CN103558330B - A kind of TLC distinguish chromatographic process of Jianwei Yuyang preparation - Google Patents
A kind of TLC distinguish chromatographic process of Jianwei Yuyang preparation Download PDFInfo
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Abstract
The invention discloses a kind of TLC distinguish chromatographic process of Jianwei Yuyang preparation, have changed radix bupleuri in Jianweiyuyang Tablets, corydalis tuber, indigo naturalis thin-layer identification method, and add Radix Glycyrrhizae TLC distinguish.5 TLC distinguish projects in existing " Chinese Pharmacopoeia " need process test sample respectively, launch respectively-develop the color-inspect with Mass Control, and complicated and loaded down with trivial details.6 TLC distinguish projects are shared need testing solution under pharmacopeia [discriminating] (2) item, are divided into four expansion-colour developing-review process by the present invention, save human and material resources and time, and present invention also adds the TLC distinguish of Radix Glycyrrhizae.TLC distinguish chromatographic process after the present invention improves, improves the quality control level of medicine, ensure that the safe and effective of medication.The TLC distinguish chromatographic process of Jianwei Yuyang preparation of the present invention, both can be used for controlling the quality of Jianweiyuyang Tablets, can be used to again to control other formulations of identical prescription as the quality of the formulation such as capsule, particle.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, be specifically related to a kind of method of quality control of Jianwei Yuyang preparation.
Background technology
Jianweiyuyang Tablets and Jianwei Yuyang Granule are all embodied in " Chinese Pharmacopoeia " 2010 editions, in its TLC Identification recorded 5 TLC distinguish projects (radix bupleuri, Radix Codonopsis, Paeoniflorin, corydalis tuber, indigo naturalis) test sample need be processed respectively, launch respectively-develop the color-inspect with Mass Control, this discrimination process is complicated, loaded down with trivial details, at substantial human and material resources, time.
Summary of the invention
The object of the present invention is to provide a kind of TLC distinguish chromatographic process of Jianwei Yuyang preparation, need testing solution only need be prepared with Same Way unification, also launch without the need to configuring separately test sample separately respectively-develop the color-inspect with Mass Control.In method after the present invention improves, 6 TLC distinguish projects (radix bupleuri, Radix Codonopsis, Paeoniflorin, corydalis tuber, indigo naturalis, Radix Glycyrrhizae) shared the need testing solution under pharmacopeia [discriminating] (2) item, be divided into four development system-colour developing-review process, greatly save human and material resources and time cost, and add the TLC distinguish of Radix Glycyrrhizae.TLC distinguish chromatographic process after improvement, improves the quality control level of medicine, ensure that security and the validity of people's medication.
For achieving the above object, the invention provides following technical scheme:
A TLC distinguish chromatographic process for Jianwei Yuyang preparation, comprises the steps:
(1) get this product 0.5 ~ 10g, porphyrize, add methyl alcohol 30 ~ 100ml, ultrasonic process 15 ~ 60 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 10 ~ 30ml, and heating makes dissolving, 2 times are extracted with water saturated normal butyl alcohol jolting, each 15 ~ 50ml, merges normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as need testing solution.Separately get radix bupleuri control medicinal material 0.2 ~ 1.0g, add water 50 ~ 250ml, decocts 0.5 ~ 2 hour, let cool, filter, filtrate evaporate to dryness, adds methyl alcohol 30 ~ 100ml, ultrasonic process 15 ~ 60 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 10 ~ 30ml, and heating makes dissolving, extract 2 times with water saturated normal butyl alcohol jolting, each 15 ~ 50ml, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as radix bupleuri control medicinal material solution.Extracting Radix Glycyrrhizae control medicinal material 0.2 ~ 1.0g, adds water-saturated n-butanol 10 ~ 30ml, and jolting 0.5 ~ 1.5 hour, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution.Test according to thin-layered chromatography (annex VIB), above-mentioned need testing solution, radix bupleuri control medicinal material solution, each 3 ~ 10 μ 1 of Radix Glycyrrhizae control medicinal material solution under absorption (1) item, put respectively on same silica gel g thin-layer plate, with ethyl acetate, alcohol and water (5 ~ 15: 1 ~ 5: 0.2 ~ 2) for developping agent, launch, take out, dry, spray with 40% sulfuric acid solution containing 2% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot development.In test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the spot of aobvious same color.Inspect under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the fluorescence spot of aobvious same color.
