CN106501440A - 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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- CN106501440A CN106501440A CN201610936802.2A CN201610936802A CN106501440A CN 106501440 A CN106501440 A CN 106501440A CN 201610936802 A CN201610936802 A CN 201610936802A CN 106501440 A CN106501440 A CN 106501440A
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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
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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- 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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- G01N1/4055—Concentrating samples by solubility techniques
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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 in a kind of Chinese medicine compound prescription field pennycress discrimination method, the thin-layer identification method of field pennycress more particularly in Chinese medicine compound prescription.The discrimination method of the present invention is comprised 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, is launched with solvent, taken out, dry；Chromatographic sheet is inspected, result is obtained and is differentiated, test sample chromatogram shows the principal spot of same color on position corresponding with control medicinal material chromatogram, and negative sample is without this spot.The discrimination method process is simple of the present invention, good separating effect, with extremely strong specificity, further increase the accuracy of field pennycress Components identification in Chinese medicine compound prescription, and there are huge popularization and application potentiality in the medicine identification field relevant with field pennycress.
Description
Technical field
The present invention relates in Chinese medicine compound prescription field pennycress discrimination method, more particularly in Chinese medicine compound prescription field pennycress thin layer mirror
Other method.
Background technology
For field pennycress section plant patrinia scabiosaefolia Fiscs Patrinia scabiosaefolia Fisch. or patrima villosa
Patrinia villosa Juss. dry herb.Before summer, the flowers are in blossom, excavation, shines to half-dried, is bundled into beam, then dries in the shade.Main product in
Jiangsu, Zhejiang, Hubei, Anhui.Field pennycress has clearing heat and detoxicating, effect of removing blood stasis and expelling pus.Cure mainly appendicitis, dysentery, enteritis, liver
Inflammation, eye conjunctivitis, postpartum blood stasis are suffered from abdominal pain, carbuncle swells furunculosis.Field pennycress can also make plurality of Chinese compound product with other medicinal material compatibilities
Kind, such as 2015 infirmity clear pieces for recording, Baijiang Tablets, compound fuyanping capsules in document, palace of the Qing Dynasty liquid, wonderful of the seed of jog's tears six
Grain etc., also contains field pennycress in its prescription.The at present only enterprise's production of wherein infirmity clear piece, is exclusive kind, and sales volume is considerable.
Chinese medicine compound prescription kind in Chinese Pharmacopoeia containing field pennycress only has infirmity clear piece a kind of, not yet sets up field pennycress in its standard
Discrimination method.
Kind Baijiang Tablets (document 1 in document：Tang, Dong Lin, Yu Xiaoqin. Baijiang Tablets quality standard research. Chinese patent drug
.2008,30 (2):223～226), compound fuyanping capsules (document 2：Luo Yuhong, beam Feihua, yellow good force etc. compound woman is scorching flat
Capsule quality standard is controlled. Journal of Chinese Hospital Pharmacy .2009,29 (1)：73～75), Yiren Liumiao granule (document 3：Cao Ming
Into Chen Bin, Li Liubing etc. Yiren Liumiao granule quality standard research. R＆D of modern TCM with put into practice .2004,18 (5)：50～
52) discriminating of field pennycress thin layer is established.Applicant once using document in discrimination method dialogue hardship lose in dysentery oral liquid
Field pennycress carries out indentification by TLC, as a result shows that these methods can't check, and separating effect is also bad.At present, domestic and international centering
The quality control of medicine compound kind is more and more stricter, is therefore badly in need of finding a kind of stable, reliable, easy thin-layered chromatography, energy
Accurate and effective differentiates to field pennycress composition in Chinese medicine compound prescription.
Content of the invention
For prior art, the unused ethyl acetate of test sample preparation method, solvent used is mixed solution, but grinds
Study carefully these preparation methods of discovery and solvent, separation degree does 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 adopt ethyl acetate for solvent, and solvent is adopted
Use ammonia vapo(u)rous, the technical scheme of the field pennycress thin-layer chromatography, with simple and efficient to handle, good separating effect, specificity strong,
The advantages of being widely used, solves the problems, such as that prior art, the present invention are concurrently facilitated and improve the medicine relevant with field pennycress
Quality standard.
