, the negative sample without field pennycress and field pennycress control medicinal material according to reference to text
Offer (Tang's Yi, Dong Lin, remaining dawn qin Baijiang Tablets quality standard research Chinese patent drugs .2008,30 (2):223~226) field pennycress reflects in
Other method carries out indentification by TLC experiment.The test sample lamellae done is sprayed into 10% ethanol solution of sulfuric acid, is heated to spot
Colour developing is clear, is inspected under ultraviolet lamp (365nm), it was observed that test sample chromatogram seems with control medicinal material chromatogram corresponding position
Spottiness is shown, but separating effect is bad, and feminine gender has interference, as a result sees Fig. 2.
By adjustment solvent n-hexane ﹣ ethyl acetate ﹣ formic acid (15: 5: 0.5), 10% ethanol solution of sulfuric acid, heating are sprayed
It is clear to spot development, inspected under ultraviolet lamp (365nm), as a result spot obscures (Fig. 3-1), sprays 5% vanillin-sulfuric acid solution,
It is clear to be heated to spot development, is inspected under daylight, on the test sample that as a result mays be seen indistinctly position corresponding with control medicinal material chromatogram, has
The spot of same color is shown, and inferior separating effect (Fig. 3-2)；Adjustment solvent be n-hexane ﹣ ethyl acetate ﹣ formic acid (15: 5:
1) 5% vanillin-sulfuric acid solution, is sprayed, it is clear to be heated to spot development, is inspected under daylight, as a result test sample and control medicinal material chromatogram
On corresponding position, the spot for having same color is shown, but edge effect is serious, and inferior separating effect (Fig. 4)；Adjust solvent
For toluene ﹣ ethyl acetate ﹣ formic acid (15: 2: 0.5), as a result on test sample position corresponding with control medicinal material chromatogram, indistinctly there is phase
Spot with color is shown, but RfIt is worth higher (Fig. 5)；Adjustment solvent is toluene ﹣ ethyl acetate ﹣ formic acid (10: 1: 0.5), knot
On fruit test sample position corresponding with control medicinal material chromatogram, the spot for having same color is shown, but RfIt is worth still higher (Fig. 6)；Adjust
Whole solvent is toluene ﹣ ethyl acetate ﹣ formic acid (5: 1: 0.5), as a result on test sample position corresponding with control medicinal material chromatogram, is had
The spot of same color is shown, but RfValue does not improve (Fig. 7).
On the basis of this technical scheme, adjustment solvent is toluene ﹣ ethyl acetate ﹣ formic acid (15: 2: 0.5), is inspected
The result arrived itself and inferior separating effect；Solvent is adjusted to toluene-ethyl acetate (10:1), another groove adds isometric ammoniacal liquor and satisfied
With achieve unexpected effect：In test sample chromatogram, on position corresponding with control medicinal material chromatogram, show same color
Spot, clear spot, good separating effect is negative noiseless, as a result sees Fig. 8.
Contrast test 3
Indentification by TLC inspection has been carried out to oneself the several Chinese medicine compound prescription kinds of listing using the method for the present invention, obtained
The results are shown in Table 1, accompanying drawing 8-12.As a result prove that technical solutions according to the invention can be widely applied in the market and contain field pennycress
Technique be boiling Chinese medicine compound prescription kind indentification by TLC, and positive effect is better than prior art.
Table 1 carries out the effect of field pennycress discriminating according to prior art and technical solution of the present invention to oneself listing Chinese medicine compound prescription kind
Fruit is compared
Although above with general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.
