CN102692466A - Detection method of Jizhong Tincture - Google Patents
Detection method of Jizhong Tincture Download PDFInfo
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- CN102692466A CN102692466A CN2012100891755A CN201210089175A CN102692466A CN 102692466 A CN102692466 A CN 102692466A CN 2012100891755 A CN2012100891755 A CN 2012100891755A CN 201210089175 A CN201210089175 A CN 201210089175A CN 102692466 A CN102692466 A CN 102692466A
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Abstract
The invention discloses a detection method of Jizhong Tincture. The Jizhong Tincture is a Chinese medicinal preparation comprising Camphora, Mentholum, Cortex Cinnamomi, Fructus Amomi, Capsici Fructus, Radix Et Rhizoma Rhei, Herba Agastaches, Dried Zingiberis Rhizoma and Fructus Foeniculi. The detection method comprises content determination of Camphora and/or Mentholum by gas chromatography (GC); and identification of Camphora, Mentholum, Radix Et Rhizoma Rhei, Herba Agastaches and Cortex Cinnamomi by thin layer chromatography (TLC). The detection method provided by the invention performs qualitative and quantitative research on Chinese medicinal materials and main ingredients of Jizhong Tincture, thereby guaranteeing effectiveness of the Jizhong Tincture.
Description
Technical field
The invention belongs to field of traditional Chinese, particularly a kind of detection method of many tinctures that help.
Background technology
Many tinctures that help record in " the 15 in Drug Standard of Ministry of Public Health of the Peoples Republic of China Chinese traditional patent formulation preparation " (WS3-B-2960-98); Form by camphor, menthol, Chinese cassia tree, fructus amomi, capsicum, rheum officinale, Pogostemon cablin, rhizoma zingiberis, fennel seeds 9 flavor Chinese crude drugs; Has relieving the exterior syndrome with drugs pungent in flavor and warm in property; Eliminating cold to stop pain, the effect of dampness elimination appetizing; Be used for because of dizziness that heatstroke causes, feel sick, symptom such as stomachache.
This researchist analyzes the said preparation ministerial standard, and the quality standard content is a proterties, amount of alcohol inspection and tincture general inspection; Through document research, the report of the aspect of the many tincture detection method researchs of not relevant Ji as yet; Portion's version standard does not have the qualitative and quantitative detection of corresponding medicinal material, causes the control of this standard low.Existing quality standard is simple, can not effectively control its product inherent quality, makes that different manufacturers many tincture mass discrepancies of helping are bigger, has influenced the product curative effect to a certain extent.For guaranteeing product quality and curative effect, the many tincture detection methods of new Ji are set up in this research, are in particular in: 1) adopt thin-layer chromatography to set up the discriminating of camphor, menthol, rheum officinale, Pogostemon cablin and Chinese cassia tree; 2) adopt gas chromatography to set up the content assaying method of camphor, menthol.The foundation of this method effectively improves the many tincture quality of Ji, guarantees the product curative effect.
Summary of the invention
The detection method that the purpose of this invention is to provide a kind of many tinctures that help.
Concrete technical scheme is following:
A kind of detection method of many tinctures that help; The Chinese medicine preparation that the many tinctures of said Ji are made up of camphor, menthol, Chinese cassia tree, fructus amomi, capsicum, rheum officinale, Pogostemon cablin, rhizoma zingiberis, fennel seeds, this detection method comprise employing gas Chromatographic Determination camphor and/or menthol content and adopt thin-layer chromatography to differentiate camphor, menthol, rheum officinale, Pogostemon cablin and Chinese cassia tree;
The step of said employing gas Chromatographic Determination camphor and/or menthol content is following:
(1) preparation of inner mark solution: it is an amount of to get cyclohexanone, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains 1～5mg cyclohexanone, promptly gets inner mark solution;
(2) preparation of reference substance solution: it is an amount of to get the camphor reference substance, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains 1～10mg camphor reference substance, promptly gets; It is an amount of that other gets the menthol reference substance, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains 0.5～6mg menthol reference substance, promptly gets;
(3) correction factor is measured: draw camphor reference substance solution and each 2ml of menthol reference substance solution respectively, put in the measuring bottle, add inner mark solution 1ml, adding 70% ethanol to cumulative volume is 10ml, shakes up, and draws 1 μ l inject gas chromatograph, the calculation correction factor;
(4) preparation of need testing solution: measure the many tincture 0.1～5ml of Ji, put in the measuring bottle, add inner mark solution 1ml, adding 70% ethanol to cumulative volume is 10ml, shakes up, and promptly gets;
(5) gas Chromatographic Determination method: accurate respectively reference substance solution and the need testing solution drawn, inject gas chromatograph is measured; Wherein chromatographic condition is: fused-silica capillary column; Column temperature temperature programme, injector temperature are 230～250 ℃, and detector temperature is 230～250 ℃; Split ratio 10～50: 1;
Said employing thin-layer chromatography differentiates that the step of camphor, menthol, rheum officinale, Pogostemon cablin and Chinese cassia tree is following:
(1) with the camphor reference substance, processes reference substance solution; Get the many tinctures of Ji as need testing solution; Adopting sodium carboxymethyl cellulose is the silica G or the GF254 thin layer plate of binder; Be 8～9: 2～1 cyclohexane with volume ratio: ethyl acetate or volume ratio are 28～29: 2～1 sherwood oil: ethyl acetate is developping agent; Launch, dry, it is smoked clear to the spot colour developing to put in the iodine vapor;
(2) be reference substance with the menthol, process reference substance solution; Get the many tinctures of Ji as need testing solution; Adopting sodium carboxymethyl cellulose is the silica gel g thin-layer plate of binder; Be 17～18: 3～2 normal hexane with volume ratio: ethyl acetate or volume ratio are 4～5: 2～1 sherwood oil: ethyl acetate is developping agent; Launch; Dry, spray is with 1-5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing at 105 ℃;
(3) be contrast with rheum officinale control medicinal material and/or archen and/or Chrysophanol and/or Rhein, process control medicinal material and/or reference substance solution respectively; Get the many tincture 10～50ml of Ji, add water 20ml, with extracted with diethyl ether 2～5 times, combined ether layer, water bath method, residue adds acetic acid ethyl dissolution, as need testing solution; Adopting sodium carboxymethyl cellulose is the silica gel g thin-layer plate of binder; With volume ratio is 14～15: 6～5: 0.5～1 sherwood oil: ethyl formate: glacial acetic acid or volume ratio are 28～30: 10～12: 0.5～1 normal hexane: ethyl acetate: formic acid is developping agent; Launch; Dry, put under the ultraviolet lamp (254nm+365nm) and inspect, show orange-yellow fluorescence spot;