The present invention relates in a kind of Chinese medicine compound prescription field pennycress discrimination method, the discrimination method comprises the following steps：
(1) preparation of control medicinal material solution：Field pennycress control medicinal material is taken, is added water, decocted, filtered, filtrate concentrates, with for examination
Prepared by product solution manufacturing method, used as control medicinal material solution；
(2) preparation of need testing solution：Testing sample liquid, plus ethyl acetate extraction, combined ethyl acetate liquid is taken, is steamed
Dry, residue adds methyl alcohol to make dissolving, used 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 concentrates, plus second
Acetoacetic ester is extracted, and combined ethyl acetate liquid is evaporated, and residue adds methyl alcohol to make dissolving, used as need testing solution；
When testing sample is solid, and field pennycress technique heats water dissolves for, during extraction, taking testing sample, filters, takes filter
Liquid, plus ethyl acetate extraction, combined ethyl acetate liquid are evaporated, and residue adds methyl alcohol to make dissolving, used as need testing solution；
(3) preparation of negative sample solution：In other medicinal materials that testing sample prescription ratio takes scarce field pennycress, preparation is not contained
The compound Chinese medicinal preparation of field pennycress, takes and testing sample equal amount, according still further in step (2) after " taking testing sample ",
Operate with method, gained methyl alcohol 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, are put on same silica gel g thin-layer plate successively；
(5) toluene, ethyl acetate mixing are taken, and another groove is put equal-volume ammoniacal liquor saturation, as solvent, is placed in dried and clean
In chromatography cylinder, the lamellae that step (4) is obtained is placed in chromatography cylinder, is launched, taken out, dry；
(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 for adding water in 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 for adding ethyl acetate in step (2) is 1～100 times of testing sample volume.
Preferably, in the solvent in step (5), toluene, the volume ratio of ethyl acetate are 10:1, use equal-volume ammonia
Water saturation.
Preferably, after inspecting chromatographic sheet in step (6) for 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, add water 150ml, decoct half an hour, filtered, filter
Liquid is concentrated into 30ml, prepares 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, is diluted or is concentrated into
30ml, plus ethyl acetate extract 2 times, each 20ml, combined ethyl acetate liquid are evaporated, and residue adds methyl alcohol 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, plus 150ml water is taken,
Decoct, filter, be concentrated into 30ml, plus ethyl acetate is extracted 2 times, each 20ml, combined ethyl acetate liquid are evaporated, and residue adds first
Alcohol 1ml makes dissolving, used as need testing solution；
When field pennycress technique is for extracting, the testing sample powder equivalent to the 2g of medicinal material containing field pennycress is taken, 50ml hot water is used
Dissolving, filters, and takes filtrate, plus ethyl acetate is extracted 2 times, and each 20ml, combined ethyl acetate liquid are evaporated, and residue adds methyl alcohol 1ml
Dissolving is made, as need testing solution；
(3) preparation of negative sample solution：In other medicinal materials that testing sample prescription ratio takes scarce field pennycress, preparation is not contained
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 after powder ", operate with method, gained methyl alcohol lysate is negative sample solution；
(4) each 1-20 μ of control medicinal material solution, need testing solution and negative sample solution are drawn respectively with capillary sample applicator
L, is put on same silica gel g thin-layer plate successively；
(5) by toluene, ethyl acetate according to volume ratio be 10:1 is well mixed, and another groove puts equal-volume ammoniacal liquor, used as expansion
Agent, is placed in the chromatography cylinder of dried and clean, and the lamellae that step (4) is obtained is placed in chromatography cylinder, launches, and takes out, dries；
(6) lamellae after dry step (5) is sprayed with 5% vanillin-sulfuric acid solution, is heated to spot development clearly, day
Inspect under light, obtain thin-layer chromatogram, judged whether containing field pennycress according to gained thin-layer chromatogram.
The testing sample loses dysentery oral liquid, infirmity clear piece, QianLieping jiaonang, Golden Horse liver Thailand particle, hemorrhoid for white hardship and comfortably washes
Liquid or white sauce cold granules.
In Chinese medicine compound prescription of the present invention, the discrimination method of field pennycress has the advantage that：
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-methyl alcohol, chloroform-methanol-water etc., in conjunction with
Technical scheme of the present invention is compared by chromatogram 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 set up by the present invention, and separating effect is than upper
State method more preferably, RfValue is more moderate, and negative noiseless, specificity is strong, and method is simple.