(2) get Radix Codonopsis control medicinal material 0.5 ~ 2.0g, add methyl alcohol 30 ~ 100ml, ultrasonic process 15 ~ 60 minutes, let cool, filter, filtrate evaporate to dryness, residue adds water 10 ~ 30ml, heating makes dissolving, extracts 2 times, each 15 ~ 50ml with water saturated normal butyl alcohol jolting, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as Radix Codonopsis control medicinal material solution.Test according to thin-layered chromatography (annex VIB), to draw under (1) item each 2 ~ 10 μ 1 of above-mentioned Radix Codonopsis control medicinal material solution under need testing solution and (2) item, put respectively on same silica gel g thin-layer plate, with normal butyl alcohol-alcohol-water (5 ~ 15: 1 ~ 5: 0.2 ~ 2) for developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear, inspects under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to Radix Codonopsis control medicinal material chromatogram, the spot of aobvious same color.
(3) get Paeoniflorin reference substance, add methyl alcohol and make every 1ml containing 0.2 ~ 1.0mg solution, as Paeoniflorin reference substance solution; Test according to thin-layered chromatography (annex VIB), to draw under (1) item each 3 ~ 10 μ 1 of above-mentioned Paeoniflorin reference substance solution under need testing solution and (3) item, put respectively on same silica gel g thin-layer plate, with ethyl acetate, alcohol and water (5 ~ 15: 1 ~ 5: 0.2 ~ 2) for developping agent, launch, take out, dry, spray is with 5% vanillin-sulfuric acid solution, and it is clear that hot blast blows to spot development; In test sample chromatogram, on the position corresponding to Paeoniflorin reference substance chromatogram, the spot of aobvious same color.
(4) get corydalis tuber control medicinal material 0.2 ~ 1.0g, add methyl alcohol 10 ~ 50ml, ultrasonic process 15 ~ 60 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as corydalis tuber control medicinal material solution.Get tetrahydropalmatine reference substance again, add methyl alcohol and make the solution of every 1ml containing 0.2 ~ 1.0mg, as corydalis tuber reference substance solution.Get indigo naturalis control medicinal material 0.l ~ 1.0g, add methyl alcohol 10 ~ 50ml, ultrasonic process 15 ~ 60 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as indigo naturalis control medicinal material solution.Test according to thin-layered chromatography (annex VIB), each 2 ~ 10 μ 1 of above-mentioned corydalis tuber control medicinal material solution, indigo naturalis control medicinal material solution and corydalis tuber reference substance solution under need testing solution, (4) item under absorption (1) item, put respectively on same silica gel g thin-layer plate, with toluene-acetone (5 ~ 15: 1 ~ 5) for developping agent, launch, take out, dry, in test sample chromatogram, on the position corresponding to indigo naturalis control medicinal material chromatogram, the spot of aobvious same color; Put and take out in iodine cylinder smoked about 1 ~ 5 minute, after waving the iodine that most plate adsorbs, inspect under putting ultraviolet lamp (365nm), in test sample chromatogram, on the position corresponding with tetrahydropalmatine reference substance chromatogram to corydalis tuber control medicinal material, the fluorescence spot of aobvious same color.
The TLC distinguish chromatographic process of Jianwei Yuyang preparation is more preferably:
(1) get this product 1.5g, porphyrize, add methyl alcohol 40ml, ultrasonic process 40 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 20ml, and heating makes dissolving, 2 times are extracted with water saturated normal butyl alcohol jolting, each 30ml, merges normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Separately get radix bupleuri control medicinal material 0.5g, add water 100ml, decocts 1 hour, let cool, filter, filtrate evaporate to dryness, adds methyl alcohol 40ml, ultrasonic process 40 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 20ml, and heating makes dissolving, extract 2 times with water saturated normal butyl alcohol jolting, each 30ml, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as radix bupleuri control medicinal material solution.Extracting Radix Glycyrrhizae control medicinal material 0.2g, adds water-saturated n-butanol 20ml, and jolting 1 hour, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution.Test according to thin-layered chromatography (annex VIB), above-mentioned need testing solution, radix bupleuri control medicinal material solution, each 5 μ 1 of Radix Glycyrrhizae control medicinal material solution under absorption (1) item, put respectively on same silica gel g thin-layer plate, with ethyl acetate, alcohol and water (12: 2: 1) for developping agent, launch, take out, dry, spray with 40% sulfuric acid solution containing 2% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot development.In test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the spot of aobvious same color.Inspect under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the fluorescence spot of aobvious same color.