(4) be contrast with Pogostemon cablin control medicinal material and/or patchouli alcohol, process control medicinal material and/or reference substance solution respectively; Get the many tincture 10～50ml of Ji, add the sherwood oil jolting and extract 2～5 times, each 20ml merges sherwood oil liquid, volatilizes, and residue adds acetic acid ethyl dissolution, as need testing solution; Adopting sodium carboxymethyl cellulose is the silica gel g thin-layer plate of binder; Be 14～12: 2～4 cyclohexane with volume ratio: acetone or volume ratio are 9～10: 1～0.5 toluene: ethyl acetate is developping agent, launches, and dries; Spray is heated to the spot colour developing with 1-5% vanillic aldehyde sulfuric acid solution at 105 ℃;
(5) be contrast with Chinese cassia tree control medicinal material and/or cinnaldehydrum, process control medicinal material solution; Get the many tincture 10～50ml of Ji, water-bath concentrates, with extracted with diethyl ether 2～5 times, combined ether layer, and evaporate to dryness, residue adds acetic acid ethyl dissolution, as need testing solution; Adopting sodium carboxymethyl cellulose is the silica gel g thin-layer plate of binder; Be 15～18: 5～2 sherwood oil with volume ratio: ethyl acetate or volume ratio are 4～5: 2～1 normal hexane: ethyl acetate is developping agent; Launch, dry, spray develops the color with 0.5-2% dinitrophenylhydrazine ethanolic solution.
Among embodiment, chromatographic condition is in said employing gas Chromatographic Determination camphor and/or the menthol content step: fused-silica capillary column therein; The column temperature temperature programme: 80 ℃ of initial temperatures, kept 1 minute, be warming up to 120 ℃ with the speed of 8 ℃ of per minutes, the speed with 15 ℃ of per minutes is warming up to 180 ℃ again, keeps 2 minutes, rises to 220 ℃ with the speed of 30 ℃ of per minutes, keeps 3 minutes; Injector temperature is 250 ℃, and detector temperature is 250 ℃; Split ratio 10～50: 1.
Among some embodiment, said camphor thin-layer chromatography discrimination method is following: get the camphor reference substance, add petroleum ether solution, as reference substance solution therein; Get the many tinctures of Ji as need testing solution; According to thin-layered chromatography test, draw need testing solution, reference substance solution, put respectively in same be on the silica G or GF254 thin layer plate of binder with the sodium carboxymethyl cellulose; With volume ratio is the cyclohexane that is at 9: 1: ethyl acetate or volume ratio are 28: 1 sherwood oil: ethyl acetate is developping agent, launches, and takes out; Dry, it is smoked clear to the spot colour developing to put in the iodine vapor, in the test sample chromatogram; With the corresponding position of reference substance chromatogram on, show the spot of same color.
Among some embodiment, said menthol thin-layer chromatography discrimination method is following: get the menthol reference substance, add petroleum ether dissolution, as reference substance solution therein; Get the many tinctures of Ji as need testing solution; According to thin-layered chromatography test, draw need testing solution, reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Be 17: 3 normal hexane with volume ratio: ethyl acetate or volume ratio are 5: 1 sherwood oil: ethyl acetate is developping agent, launches, and takes out; Dry, spray is with 2% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
Among some embodiment, said rheum officinale thin-layer chromatography discrimination method is following therein: get the rheum officinale control medicinal material, added the methyl alcohol sonicated 15～45 minutes, filter, concentrate, process rheum officinale control medicinal material solution; Get archen, Chrysophanol, Rhein reference substance, add dissolve with ethanol, as reference substance solution; Get the many tincture 10～50ml of Ji, add water 20ml, with extracted with diethyl ether 2～5, combined ether layer, water bath method, residue adds acetic acid ethyl dissolution, as need testing solution; According to the thin-layered chromatography test, draw above-mentioned reference substance solution and control medicinal material solution respectively, need testing solution; Put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be 14: 6: 1 sherwood oils with volume ratio: ethyl formate: glacial acetic acid or volume ratio are 30: 10: 0.5 normal hexane: ethyl acetate: formic acid is developping agent, launches; Exhibition is taken out apart from about 8cm, dries; Put under the ultraviolet lamp 254nm+365nm and inspect; In the test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show identical orange-yellow fluorescence spot.
Among some embodiment, said Pogostemon cablin thin-layer chromatography discrimination method is following therein: get the Pogostemon cablin control medicinal material, add the sherwood oil sonicated, filter, filtrating concentrates, as control medicinal material solution; Get the patchouli alcohol reference substance, add acetic acid ethyl dissolution, as reference substance solution; Get the many tincture 10～50ml of Ji, add the sherwood oil jolting and extract 2～5 times, each 20ml merges sherwood oil liquid, volatilizes, and residue adds acetic acid ethyl dissolution, as need testing solution; According to thin-layered chromatography test, draw need testing solution, reference substance solution and control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Be 12: 2 cyclohexane with volume ratio: acetone or volume ratio are 9: 1 toluene: ethyl acetate is developping agent, launches, and takes out; Dry; Spray is heated to the spot colour developing at 105 ℃, in the test sample chromatogram with 2% vanillic aldehyde sulfuric acid solution; With control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color.
Among some embodiment, said Chinese cassia tree thin-layer chromatography discrimination method is following therein: get the Chinese cassia tree control medicinal material, add the sherwood oil sonicated, filter, get filtrating concentrating, as control medicinal material solution; Other gets the cinnaldehydrum reference substance, adds anhydrous alcohol solution, as reference substance solution; Get the many tincture 10～50ml of Ji, water-bath concentrates, with extracted with diethyl ether 2～5 times, combined ether layer, and evaporate to dryness, residue adds acetic acid ethyl dissolution, as need testing solution; According to thin-layered chromatography test, draw need testing solution, control medicinal material solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Be 15: 5 sherwood oil with volume ratio: ethyl acetate or volume ratio are 5: 2 normal hexane: ethyl acetate is developping agent, launches, and takes out; Dry, spray is with 1% dinitrophenylhydrazine ethanolic solution, in the test sample chromatogram; With control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color.