2. indentification by TLC inspection has been carried out to oneself Chinese medicine compound prescription kinds of listing several using the method for the present invention, obtained
To the results are shown in Table 1, as a result prove technical solutions according to the invention can be widely applied on market containing field pennycress Chinese medicine
Compound kind indentification by TLC, and effect is substantially better than prior art.
Description of the drawings
Below in conjunction with the accompanying drawings the present invention is further detailed.
Fig. 1 is according to the field pennycress thin-layer chromatography photo obtained by document 1；Wherein, 1. 5 μ l of field pennycress control medicinal material, 2.
10 μ l of field pennycress control medicinal material, 3. 2 μ l of test sample, 4. 3 μ l of test sample, 5. 4 μ l of test sample, 6. 4 μ l of test sample, 7. feminine gender (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 heated to spot development clear, inspects under ultraviolet lamp (365nm).
Fig. 2 is the field pennycress thin-layer chromatography photo on the basis of document 1 obtained by adjustment solvent ratio；Wherein, 1. bear
2 μ l of tartaric acid reference substance, 2. 2 μ l of field pennycress control medicinal material, 3. feminine gender (scarce field pennycress) 2 μ l, 4～8. test sample, 1～5 μ l；Launch
System：Ethyl acetate hexane formic acid (30: 10: 0.5), inspection system：10% ethanol solution of sulfuric acid, is heated to spot development
Clearly, inspect under ultraviolet lamp (365nm).
Fig. 3 is the field pennycress thin-layer chromatography photo on the basis of document 1 obtained by adjustment solvent ratio；Wherein, 1. lose
Sauce grass 5 μ l of control medicinal material, 2. 2 μ l of test sample, 3. 2 μ l of test sample, 4. 2 μ l of test sample, 5. feminine gender (scarce field pennycress) 2 μ l；Launch
System：Ethyl acetate hexane formic acid (15: 5: 0.5)；The wherein inspection system of Fig. 3-1：10% ethanol solution of sulfuric acid is sprayed, plus
Heat is clear to spot development, inspects under ultraviolet lamp (365nm)；The wherein inspection system of Fig. 3-2：Spray 5% vanillin-sulfuric acid molten
Liquid, is heated to spot development clearly, inspects under daylight.
Fig. 4 is the field pennycress thin-layer chromatography photo on the basis of document 1 obtained by adjustment solvent ratio；Wherein, 1. lose
Sauce grass 5 μ l of control medicinal material, 2. 2 μ l of test sample, 3. 2 μ l of test sample, 4. 2 μ l of test sample, 5. feminine gender (scarce field pennycress) 2 μ l；Launch
System：Ethyl acetate hexane formic acid (15: 5: 1), inspection system：5% vanillin-sulfuric acid solution is sprayed, spot development is heated to
Clearly, inspect under daylight.
Fig. 5 is the field pennycress thin-layer chromatography photo on the basis of document 1 obtained by adjustment solvent ratio；Wherein, wherein,
1. 5 μ l of field pennycress control medicinal material, 2. 2 μ l of test sample, 3. 2 μ l of test sample, 4. 2 μ l of test sample, 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, spot is heated to
Colour developing is clear, inspects under daylight.
Fig. 6 is the field pennycress thin-layer chromatography photo on the basis of document 1 obtained by adjustment solvent ratio；Wherein, wherein,
1. 5 μ l of field pennycress control medicinal material, 2. 2 μ l of test sample, 3. 2 μ l of test sample, 4. 2 μ l of test sample, 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, spot is heated to
Colour developing is clear, inspects under daylight.
Fig. 7 is the field pennycress thin-layer chromatography photo on the basis of document 1 obtained by adjustment solvent ratio；Wherein, wherein,
1. 5 μ l of field pennycress control medicinal material, 2. 2 μ l of test sample, 3. 2 μ l of test sample, 4. 2 μ l of test sample, 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, spot is heated to
Colour developing is clear, inspects under daylight.