(2) get Radix Codonopsis control medicinal material lg, add methyl alcohol 40ml, ultrasonic process 40 minutes, let cool, filter, filtrate evaporate to dryness, residue adds water 20ml, heating makes dissolving, extracts 2 times, each 30ml with water saturated normal butyl alcohol jolting, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as Radix Codonopsis control medicinal material solution.Test according to thin-layered chromatography (annex VIB), to draw under (1) item each 2 μ 1 of above-mentioned Radix Codonopsis control medicinal material solution under need testing solution and (2) item, put respectively on same silica gel g thin-layer plate, with normal butyl alcohol-alcohol-water (7: 2: 1) for developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear, inspects under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to Radix Codonopsis control medicinal material chromatogram, the spot of aobvious same color.
(3) get Paeoniflorin reference substance, add methyl alcohol and make every 1ml containing 0.5mg solution, as Paeoniflorin reference substance solution; Test according to thin-layered chromatography (annex VIB), to draw under (1) item each 5 μ 1 of above-mentioned Paeoniflorin reference substance solution under need testing solution and (3) item, put respectively on same silica gel g thin-layer plate, with ethyl acetate, alcohol and water (12: 2: 1) for developping agent, launch, take out, dry, spray is with 5% vanillin-sulfuric acid solution, and it is clear that hot blast blows to spot development; In test sample chromatogram, on the position corresponding to Paeoniflorin reference substance chromatogram, the spot of aobvious same color;
(4) get corydalis tuber control medicinal material 0.2g, add methyl alcohol 30ml, ultrasonic process 15 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as corydalis tuber control medicinal material solution; Get tetrahydropalmatine reference substance again, add methyl alcohol and make the solution of every 1ml containing 0.5mg, as corydalis tuber reference substance solution; Get indigo naturalis control medicinal material 0.lg, add methyl alcohol 20ml, ultrasonic process 40 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as indigo naturalis control medicinal material solution.Test according to thin-layered chromatography (annex VIB), each 5 μ 1 of above-mentioned corydalis tuber control medicinal material solution, indigo naturalis control medicinal material solution and corydalis tuber reference substance solution under need testing solution, (4) item under absorption (1) item, put respectively on same silica gel g thin-layer plate, with toluene-acetone (9: 2) for developping agent, launch, take out, dry, in test sample chromatogram, on the position corresponding to indigo naturalis control medicinal material chromatogram, the spot of aobvious same color; Put and take out in iodine cylinder smoked about 3 minutes, after waving the iodine that most plate adsorbs, inspect under putting ultraviolet lamp (365nm), in test sample chromatogram, on the position corresponding with tetrahydropalmatine reference substance chromatogram to corydalis tuber control medicinal material, the fluorescence spot of aobvious same color.
Jianwei Yuyang preparation formulation of the present invention is any one in capsule, tablet, granule.
Beneficial effect of the present invention: 5 TLC distinguish projects (radix bupleuri, Radix Codonopsis, Chinese herbaceous peony, corydalis tuber, indigo naturalis) of " Chinese Pharmacopoeia " 2010 editions one middle Jianwei Yuyang preparation need process test sample respectively, launch respectively-develop the color-inspect with Mass Control, because each test sample disposal route is different, expansions-colour developing-inspection method difference, complexity and loaded down with trivial details.And the present invention improve after TLC distinguish chromatographic process in 6 TLC distinguish projects (radix bupleuri, Radix Codonopsis, corydalis tuber, indigo naturalis, Radix Glycyrrhizae) shared need testing solution under pharmacopeia [discriminating] (2) item, be divided into four development system-colour developing-review process, and Paeoniflorin wherein development system used is consistent with the development system of radix bupleuri, Radix Glycyrrhizae, thus greatly save human and material resources and time cost, and the present invention also add the TLC distinguish of Radix Glycyrrhizae on former official method.TLC distinguish chromatographic process after the present invention improves, improves the quality control level of medicine, ensure that security and the validity of people's medication.The TLC distinguish chromatographic process of Jianwei Yuyang preparation of the present invention, both may be used for controlling the quality of Jianweiyuyang Tablets, can be used for again controlling other formulations of identical prescription as the quality of the formulation such as capsule, particle.