Compared with prior art, the present invention has following beneficial effect:
1. the present invention adopts gas chromatography to set up the content assaying method of the many tincture leading indicator camphors of Ji, menthol; Adopt thin-layer chromatography to set up the discrimination method of main Chinese medicinal materials camphor, menthol, rheum officinale, Pogostemon cablin and Chinese cassia tree in the many tinctures of Ji; Qualitative identification the active ingredient emodin of rheum officinale, Chrysophanol, Rhein; The characteristic component patchouli alcohol of Pogostemon cablin, the characteristic component cinnamic acid of Chinese cassia tree; To many tincture Chinese crude drugs and the principal ingredient qualitative, quantitative research of helping, the validity of many tinctures that help guaranteeing helping;
2. the detection method set up of the present invention quality of many tinctures that systematically guaranteed from qualitative and quantitative aspect to help, the common quality standard system that constitutes the many tinctures of Ji, thereby control many tincture quality of helping effectively, the validity and the patients'benefit of assurance medication.
Description of drawings
Fig. 1 is camphor, menthol reference substance gas chromatogram;
Fig. 2 is the test sample gas chromatogram;
Fig. 3 is the thin-layer chromatogram of camphor;
Fig. 4 is the menthol thin-layer chromatogram;
Fig. 5 is the rheum officinale thin-layer chromatogram;
Fig. 6 is the Pogostemon cablin thin-layer chromatogram;
Fig. 7 is the Chinese cassia tree thin-layer chromatogram.
Embodiment
The Chinese medicine preparation that many tinctures that help are made up of camphor, menthol, Chinese cassia tree, fructus amomi, capsicum, rheum officinale, Pogostemon cablin, rhizoma zingiberis, fennel seeds.
Below specify the present invention through specific embodiment.
(1) preparation of inner mark solution: it is an amount of to get cyclohexanone, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains the 2mg cyclohexanone, promptly gets;
(2) preparation of reference substance solution: it is an amount of to get the camphor reference substance, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains 2mg camphor reference substance, promptly gets; It is an amount of that other gets the menthol reference substance, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains 1.5mg menthol reference substance, promptly gets;
(3) preparation of need testing solution: precision is measured the many tincture 0.2ml of Ji, puts in the 10ml measuring bottle, and the accurate inner mark solution 1ml that adds adds 70% ethanol to the 10ml scale, shakes up, and promptly gets;
(4) chromatographic condition is: chromatographic column: the ZB-FFAP quartz capillary chromatographic column (0.25mm * 30m, 0.25 μ m); Detecting device: hydrogen flame ionization detector; Column temperature: temperature programme, 80 ℃ of initial temperatures keep 1min, rise to 120 ℃ with 8 ℃/min heating rate, rise to 180 ℃ with 15 ℃/min again, keep 2min, rise to 220 ℃ with 30 ℃/min heating rate, keep 3min; Injector temperature and detector temperature: 230 ℃; Carrier gas: nitrogen, flow: 1ml/min; Sample size: 1 μ l; Split ratio: 30: 1; The camphor theoretical cam curve is 13000, and the menthol theoretical cam curve is 20000;
The collection of illustrative plates of gas chromatography gained is seen Fig. 1, Fig. 2, and wherein Fig. 1 is camphor, menthol reference substance chromatogram collection of illustrative plates, and Fig. 2 is the test sample chromatogram, and peak 1 is the cyclohexanone internal standard compound, and peak 2 is the camphor reference substance, peak 3 is the menthol reference substance;
(5) confirming of the preparation of typical curve and the range of linearity: precision is got reference substance storing solution configuration camphor reference substance 0.04044,0.1011,0.2022,0.3033,0.5055mg/ml respectively; The 70% ethanol reference substance solution that respectively contains cyclohexanone 0.2mg/ml; Draw 1 μ l respectively; Injecting chromatograph by above-mentioned chromatographic condition, is measured; Precision is got reference substance storing solution configuration menthol reference substance 0.04984,0.09968,0.1495,0.1994,0.2492mg/ml respectively, respectively contains the 70% ethanol reference substance solution of cyclohexanone 0.1790mg/ml, draws 1 μ l respectively; Injecting chromatograph; By above-mentioned chromatographic condition, measure, be horizontal ordinate with camphor concentration (C) or menthol concentration (C); The ratio (Ai/As) of the ratio of camphor and cyclohexanone peak area or menthol and cyclohexanone peak area is an ordinate, the drawing standard curve.Experimental result shows, camphor, menthol are good in concentration range internal linear separately, and the result sees table 1;
Table 1 typical curve and the range of linearity (n=5)
(6) stability test: get need testing solution (lot number DR9S001), at room temperature place different time and measure, the result shows that sample is comparatively stable in 24h, and the result sees table 2;
Table 2 stability test result
(7) replica test: get 7 parts in same lot number (DR9S001) sample, repeat test by the test sample preparation method, the result shows that the repeatability of method is good, and the result sees table 3;
Table 3 replica test result
(8) average recovery test: precision is got the sample 0.1ml of same lot number (DR9S001), and operation repetitive (contains camphor 0.9095mg for 6 parts; Menthol 0.5195mg), the reference substance 0.8424mg that camphorates respectively, menthol reference substance 0.4680mg and an amount of internal standard compound cyclohexanone are used 70% ethanol dilution; Constant volume is in the 10ml volumetric flask; Draw 1 μ l respectively, injecting chromatograph is by above-mentioned chromatographic condition; Measure, the result sees table 4, table 5;
The table 4 camphor recovery
The table 5 menthol recovery
(9) sample determination: get the many tincture samples of Ji of lot number DR9S001～DR9S010, press test sample preparation item method down, measure content, the result sees table 6;
Table 6 sample determination result
According to the experimental result of survey 10 lot sample article, consider factors such as big production and raw material fluctuation, the content limit of the many tinctures of tentative Ji is: these article contain camphor (C
10H
16O) every 1ml must not be less than 8mg; Contain menthol (C
10H
20O) every 1ml must not be less than 4mg.