Fig. 8 is field pennycress thin layer photo in infirmity clear piece obtained by the present invention；Wherein, 1. field pennycress control medicinal material, 2～
4.20130226,5. negative (scarce field pennycress)；
Fig. 9 is field pennycress thin layer photo in QianLieping jiaonang obtained by the present invention；Wherein, 1. field pennycress control medicinal material, 2
～4.20140702,5. negative (scarce field pennycress)；
Figure 10 is field pennycress thin layer photo in 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 comfortable wash liquid for hemorrhoids obtained by the present invention；Wherein, 1. field pennycress control medicinal material,
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：Tolyl-acetic acid
Ethyl ester (10: 1), another groove put equal-volume ammoniacal liquor saturation；Inspection system：5% vanillin-sulfuric acid solution, is heated to spot development clear
Clear, inspect under daylight.
Specific embodiment
Following examples are used for the present invention to be described, but are not limited to the scope of the present invention.
Embodiment 1
In the Chinese medicine compound prescription of the present embodiment, the discrimination method of field pennycress is the indentification by TLC to field pennycress in infirmity clear piece：
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：0.6 gram is weighed per piece, and lot number is：20130226)；Silica G plate (100mm × 100mm, Haiyang Chemical Plant, Qingdao)；Other reagents
It is analysis pure.
2. method and result
(1) preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, add water 150ml, decoct half an hour, filtered, filter
Liquid is concentrated into 30ml, prepares 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 take supernatant, plus acetic acid
Ethyl ester is extracted 2 times, and each 20ml, combined ethyl acetate liquid are evaporated, and residue adds methyl alcohol 1ml to make dissolving, used as need testing solution；
(3) preparation of negative sample solution：In other medicinal materials that testing sample prescription ratio takes scarce field pennycress, preparation is not contained
The Chinese medicine compound prescription piece of field pennycress, according still further to from after " finely ground ", operating with method in step (2), gained methyl alcohol lysate is
Negative sample solution；
(4) 2 μ L of control medicinal material solution, need testing solution and each 1- of negative sample solution are drawn respectively with capillary sample applicator
10 μ L, are put on same silica gel g thin-layer plate successively；
(5) by toluene, ethyl acetate according to volume ratio be 10:1 is well mixed, and another groove puts equal-volume ammoniacal liquor, used as expansion
Agent, is placed in the chromatography cylinder of dried and clean, and the lamellae that step (4) is obtained is placed in chromatography cylinder, launches, and takes out, dries；
(6) lamellae after dry step (5) is sprayed with 5% vanillin-sulfuric acid solution, is heated to spot development clearly, day
Inspect 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
In the Chinese medicine compound prescription of the present embodiment, the discrimination method of field pennycress is the thin-layer chromatography to field pennycress in QianLieping jiaonang
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)；It is pure that other reagents are analysis.
2. method and result
(1) preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, add water 150ml, decoct half an hour, filtered, filter
Liquid is concentrated into 30ml, prepares with need testing solution preparation method, as field pennycress control medicinal material solution；
(2) preparation of need testing solution：
QianLieping jiaonang 3 is taken, content is poured out, heating water 30ml makes dissolving, is centrifuged, takes supernatant, plus ethyl acetate
Extraction 2 times, each 20ml, combined ethyl acetate liquid are evaporated, and residue adds methyl alcohol 1ml to make dissolving, used as need testing solution；
(3) preparation of negative sample solution：In other medicinal materials that testing sample prescription ratio takes scarce field pennycress, preparation is not contained
The Chinese medicine compound prescription liquid of field pennycress, according still further to from after " pouring out content ", operating with method in step (2), gained methyl alcohol is molten
Solution liquid is negative sample solution；
(4) 2 μ L of control medicinal material solution, need testing solution and each 1 μ of negative sample solution are drawn respectively with capillary sample applicator
L, is put on same silica gel g thin-layer plate successively；
(5) by toluene, ethyl acetate according to volume ratio be 10:1 is well mixed, and another groove puts equal-volume ammoniacal liquor, used as expansion
Agent, is placed in the chromatography cylinder of dried and clean, and the lamellae that step (4) is obtained is placed in chromatography cylinder, launches, and takes out, dries；
(6) lamellae after dry step (5) is sprayed with 5% vanillin-sulfuric acid solution, is heated to spot development clearly, day
Inspect 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
In the Chinese medicine compound prescription of the present embodiment, the discrimination method of field pennycress is the thin layer color to field pennycress in Golden Horse liver Thailand particle
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 (without sugarcane
Sugar), lot number is：20160301)；Silica G plate (100mm × 100mm, Haiyang Chemical Plant, Qingdao)；It is pure that other reagents are analysis.