Accompanying drawing explanation
Fig. 1 is radix bupleuri in Jianwei Yuyang preparation of the present invention, Radix Glycyrrhizae TLC distinguish figure (daylight);
Fig. 2 is radix bupleuri in Jianwei Yuyang preparation of the present invention, Radix Glycyrrhizae TLC distinguish figure (365nm);
Fig. 3 is Radix Codonopsis TLC distinguish figure (daylight) in Jianwei Yuyang preparation of the present invention;
Fig. 4 is Radix Codonopsis TLC distinguish figure (365nm) in Jianwei Yuyang preparation of the present invention;
Fig. 5 is Paeoniflorin TLC distinguish figure (daylight) in Jianwei Yuyang preparation of the present invention;
Fig. 6 is the TLC distinguish figure (365nm) of corydalis tuber in Jianwei Yuyang preparation of the present invention;
Fig. 7 is the TLC distinguish figure (daylight) of indigo naturalis in Jianwei Yuyang preparation of the present invention.
Embodiment
Embodiment 1
(1) get Jianweiyuyang Tablets 1.5g, porphyrize, add methyl alcohol 40ml, ultrasonic process 40 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 20ml, and heating makes dissolving, 2 times are extracted with water saturated normal butyl alcohol jolting, each 30ml, merges normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Separately get radix bupleuri control medicinal material 0.5g, add water 100ml, decocts 1 hour, let cool, filter, filtrate evaporate to dryness, adds methyl alcohol 40ml, ultrasonic process 40 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 20ml, and heating makes dissolving, extract 2 times with water saturated normal butyl alcohol jolting, each 30ml, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as radix bupleuri control medicinal material solution.Extracting Radix Glycyrrhizae control medicinal material 0.5g, adds water-saturated n-butanol 15ml, and jolting 1 hour, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution.Test according to thin-layered chromatography (annex VIB), above-mentioned need testing solution, radix bupleuri control medicinal material solution, each 5 μ 1 of Radix Glycyrrhizae control medicinal material solution under absorption (1) item, put respectively on same silica gel g thin-layer plate, with ethyl acetate, alcohol and water (12: 2: 1) for developping agent, launch, take out, dry, spray with 40% sulfuric acid solution containing 2% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot development.In test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the spot of aobvious same color.Inspect under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the fluorescence spot of aobvious same color.
(2) get Radix Codonopsis control medicinal material 1.5g, add methyl alcohol 40ml, ultrasonic process 40 minutes, let cool, filter, filtrate evaporate to dryness, residue adds water 20ml, heating makes dissolving, extracts 2 times, each 20ml with water saturated normal butyl alcohol jolting, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as Radix Codonopsis control medicinal material solution.Test according to thin-layered chromatography (annex VIB), to draw under (1) item each 5 μ 1 of above-mentioned Radix Codonopsis control medicinal material solution under need testing solution and (2) item, put respectively on same silica gel g thin-layer plate, with normal butyl alcohol-alcohol-water (10: 3: 0.4) for developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear, inspects under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to Radix Codonopsis control medicinal material chromatogram, the spot of aobvious same color.
(3) get Paeoniflorin reference substance, add methyl alcohol and make every 1ml containing 0.5mg solution, as Paeoniflorin reference substance solution.Test according to thin-layered chromatography (annex VIB), to draw under (1) item each 5 μ 1 of above-mentioned Paeoniflorin reference substance solution under need testing solution and (3) item, put respectively on same silica gel g thin-layer plate, with ethyl acetate, alcohol and water (12: 2: 1) for developping agent, launch, take out, dry, spray is with 5% vanillin-sulfuric acid solution, and it is clear that hot blast blows to spot development.In test sample chromatogram, on the position corresponding to Paeoniflorin reference substance chromatogram, the spot of aobvious same color.