Claims (5)
- A kind of 1. discrimination method of field pennycress in Chinese medicine compound prescription, it is characterised in that：The discrimination method comprises the following steps：（1）The preparation of control medicinal material solution：Field pennycress control medicinal material is taken, adds water, is decocted, filtering, filtrate concentration, adds ethyl acetate Extraction, combined ethyl acetate liquid, is evaporated, residue adds methanol to make dissolving, as control medicinal material solution；（2）The preparation of need testing solution：Take testing sample；Or testing sample is taken, and add water to cook, filter, filtrate concentration；Or take and treat Test sample product, add hot water dissolving, filter, take filtrate；Add ethyl acetate to extract, combined ethyl acetate liquid, be evaporated, residue adds methanol to make Dissolving, as need testing solution；（3）The preparation of negative sample solution：Other medicinal materials of scarce field pennycress are taken in testing sample prescription ratio, preparation is free of Patrinia scaniosaefolia Grass compound Chinese medicinal preparation, take with testing sample equal amount, according still further to step（2）In after " taking testing sample ", same to method Operation, gained methanol lysate is negative sample solution；（4）It is each that μ L of control medicinal material solution 0.1 ~ 20, need testing solution and negative sample solution are drawn respectively with capillary sample applicator 0.1 ~ 50 μ L, put successively on same silica gel g thin-layer plate；（5）By toluene, ethyl acetate according to volume ratio be 10:1 is well mixed, and another groove puts isometric ammoniacal liquor, as solvent, It is placed in the chromatography cylinder of dried and clean, by step（4）Obtained lamellae is placed in chromatography cylinder, is deployed, and is taken out, is dried；（6）Chromatographic sheet is inspected, is differentiated to obtaining result；The testing sample for infirmity clear piece, QianLieping jiaonang, Golden Horse liver Thailand particle, comfortable wash liquid for hemorrhoids, white hardship lose dysentery oral liquid or White sauce cold granules.
- 2. discrimination method according to claim 1, it is characterised in that：The step（1）The middle amount for adding water is field pennycress 5 ~ 500 times of control medicinal material quality；Filtrate is concentrated into 1 ~ 50 times of field pennycress control medicinal material quality；Add ethyl acetate amount be Step（1）0.1 ~ 10 times of middle concentrate quality.
- 3. discrimination method according to claim 1, it is characterised in that：The step（2）It is middle add ethyl acetate amount be 0.1 ~ 100 times of testing sample volume.
- 4. discrimination method according to claim 1, it is characterised in that：The step（6）In inspect chromatographic sheet for spray With 5% vanillin-sulfuric acid solution, it is clear to be heated to spot development, is inspected under daylight.
- 5. discrimination method according to claim 1, it is characterised in that the discrimination method is carried out according to the following steps：（1）The preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, adds water 150ml, decocts half an hour, is filtered, filtrate is dense 30ml is reduced to, adds ethyl acetate to extract 2 times, each 20ml, combined ethyl acetate liquid, is evaporated, residue adds the ml of methanol 1 to make dissolving, As field pennycress control medicinal material solution；（2）The preparation of need testing solution：When testing sample is liquid, the testing sample liquid equivalent to the 2g of medicinal material containing field pennycress is taken, dilutes or is concentrated into 30ml, Add ethyl acetate to extract 2 times, each 20ml, combined ethyl acetate liquid, be evaporated, residue adds the ml of methanol 1 to make dissolving, as trying Product solution；When field pennycress technique is former powder, the testing sample powder equivalent to the 2g of medicinal material containing field pennycress is taken, adds 150ml water, decocted, Filtering, is concentrated into 30ml, adds ethyl acetate to extract 2 times, each 20ml, combined ethyl acetate liquid, is evaporated, residue adds the ml of methanol 1 Make dissolving, as need testing solution；When field pennycress technique for extraction when, take the testing sample powder equivalent to the 2g of medicinal material containing field pennycress, with 50ml hot water dissolvings, Filtering, takes filtrate, adds ethyl acetate to extract 2 times, each 20ml, combined ethyl acetate liquid, is evaporated, it is molten that residue adds the ml of methanol 1 to make Solution, as need testing solution；（3）The preparation of negative sample solution：Other medicinal materials of scarce field pennycress are taken in testing sample prescription ratio, preparation is free of Patrinia scaniosaefolia The compound Chinese medicinal preparation of grass, according still further to step（2）In from " taking the testing sample liquid or powder equivalent to the 2g of medicinal material containing field pennycress Rise, operated with method, gained methanol lysate is negative sample solution after end "；（4）Control medicinal material solution, need testing solution and each 1-20 μ L of negative sample solution are drawn respectively with capillary sample applicator, according to Secondary point is on same silica gel g thin-layer plate；（5）By toluene, ethyl acetate according to volume ratio be 10:1 is well mixed, and another groove puts isometric ammoniacal liquor, as solvent, It is placed in the chromatography cylinder of dried and clean, by step（4）Obtained lamellae is placed in chromatography cylinder, is deployed, and is taken out, is dried；（6）By step（5）Lamellae after drying is sprayed with 5% vanillin-sulfuric acid solution, and it is clear to be heated to spot development, under daylight Inspect, obtain thin-layer chromatogram, judged whether to contain field pennycress according to gained thin-layer chromatogram.
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