2. method and result
(1) preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, add water 150ml, decoct half an hour, filtered, filter
Liquid is concentrated into 30ml, prepares with need testing solution preparation method, as field pennycress control medicinal material solution；
(2) preparation of need testing solution：
Golden Horse liver Thailand particle 18g is taken, heating water 30ml makes dissolving, is centrifuged, and takes supernatant, plus ethyl acetate is extracted 2 times, per
Secondary 20ml, combined ethyl acetate liquid, is evaporated, and residue adds methyl alcohol 1ml to make dissolving, used as need testing solution；
(3) preparation of negative sample solution：In other medicinal materials that testing sample prescription ratio takes scarce field pennycress, preparation is not contained
The compound Chinese medicinal preparation of field pennycress, according still further to from after " pouring out content ", operating with method in step (2), gained methyl alcohol is molten
Solution liquid is negative sample solution；
(4) 5 μ L of control medicinal material solution, need testing solution and each 5 μ of negative sample solution are drawn respectively with capillary sample applicator
L, is put on same silica gel g thin-layer plate successively；
(5) by toluene, ethyl acetate according to volume ratio be 10:1 is well mixed, and another groove puts equal-volume ammoniacal liquor, used as expansion
Agent, is placed in the chromatography cylinder of dried and clean, and the lamellae that step (4) is obtained is placed in chromatography cylinder, launches, and takes out, dries；
(6) lamellae after dry step (5) is sprayed with 5% vanillin-sulfuric acid solution, is heated to spot development clearly, day
Inspect 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
In the Chinese medicine compound prescription of the present embodiment, the discrimination method of field pennycress is the thin-layer chromatography to field pennycress in comfortable wash liquid for hemorrhoids
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
Analysis is pure.
2. method and result
(1) preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, add water 150ml, decoct half an hour, filtered, filter
Liquid is concentrated into 30ml, prepares 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, the 10ml that adds water dilutes, plus ethyl acetate is extracted 2 times, each 20ml, combined ethyl acetate
Liquid, is evaporated, and residue adds methyl alcohol 1ml to make dissolving, used as need testing solution；
(3) preparation of negative sample solution：In other medicinal materials that testing sample prescription ratio takes scarce field pennycress, preparation is not contained
The Chinese medicine compound prescription liquid of field pennycress, according still further to from " addition ethyl acetate ", operating with method in step (2), gained methyl alcohol dissolves
Liquid is negative sample solution；
(4) each 2 μ L of control medicinal material solution, need testing solution and negative sample solution are drawn respectively with capillary sample applicator,
Put on same silica gel g thin-layer plate successively；
(5) by toluene, ethyl acetate according to volume ratio be 10:1 is well mixed, and another groove puts equal-volume ammoniacal liquor, used as expansion
Agent, is placed in the chromatography cylinder of dried and clean, and the lamellae that step (4) is obtained is placed in chromatography cylinder, launches, and takes out, dries；
(6) lamellae after dry step (5) is sprayed with 5% vanillin-sulfuric acid solution, is heated to spot development clearly, day
Inspect 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
In the Chinese medicine compound prescription of the present embodiment, the discrimination method of field pennycress is the thin layer that dialogue hardship loses field pennycress in dysentery oral liquid
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：Per 1g equivalent to primary crude drug 0.5g, lot number is：20120501、20120502、20120503)；Silica G plate
(100mm × 100mm, Yantai Chemical Industry Research Inst.)；It is pure that other reagents are analysis.