(1) solution that every 1ml contains the 5mg cyclohexanone is processed in the preparation of inner mark solution;
(2) solution that every 1ml contains 10mg camphor reference substance is processed in the preparation of reference substance solution; Process the solution that every 1ml contains 6mg menthol reference substance;
(3) correction factor is measured accurate respectively draw camphor reference substance solution and each 1ml of menthol reference substance solution, puts in the 10ml measuring bottle, and the accurate inner mark solution 1ml that adds adds 70% ethanol to scale, shakes up, and draws 1 μ l inject gas chromatograph, the calculation correction factor.
(4) the preparation precision of need testing solution is measured the many tincture 5ml of Ji, puts in the 10ml measuring bottle, and the accurate inner mark solution 1ml that adds adds 70% ethanol to the 10ml scale, shakes up, and promptly gets;
(5) chromatographic condition is:
Chromatographic column: FFAP quartz capillary chromatographic column (0.25mm * 30m, 0.5 μ m);
The column temperature temperature programme: 90 ℃ of initial temperatures, keep 1min, rise to 150 ℃ with 6 ℃/min heating rate, rise to 200 ℃ with 10 ℃/min again, keep 2min;
Injector temperature and detector temperature: 250 ℃; Split ratio: 50: 1;
Other steps are with embodiment 1.
(1) solution that every 1ml contains the 1mg cyclohexanone is processed in the preparation of inner mark solution;
(2) solution 1 that every 1ml contains 1mg camphor reference substance is processed in the preparation of reference substance solution; Process the solution that every 1ml contains 0.5mg camphor reference substance;
(3) correction factor is measured accurate respectively draw camphor reference substance solution and each 2ml of menthol reference substance solution, puts in the 10ml measuring bottle, and the accurate inner mark solution 1ml that adds adds 70% ethanol to scale, shakes up, and draws 1 μ l inject gas chromatograph, the calculation correction factor.
(4) the preparation precision of need testing solution is measured these article 2ml, puts in the 10ml measuring bottle, and the accurate inner mark solution 1ml that adds adds 70% ethanol to the 10ml scale, shakes up, and promptly gets;
(5) chromatographic condition is:
Chromatographic column: FFAP quartz capillary chromatographic column (0.25mm * 30m, 0.5 μ m);
The column temperature temperature programme: 60 ℃ of initial temperatures, keep 1min, rise to 100 ℃ with 10 ℃/min heating rate, rise to 150 ℃ with 15 ℃/min again, keep 1min; Rise to 180 ℃ with 30 ℃/min heating rate, keep 3min;
Injector temperature and detector temperature: 240 ℃; Split ratio: 50: 1;
Other steps are with embodiment 1.
(1) preparation of contrast solution: get the camphor reference substance, add petroleum ether dissolution and process the camphor reference substance solution that 1ml contains 30mg;
(2) preparation of need testing solution: get the many tinctures of Ji as need testing solution;
(3) preparation of negative control solution: get the prescription medicinal material that lacks camphor in the recipe quantity ratio, prepare negative sample according to process.Get the negative sample that lacks camphor, directly as negative control solution;
(4) point sample, expansion, colour developing: drawing need testing solution 10 μ l, camphor reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, is developping agent with cyclohexane-ethyl acetate (9: 1); Launch; Take out, dry, it is smoked clear to the spot colour developing to put in the iodine vapor;
(5) result: in Fig. 3 camphor thin-layer chromatogram, S-camphor reference substance; The 1-many tinctures (lot number 1) that help; The 2-many tinctures (lot number 2) that help; The 3-many tinctures (lot number 3) that help; The 4-many tinctures (lot number 4) that help; The 5-many tinctures (lot number 5) that help; The B-negative control.The result shows in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color, the negative control chromatogram is noiseless on the relevant position, the thin-layer chromatography discrimination method of foundation can be used as the method for quality control of the many tinctures of Ji.
(1) preparation of contrast solution: with embodiment 4;
(2) preparation of need testing solution: with embodiment 4;
(3) preparation of negative control solution: with embodiment 4;
(4) point sample, expansion, colour developing: drawing need testing solution 10 μ l, camphor reference substance solution 2 μ l, put respectively on same silica GF254 thin layer plate, is developping agent with petroleum ether-ethyl acetate (28: 1); Launch; Take out, dry, it is smoked clear to the spot colour developing to put in the iodine vapor;
Other steps are with embodiment 4.
(1) contrast solution, need testing solution, the preparation of negative control solution is with embodiment 4;
(2) thin-layer chromatography condition contrast test: because of developping agent solvent system and ratio are the principal elements of thin layer identification experiment, this experiment adopts different developping agent solvent systems and solvent ratios to make an experiment, and developping agent is following: cyclohexane-ethyl acetate (8: 2); Cyclohexane-ethyl acetate (9: 2); Cyclohexane-ethyl acetate (8: 1), cyclohexane-ethyl acetate (10: 1), petroleum ether-ethyl acetate (29: 1); Petroleum ether-ethyl acetate (29: 2), petroleum ether-ethyl acetate (28: 2); Other thin-layer chromatography conditions are with embodiment 4;
(3) discuss: above developping agent experimental result is with embodiment 4, and many tincture camphors that can be used for helping become thin-layered discriminating.
(1) preparation of contrast solution: get the menthol reference substance, add petroleum ether dissolution and process the menthol reference substance solution that every 1ml contains 8mg;
(2) preparation of need testing solution: get the many tinctures of Ji as need testing solution;
(3) preparation of negative control solution: get the prescription medicinal material that lacks menthol in the recipe quantity ratio, prepare negative sample, get the negative sample that lacks menthol, directly as negative control solution according to process;
(4) point sample, expansion, colour developing: draw need testing solution 3 μ l, menthol reference substance solution 2 μ l; Putting respectively on same silica gel g thin-layer plate, is developping agent with normal hexane-ethyl acetate (17: 3), launches; Take out; Dry, spray is with 2% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing at 105 ℃;
(5) result: in Fig. 4 menthol thin-layer chromatogram, S-menthol reference substance; The 1-many tinctures (lot number 1) that help; The 2-many tinctures (lot number 2) that help; The 3-many tinctures (lot number 3) that help; The 4-many tinctures (lot number 4) that help; The 5-many tinctures (lot number 5) that help; B-negative control article.The result shows in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color, the negative control chromatogram is noiseless on the relevant position, the thin-layer chromatography discrimination method of foundation can be used as the method for quality control of the many tinctures of Ji.