2. method and result
(1) preparation of control medicinal material solution：Field pennycress control medicinal material 2g is taken, add water 150ml, decoct half an hour, filtered, filter
Liquid is concentrated into 30ml, prepares with need testing solution preparation method, as field pennycress control medicinal material solution；
(2) preparation of need testing solution：
Take white hardship and lose dysentery oral liquid 30ml, plus ethyl acetate is extracted 2 times, each 20ml, combined ethyl acetate liquid are evaporated,
Residue adds methyl alcohol 1ml to make dissolving, used as need testing solution；
(3) preparation of negative sample solution：In other medicinal materials that testing sample prescription ratio takes scarce field pennycress, preparation is not contained
The Chinese medicine compound prescription liquid of field pennycress, according still further to from " addition ethyl acetate ", operating with method in step (2), gained methyl alcohol dissolves
Liquid is negative sample solution；
(4) each 2 μ L of control medicinal material solution, need testing solution and negative sample solution are drawn respectively with capillary sample applicator,
Put on same silica gel g thin-layer plate successively；
(5) by toluene, ethyl acetate according to volume ratio be 10:1 is well mixed, and another groove puts equal-volume ammoniacal liquor, used as expansion
Agent, is placed in the chromatography cylinder of dried and clean, and the lamellae that step (4) is obtained is placed in chromatography cylinder, launches, and takes out, dries；
(6) lamellae after dry step (5) is sprayed with 5% vanillin-sulfuric acid solution, is heated to spot development clearly, day
Inspect 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 ()
In fascicle, in white sauce cold granules standard, its thin-layer identification method is established, the present invention is studied early stage, respectively according to above-mentioned side
The development system of method is tested, and is compared according to test, the technical scheme set up by the present invention, and separating effect is than said method more
Good, RfValue is more moderate, and spot is apparent.
Contrast test 2
Take white hardship dysentery oral liquid sample, the negative sample without field pennycress and field pennycress control medicinal material is lost according to reference text
Offer (Tang, Dong Lin, Yu Xiaoqin. Baijiang Tablets quality standard research. Chinese patent drug .2008,30 (2):223～226) in field pennycress mirror
Other method carries out indentification by TLC test.The test sample lamellae for being done is sprayed 10% ethanol solution of sulfuric acid, spot is heated to
Colour developing is clear, inspects, observe that test sample chromatogram is being seemed with control medicinal material chromatogram corresponding position under ultraviolet lamp (365nm)
Spottiness shows, but separating effect is not good, and feminine gender has interference, as a result sees Fig. 2.
By adjustment solvent ethyl acetate hexane formic acid (15: 5: 0.5), 10% ethanol solution of sulfuric acid, heating is sprayed
Clear to spot development, inspect under ultraviolet lamp (365nm), as a result spot is fuzzy (Fig. 3-1), sprays 5% vanillin-sulfuric acid solution,
It is heated to spot development clear, inspects under daylight, on the test sample that as a result mays be seen indistinctly position corresponding with control medicinal material chromatogram, have
The spot of same color shows, and inferior separating effect (Fig. 3-2)；Adjustment solvent be ethyl acetate hexane formic acid (15: 5:
1) 5% vanillin-sulfuric acid solution is sprayed, spot development is heated to clearly, is inspected under daylight, as a result test sample and control medicinal material chromatogram
On corresponding position, the spot for having same color shows, but edge effect is serious, and inferior separating effect (Fig. 4)；Adjustment 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
Show with the spot of color, but RfIt is worth higher (Fig. 5)；Adjustment solvent is toluene ethyl acetate formic acid (10: 1: 0.5), ties
On fruit test sample position corresponding with control medicinal material chromatogram, the spot for having same color shows, 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, has
The spot of same color shows, 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), inspects
The result for arriving itself and inferior separating effect；Solvent is adjusted to toluene-ethyl acetate (10:1), another groove adds equal-volume ammoniacal liquor to satisfy
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 is carried out to oneself Chinese medicine compound prescription kinds of listing several using the method for the present invention, has been 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 to contain field pennycress on market
The Chinese medicine compound prescription kind indentification by TLC that boils for water of technique, and effect is substantially 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, the present invention is described in detail above to have used general explanation and specific embodiment, 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, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (8)
1. in a kind of Chinese medicine compound prescription field pennycress discrimination method, it is characterised in that：The discrimination method is comprised the following steps：
(1) preparation of control medicinal material solution：Field pennycress control medicinal material is taken, is added water, decocted, filtered, filtrate concentrates, molten with test sample
Prepared by liquid and preparation method thereof, used as control medicinal material solution；
(2) preparation of need testing solution：Take testing sample；Or testing sample is taken, and adding water to cook, filter, filtrate concentrates；Or take and treat
Test sample product, heat water dissolves, filter, take filtrate；Plus ethyl acetate is extracted, combined ethyl acetate liquid is evaporated, and residue adds methyl alcohol to make
Dissolving, used as need testing solution；
(3) preparation of negative sample solution：In other medicinal materials that testing sample prescription ratio takes scarce field pennycress, prepare and do not contain Patrinia scaniosaefolia
The compound Chinese medicinal preparation of grass, takes and testing sample equal amount, according still further in step (2) from " taking testing sample " afterwards, same to method
Operation, gained methyl alcohol lysate are negative sample solution；
(4) it is each 0.1～20 μ L of control medicinal material solution, need testing solution and negative sample solution to be drawn respectively with capillary sample applicator
0.1～50 μ L, are put on same silica gel g thin-layer plate successively；
(5) toluene, ethyl acetate mixing are taken, and another groove is put equal-volume ammoniacal liquor saturation, as solvent, is placed in the chromatography of dried and clean
In cylinder, the lamellae that step (4) is obtained is placed in chromatography cylinder, is launched, taken out, dry；
(6) chromatographic sheet is inspected, is differentiated to obtaining result；
The testing sample is the compound Chinese medicinal preparation containing field pennycress.
2. discrimination method according to claim 1, it is characterised in that：The amount for adding water in step (1) 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 the amount of ethyl acetate
0.1～10 times for concentrate quality in step (1).
3. discrimination method according to claim 1, it is characterised in that：In step (2), the amount of addition ethyl acetate is
0.1～100 times of testing sample volume.
4. discrimination method according to claim 1, it is characterised in that：Toluene, acetic acid in solvent in step (5)
The volume ratio of ethyl ester is 9～11:0.1～2, another groove puts equal-volume ammoniacal liquor saturation.
5. discrimination method according to claim 1, it is characterised in that：Toluene, acetic acid in solvent in step (5)
The volume ratio of ethyl ester is 10:1, another groove puts equal-volume ammoniacal liquor saturation.
6. discrimination method according to claim 1, it is characterised in that：Chromatographic sheet is inspected in step (6) for spray
With 5% vanillin-sulfuric acid solution, it is heated to spot development clearly, inspects under daylight.
7. discrimination method according to claim 1, it is characterised in that 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, add water 150ml, decoct half an hour, filtered, filtrate is dense
30ml is reduced to, 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, is diluted or is concentrated into 30ml,
Plus ethyl acetate is extracted 2 times, each 20ml, combined ethyl acetate liquid are evaporated, and residue adds methyl alcohol 1ml to make dissolving, used as test sample
Solution；
When field pennycress technique is former powder, the testing sample powder equivalent to the 2g of medicinal material containing field pennycress, plus 150ml water is taken, is decocted,
Filter, be concentrated into 30ml, plus ethyl acetate is extracted 2 times, each 20ml, combined ethyl acetate liquid are evaporated, and residue adds methyl alcohol 1ml
Dissolving is made, as need testing solution；
When field pennycress technique is for extracting, the testing sample powder equivalent to the 2g of medicinal material containing field pennycress is taken, 50ml hot water dissolvings are used,
Filter, take filtrate, plus ethyl acetate is extracted 2 times, each 20ml, combined ethyl acetate liquid are evaporated, and it is molten that residue adds methyl alcohol 1ml to make
Solution, used as need testing solution；
(3) preparation of negative sample solution：In other medicinal materials that testing sample prescription ratio takes scarce field pennycress, prepare and do not contain Patrinia scaniosaefolia
The compound Chinese medicinal preparation of grass, " takes the testing sample liquid or powder equivalent to the 2g of medicinal material containing field pennycress certainly according still further in step (2)
Rise after end ", operate with method, gained methyl alcohol lysate is negative sample solution；
(4) each 1-20 μ L of control medicinal material solution, need testing solution and 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 equal-volume ammoniacal liquor, as solvent, puts
In the chromatography cylinder of dried and clean, the lamellae that step (4) is obtained is placed in chromatography cylinder, is launched, taken out, dry；
(6) lamellae after dry step (5) is sprayed with 5% vanillin-sulfuric acid solution, is heated to spot development clearly, under daylight
Inspect, obtain thin-layer chromatogram, judged whether containing field pennycress according to gained thin-layer chromatogram.
8. discrimination method according to claim 1, it is characterised in that：The testing sample be infirmity clear piece, QianLieping jiaonang,
Golden Horse liver Thailand particle, comfortable wash liquid for hemorrhoids, white hardship lose dysentery oral liquid, white sauce cold granules.
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