(1) preparation of contrast solution: with embodiment 7;
(2) preparation of need testing solution: with embodiment 7;
(3) preparation of negative control solution: with embodiment 7;
(4) point sample, expansion, colour developing: draw need testing solution 3 μ l, menthol reference substance solution 2 μ l; Putting respectively on same silica gel g thin-layer plate, is developping agent with petroleum ether-ethyl acetate (5: 1), launches; Take out; Dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing at 105 ℃;
Other steps are with embodiment 7.
Embodiment 9 thin-layered chromatography are differentiated menthol composition in the many tinctures of Ji
(1) contrast solution, need testing solution, the preparation of negative control solution is with embodiment 7;
(2) thin-layer chromatography condition contrast test: because of developping agent solvent system and ratio are the principal elements of thin layer identification experiment, this experiment adopts different developping agent solvent systems and solvent ratios to make an experiment, and developping agent is following: normal hexane-ethyl acetate (18: 2); Normal hexane-ethyl acetate (17: 2); Normal hexane-ethyl acetate (18: 3), normal hexane-ethyl acetate (16: 3), petroleum ether-ethyl acetate (4: 2); Petroleum ether-ethyl acetate (5: 2), petroleum ether-ethyl acetate (4: 1); Developer is 1% vanillic aldehyde sulfuric acid solution; Other chromatographic conditions are with embodiment 7;
(3) discuss: above developping agent and developer experimental result are with embodiment 7, and many tincture menthols that can be used for helping become thin-layered discriminating.
(1) preparation of contrast solution: get rheum officinale control medicinal material 0.5g, added the methyl alcohol sonicated 15 minutes, filter, be concentrated into 2ml, process rheum officinale control medicinal material solution; Get archen, Chrysophanol, Rhein reference substance, add ethanol and process concentration and be the solution that every 1ml contains 1.5mg, as reference substance solution;
(2) preparation of need testing solution: get the many tincture 10ml of Ji, add water 20ml, with extracted with diethyl ether 5 times, combined ether layer, water bath method, residue adds acetic acid ethyl dissolution, as need testing solution;
(3) preparation of negative control solution: in the recipe quantity ratio, get the prescription medicinal material that lacks rheum officinale, prepare negative sample according to process.Get the negative sample that lacks rheum officinale, the preparation method processes negative control solution with method by test sample;
(4) point sample, expansion, colour developing: draw above-mentioned reference substance solution and control medicinal material solution 4 μ l respectively; Need testing solution 10 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be 14: 6: 1 sherwood oils with volume ratio: ethyl formate: glacial acetic acid is a developping agent; Launch; Take out, dry, put under the ultraviolet lamp (254nm+365nm) and inspect;
(5) result: in Fig. 5 rheum officinale thin-layer chromatogram, 1-Chrysophanol, archen, Rhein, aloe-emodin (successively from top to bottom) reference substance; 2-rheum officinale control medicinal material; The 3-many tinctures (lot number 1) that help; The 4-many tinctures (lot number 2) that help; The 5-many tinctures (lot number 3) that help; The 6-many tinctures (lot number 4) that help; The 7-many tinctures (lot number 5) that help; 8-rheum officinale negative control.The result shows in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show identical orange-yellow fluorescence spot, the negative control chromatogram is noiseless on the relevant position, the thin-layer chromatography discrimination method of foundation can be used as the method for quality control of the many tinctures of Ji.
Embodiment 11 thin-layered chromatography are differentiated rhubarb medicinal material in the many tinctures of Ji
(1) preparation of contrast solution: get rheum officinale control medicinal material 0.5g, added the methyl alcohol sonicated 45 minutes, filter, be concentrated into 2ml, process rheum officinale control medicinal material solution; Get archen, Chrysophanol, Rhein reference substance, add ethanol and process concentration and be the solution that every 1ml contains 3mg, as reference substance solution;
(2) preparation of need testing solution: get the many tincture 50ml of Ji, add water 20ml, with extracted with diethyl ether 2 times, combined ether layer, water bath method, residue adds acetic acid ethyl dissolution, as need testing solution;
(3) preparation of negative control solution: with embodiment 10;
(4) point sample, expansion, colour developing: draw above-mentioned reference substance solution and control medicinal material solution 1 μ l respectively; Need testing solution 4 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be 30: 10: 0.5 normal hexane with volume ratio: ethyl acetate: formic acid is developping agent; Launch; Take out, dry, put under the ultraviolet lamp (254nm+365nm) and inspect;
Other steps are with embodiment 10.
Embodiment 12 thin-layered chromatography are differentiated rhubarb medicinal material in the many tinctures of Ji
(1) preparation of contrast solution: get rheum officinale control medicinal material 0.5g, added the methyl alcohol sonicated 30 minutes, filter, be concentrated into 2ml, process rheum officinale control medicinal material solution; Get archen, Chrysophanol, Rhein reference substance, add ethanol and process concentration and be the solution that every 1ml contains 5mg, as reference substance solution;
(2) preparation of need testing solution: get the many tincture 30ml of Ji, add water 20ml, with extracted with diethyl ether 3 times, combined ether layer, water bath method, residue adds acetic acid ethyl dissolution, as need testing solution;
(4) preparation of negative control solution: with embodiment 10;
(5) thin-layer chromatography condition contrast test: because of developping agent solvent system and ratio are the principal elements of thin layer identification experiment; This experiment adopts different developping agent solvent systems and solvent ratios to make an experiment; Developping agent is following: sherwood oil: ethyl formate: glacial acetic acid (15: 6: 1), sherwood oil: ethyl formate: glacial acetic acid (14: 5: 1), sherwood oil: ethyl formate: glacial acetic acid (15: 5: 1); Normal hexane: ethyl acetate: formic acid (28: 10: 0.5); Normal hexane: ethyl acetate: formic acid (28: 12: 0.5), normal hexane: ethyl acetate: formic acid (28: 12: 1), normal hexane: ethyl acetate: formic acid (30: 10: 1); Normal hexane: ethyl acetate: formic acid (30: 12: 0.5), other chromatographic conditions are with embodiment 10;
(6) discuss: above developping agent and developer experimental result be with embodiment 10, and the thin layer of can be used for helping many tincture rhubarb medicinal materials and rheum officinale characteristic component is differentiated.
Embodiment 13 thin-layered chromatography are differentiated Pogostemon cablin medicinal material in the many tinctures of Ji
(1) preparation of contrast solution: get Pogostemon cablin control medicinal material 3g, add sherwood oil 20ml sonicated 30min, filter, filtrating is concentrated into 1ml, as control medicinal material solution; Get the patchouli alcohol reference substance, add the solution that ethyl acetate is processed 2mg/ml, as reference substance solution;
(2) preparation of need testing solution: get the many tincture 10ml of Ji, add the sherwood oil jolting and extract 5 times, each 20ml merges sherwood oil liquid, volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution;
(3) preparation of negative control solution: in the recipe quantity ratio, get the prescription medicinal material that lacks Pogostemon cablin, prepare negative sample according to process.Get the negative sample that lacks Pogostemon cablin, the preparation method processes negative control solution with method by test sample;
(4) point sample, expansion, colour developing: draw need testing solution 5 μ l, reference substance solution and control medicinal material solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Be 12: 2 cyclohexane with volume ratio: acetone is developping agent; Launch, take out, dry; Spray is heated to the spot colour developing with 2% vanillic aldehyde sulfuric acid solution at 105 ℃;
(5) result: in Fig. 6 Pogostemon cablin thin-layer chromatogram, 1-patchouli alcohol reference substance, 2-Pogostemon cablin control medicinal material; The 3-many tinctures (lot number 1) that help; The 4-many tinctures (lot number 2) that help; The 5-many tinctures (lot number 3) that help; The 6-many tinctures (lot number 4) that help; The 7-many tinctures (lot number 5) that help; 8-Pogostemon cablin negative control.The result shows in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show identical orange-yellow fluorescence spot, the negative control chromatogram is noiseless on the relevant position, the thin-layer chromatography discrimination method of foundation can be used as the method for quality control of the many tinctures of Ji.
Embodiment 14 thin-layered chromatography are differentiated Pogostemon cablin medicinal material in the many tinctures of Ji
(1) preparation of reference substance solution: with embodiment 13;
(2) preparation of need testing solution: get the many tincture 50ml of Ji, add the sherwood oil jolting and extract 2 times, each 20ml merges sherwood oil liquid, volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution;
(3) preparation of negative control solution: with embodiment 13;
(4) point sample, expansion, colour developing: draw need testing solution 5 μ l, reference substance solution and control medicinal material solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; With volume ratio is 9: 1 toluene: ethyl acetate is developping agent; Launch, take out, dry; Spray is heated to the spot colour developing with 1% vanillic aldehyde sulfuric acid solution at 105 ℃;
Other steps are with embodiment 13.
(1) preparation of reference substance solution: with embodiment 13;
(2) preparation of need testing solution: get the many tincture 30ml of Ji, add the sherwood oil jolting and extract 3 times, each 20ml merges sherwood oil liquid, volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution;
(3) preparation of negative control solution: with embodiment 13;
(4) thin-layer chromatography condition contrast test: because of developping agent solvent system and ratio are the principal elements of thin layer identification experiment, this experiment adopts different developping agent solvent systems and solvent ratios to make an experiment, and developping agent is following: cyclohexane: acetone (12: 4); Cyclohexane: acetone (14: 4); Cyclohexane: acetone (13: 2), cyclohexane: acetone (14: 2), toluene: ethyl acetate (10: 1); Toluene: ethyl acetate (10: 0.5), toluene: ethyl acetate (9: 0.5); Developer is 5% vanillic aldehyde sulfuric acid solution; Other chromatographic conditions are with embodiment 13;
(5) discuss: above developping agent and developer experimental result are with embodiment 13, and can be used for helping many tincture Pogostemon cablin medicinal materials and characteristic component thin layer are differentiated.
Embodiment 16 thin-layered chromatography are differentiated Chinese cassia tree medicinal material in the many tinctures of Ji
(1) preparation of reference substance solution: get the cinnaldehydrum reference substance, add ethanol and process the solution that concentration is 1 μ l/ml, as reference substance solution.Get Chinese cassia tree control medicinal material 2g, add sherwood oil 10ml, sonicated 20 minutes filters, and filtrating is as control medicinal material solution;
(2) preparation of need testing solution: get the many tincture 20ml of Ji, water bath method is to about 5ml, and water 15ml dissolves; Put in the separating funnel with extracted with diethyl ether 3 times each 20ml, combined ether layer; Put evaporate to dryness in the water-bath, residue adds ethyl acetate 1ml makes dissolving, as need testing solution;
(3) preparation of negative control solution: in the recipe quantity ratio, get the prescription medicinal material in misrun osmanthus, prepare negative sample according to process.Get the negative sample in misrun osmanthus, the preparation method processes negative control solution with method by test sample;
(4) point sample, expansion, colour developing: draw need testing solution 6 μ l, control medicinal material solution and reference substance solution 3 μ l; Put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Be 15: 5 sherwood oil with volume ratio: ethyl acetate is developping agent, launches, and takes out; Dry, spray is with 1% dinitrophenylhydrazine ethanolic solution;
(5) result: in Fig. 7 Chinese cassia tree thin-layer chromatogram, 1-cinnaldehydrum reference substance, 2-Chinese cassia tree control medicinal material; The 3-many tinctures (lot number 1) that help; The 4-many tinctures (lot number 2) that help; The 5-many tinctures (lot number 3) that help; The 6-many tinctures (lot number 4) that help; The 7-many tinctures (lot number 5) that help; 8-Chinese cassia tree negative control.The result shows in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show identical orange-yellow fluorescence spot, the negative control chromatogram is noiseless on the relevant position, the thin-layer chromatography discrimination method of foundation can be used as the method for quality control of the many tinctures of Ji.
Embodiment 17 thin-layered chromatography are differentiated Chinese cassia tree medicinal material in the many tinctures of Ji
(1) preparation of reference substance solution: get the cinnaldehydrum reference substance, add ethanol and process the solution that concentration is 2 μ l/ml, as reference substance solution; Get Chinese cassia tree control medicinal material 1g, add sherwood oil 20ml, sonicated 30 minutes filters, and filtrating is as control medicinal material solution;
(2) preparation of need testing solution: these article 50ml, water bath method be to about 5ml, and water 15ml dissolving is put in the separating funnel with extracted with diethyl ether 2 times, 20ml at every turn, and combined ether layer is put evaporate to dryness in the water-bath, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution;
(3) preparation of negative control solution: with embodiment 16;
(4) point sample, expansion, colour developing: draw need testing solution 10 μ l, control medicinal material solution and reference substance solution 5 μ l; Put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Be 5: 2 normal hexane with volume ratio: ethyl acetate is developping agent, launches, and takes out; Dry, spray is with 0.5% dinitrophenylhydrazine ethanolic solution;
Other steps are with embodiment 16.
Embodiment 18 thin-layered chromatography are differentiated Chinese cassia tree medicinal material in the many tinctures of Ji
(1) contrast solution, need testing solution, the preparation of negative control solution is with embodiment 16;
(2) thin-layer chromatography condition contrast test: because of developping agent solvent system and ratio are the principal elements of thin layer identification experiment; This experiment adopts different developping agent solvent systems and solvent ratios to compare test; Developping agent is following: sherwood oil: ethyl acetate (15: 3), sherwood oil: ethyl acetate (15: 2), sherwood oil: ethyl acetate (16: 5); Sherwood oil: ethyl acetate (18: 5); Normal hexane: ethyl acetate (4: 2), normal hexane: ethyl acetate (4: 1), normal hexane: ethyl acetate (5: 1); Developer is 2% dinitrophenylhydrazine ethanolic solution; Other chromatographic conditions are with embodiment 16;
(3) discuss: above developping agent and developer experimental result are with embodiment 16, and can be used for helping many tincture Chinese cassia tree medicinal materials and characteristic component thin layer are differentiated.
The above embodiment has only expressed several kinds of embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art under the prerequisite that does not break away from the present invention's design, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with accompanying claims.
Claims (7)
1. the detection method of many tinctures that help; The Chinese medicine preparation that the many tinctures of said Ji are made up of camphor, menthol, Chinese cassia tree, fructus amomi, capsicum, rheum officinale, Pogostemon cablin, rhizoma zingiberis, fennel seeds; It is characterized in that this detection method comprises employing gas Chromatographic Determination camphor and/or menthol content and adopts thin-layer chromatography to differentiate camphor, menthol, rheum officinale, Pogostemon cablin and Chinese cassia tree;
The step of said employing gas Chromatographic Determination camphor and/or menthol content is following:
(1) preparation of inner mark solution: it is an amount of to get cyclohexanone, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains 1～5mg cyclohexanone, promptly gets inner mark solution;
(2) preparation of reference substance solution: it is an amount of to get the camphor reference substance, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains 1～10mg camphor reference substance, promptly gets; It is an amount of that other gets the menthol reference substance, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains 0.5～6mg menthol reference substance, promptly gets;
(3) correction factor is measured: draw camphor reference substance solution and each 2ml of menthol reference substance solution respectively, put in the measuring bottle, add inner mark solution 1ml, adding 70% ethanol to cumulative volume is 10ml, shakes up, and draws 1 μ l inject gas chromatograph, the calculation correction factor;
(4) preparation of need testing solution: measure the many tincture 0.1～5ml of Ji, put in the measuring bottle, add inner mark solution 1ml, adding 70% ethanol to cumulative volume is 10ml, shakes up, and promptly gets;
(5) gas Chromatographic Determination method: accurate respectively reference substance solution and the need testing solution drawn, inject gas chromatograph is measured; Wherein chromatographic condition is: fused-silica capillary column; Column temperature temperature programme, injector temperature are 230～250 ℃, and detector temperature is 230～250 ℃; Split ratio 10～50: 1;
Said employing thin-layer chromatography differentiates that the step of camphor, menthol, rheum officinale, Pogostemon cablin and Chinese cassia tree is following:
(1) is reference substance with camphor, processes reference substance solution; Get the many tinctures of Ji as need testing solution; Adopting sodium carboxymethyl cellulose is the silica G or the GF254 thin layer plate of binder; Be 8～9: 2～1 cyclohexane with volume ratio: ethyl acetate or volume ratio are 28～29: 2～1 sherwood oil: ethyl acetate is developping agent; Launch, dry, it is smoked clear to the spot colour developing to put in the iodine vapor;
(2) be reference substance with the menthol, process reference substance solution; Get the many tinctures of Ji as need testing solution; Adopting sodium carboxymethyl cellulose is the silica gel g thin-layer plate of binder; Be 17～18: 3～2 normal hexane with volume ratio: ethyl acetate or volume ratio are 4～5: 2～1 sherwood oil: ethyl acetate is developping agent; Launch; Dry, spray is with 1-5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing at 105 ℃;
(3) be reference substance with rheum officinale control medicinal material and/or archen and/or Chrysophanol and/or Rhein, process control medicinal material and/or reference substance solution respectively; Get the many tincture 10～50ml of Ji, add water 20ml, with extracted with diethyl ether 2～5 times, combined ether layer, water bath method, residue adds acetic acid ethyl dissolution, as need testing solution; Adopting sodium carboxymethyl cellulose is the silica gel g thin-layer plate of binder; With volume ratio is 14～15: 6～5: 0.5～1 sherwood oil: ethyl formate: glacial acetic acid or volume ratio are 28～30: 10～12: 0.5～1 normal hexane: ethyl acetate: formic acid is developping agent; Launch; Dry, put under the ultraviolet lamp and inspect, show orange-yellow fluorescence spot;
(4) be reference substance with Pogostemon cablin control medicinal material and/or patchouli alcohol, process control medicinal material and/or reference substance solution respectively; Get the many tincture 10～50ml of Ji, add the sherwood oil jolting and extract 2～5 times, each 20ml merges sherwood oil liquid, volatilizes, and residue adds acetic acid ethyl dissolution, as need testing solution; Adopting sodium carboxymethyl cellulose is the silica gel g thin-layer plate of binder; Be 14～12: 2～4 cyclohexane with volume ratio: acetone or volume ratio are 9～10: 1～0.5 toluene: ethyl acetate is developping agent, launches, and dries; Spray is heated to the spot colour developing with 1-5% vanillic aldehyde sulfuric acid solution at 105 ℃;
(5) be contrast with Chinese cassia tree control medicinal material and/or cinnaldehydrum, process control medicinal material solution; Get the many tincture 10～50ml of Ji, water-bath concentrates, with extracted with diethyl ether 2～5 times, combined ether layer, and evaporate to dryness, residue adds acetic acid ethyl dissolution, as need testing solution; Adopting sodium carboxymethyl cellulose is the silica gel g thin-layer plate of binder; Be 15～18: 5～2 sherwood oil with volume ratio: ethyl acetate or volume ratio are 4～5: 2～1 normal hexane: ethyl acetate is developping agent; Launch, dry, spray develops the color with 0.5-2% dinitrophenylhydrazine ethanolic solution.
2. detection method according to claim 1 is characterized in that, chromatographic condition is in said employing gas Chromatographic Determination camphor and/or the menthol content step: fused-silica capillary column; The column temperature temperature programme: 80 ℃ of initial temperatures, kept 1 minute, be warming up to 120 ℃ with the speed of 8 ℃ of per minutes, the speed with 15 ℃ of per minutes is warming up to 180 ℃ again, keeps 2 minutes, rises to 220 ℃ with the speed of 30 ℃ of per minutes, keeps 3 minutes; Injector temperature is 250 ℃, and detector temperature is 250 ℃; Split ratio 10～50: 1.
3. detection method according to claim 1 is characterized in that, said camphor thin-layer chromatography discrimination method is following: get the camphor reference substance, add petroleum ether solution, as reference substance solution; Get the many tinctures of Ji as need testing solution; According to thin-layered chromatography test, draw need testing solution, reference substance solution, put respectively in same be on the silica G or GF254 thin layer plate of binder with the sodium carboxymethyl cellulose; With volume ratio is the cyclohexane that is at 9: 1: ethyl acetate or volume ratio are 28: 1 sherwood oil: ethyl acetate is developping agent, launches, and takes out; Dry, it is smoked clear to the spot colour developing to put in the iodine vapor, in the test sample chromatogram; With the corresponding position of reference substance chromatogram on, show the spot of same color.
4. according to each described detection method of claim 1-3, it is characterized in that said menthol thin-layer chromatography discrimination method is following: get the menthol reference substance, add petroleum ether dissolution, as reference substance solution; Get the many tinctures of Ji as need testing solution; According to thin-layered chromatography test, draw need testing solution, reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Be 17: 3 normal hexane with volume ratio: ethyl acetate or volume ratio are 5: 1 sherwood oil: ethyl acetate is developping agent, launches, and takes out; Dry, spray is with 2% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
5. according to each described detection method of claim 1-3, it is characterized in that said rheum officinale thin-layer chromatography discrimination method is following: get the rheum officinale control medicinal material, added the methyl alcohol sonicated 15～45 minutes, filter, concentrate, process rheum officinale control medicinal material solution; Get archen, Chrysophanol, Rhein reference substance, add dissolve with ethanol, as reference substance solution; Get the many tincture 10～50ml of Ji, add water 20ml, with extracted with diethyl ether 2～5 times, combined ether layer, water bath method, residue adds acetic acid ethyl dissolution, as need testing solution; According to the thin-layered chromatography test, draw above-mentioned reference substance solution and control medicinal material solution respectively, need testing solution; Put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be 14: 6: 1 sherwood oil with volume ratio: ethyl formate: glacial acetic acid or volume ratio are 30: 10: 0.5 normal hexane: ethyl acetate: formic acid is developping agent, launches; Exhibition is taken out apart from about 8cm, dries; Put under the ultraviolet lamp and inspect; In the test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show identical orange-yellow fluorescence spot.
6. according to each described detection method of claim 1-3, it is characterized in that said Pogostemon cablin thin-layer chromatography discrimination method is following: get the Pogostemon cablin control medicinal material, add the sherwood oil sonicated, filter, filtrating concentrates, as control medicinal material solution; Get the patchouli alcohol reference substance, add acetic acid ethyl dissolution, as reference substance solution; Get the many tincture 10～50ml of Ji, add the sherwood oil jolting and extract 2～5 times, each 20ml merges sherwood oil liquid, volatilizes, and residue adds acetic acid ethyl dissolution, as need testing solution; According to thin-layered chromatography test, draw need testing solution, reference substance solution and control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Be 12: 2 cyclohexane with volume ratio: acetone or volume ratio are 9: 1 toluene: ethyl acetate is developping agent, launches, and takes out; Dry; Spray is heated to the spot colour developing at 105 ℃, in the test sample chromatogram with 2% vanillic aldehyde sulfuric acid solution; With control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color.
7. according to each described detection method of claim 1-3, it is characterized in that said Chinese cassia tree thin-layer chromatography discrimination method is following: get the Chinese cassia tree control medicinal material, add the sherwood oil sonicated, filter, get filtrating concentrating, as control medicinal material solution; Other gets the cinnaldehydrum reference substance, adds anhydrous alcohol solution, as reference substance solution; Get the many tincture 10～50ml of Ji, water-bath concentrates, with extracted with diethyl ether 2～5 times, combined ether layer, and evaporate to dryness, residue adds acetic acid ethyl dissolution, as need testing solution; According to thin-layered chromatography test, draw need testing solution, control medicinal material solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Be 15: 5 sherwood oil with volume ratio: ethyl acetate or volume ratio are 5: 2 normal hexane: ethyl acetate is developping agent, launches, and takes out; Dry, spray is with 1% dinitrophenylhydrazine ethanolic solution, in the test sample chromatogram; With control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color.
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