(4) get corydalis tuber control medicinal material 0.5g, add methyl alcohol 30ml, ultrasonic process 30 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as corydalis tuber control medicinal material solution.Get tetrahydropalmatine reference substance again, add methyl alcohol and make the solution of every 1ml containing 0.5mg, as corydalis tuber reference substance solution.Get indigo naturalis control medicinal material 0.5g, add methyl alcohol 30ml, ultrasonic process 30 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as indigo naturalis control medicinal material solution.Test according to thin-layered chromatography (annex VIB), each 10 μ 1 of above-mentioned corydalis tuber control medicinal material solution, indigo naturalis control medicinal material solution and corydalis tuber reference substance solution under need testing solution, (4) item under absorption (1) item, put respectively on same silica gel g thin-layer plate, with toluene-acetone (9: 2) for developping agent, launch, take out, dry, in test sample chromatogram, on the position corresponding to indigo naturalis control medicinal material chromatogram, the spot of aobvious same color; Put and take out in iodine cylinder smoked about 1 minute, after waving the iodine that most plate adsorbs, inspect under putting ultraviolet lamp (365nm), in test sample chromatogram, on the position corresponding with tetrahydropalmatine reference substance chromatogram to corydalis tuber control medicinal material, the fluorescence spot of aobvious same color.
Embodiment 2
(1) get Jianwei Yuyang Granule 5g, porphyrize, add methyl alcohol 30ml, ultrasonic process 60 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 10ml, and heating makes dissolving, 2 times are extracted with water saturated normal butyl alcohol jolting, each 15ml, merges normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 0.5ml makes dissolving, as need testing solution.Separately get radix bupleuri control medicinal material 0.2g, add water 50ml, decocts 0.5 hour, let cool, filter, filtrate evaporate to dryness, adds methyl alcohol 30ml, ultrasonic process 60 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 10ml, and heating makes dissolving, extract 2 times with water saturated normal butyl alcohol jolting, each 15ml, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 0.5ml makes dissolving, as radix bupleuri control medicinal material solution.Extracting Radix Glycyrrhizae control medicinal material 0.2g, adds water-saturated n-butanol 10ml, and jolting 1.5 hours, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 0.5ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution.Test according to thin-layered chromatography (annex VIB), above-mentioned need testing solution, radix bupleuri control medicinal material solution, each 3 μ 1 of Radix Glycyrrhizae control medicinal material solution under absorption (1) item, put respectively on same silica gel g thin-layer plate, with ethyl acetate, alcohol and water (5: 5: 0.5) for developping agent, launch, take out, dry, spray with 40% sulfuric acid solution containing 2% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot development.In test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the spot of aobvious same color.Inspect under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the fluorescence spot of aobvious same color.
(2) get Radix Codonopsis control medicinal material 2.0g, add methyl alcohol 100ml, ultrasonic process 15 minutes, let cool, filter, filtrate evaporate to dryness, residue adds water 30ml, heating makes dissolving, extracts 2 times, each 50ml with water saturated normal butyl alcohol jolting, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 5ml makes dissolving, as Radix Codonopsis control medicinal material solution.Test according to thin-layered chromatography (annex VIB), to draw under (1) item each 10 μ 1 of above-mentioned Radix Codonopsis control medicinal material solution under need testing solution and (2) item, put respectively on same silica gel g thin-layer plate, with normal butyl alcohol-alcohol-water (15: 3: 0.8) for developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear, inspects under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to Radix Codonopsis control medicinal material chromatogram, the spot of aobvious same color.
(3) get Paeoniflorin reference substance, add methyl alcohol and make every 1ml containing 1.0mg solution, as Paeoniflorin reference substance solution.Test according to thin-layered chromatography (annex VIB), to draw under (1) item each 10 μ 1 of above-mentioned Paeoniflorin reference substance solution under need testing solution and (3) item, put respectively on same silica gel g thin-layer plate, with ethyl acetate, alcohol and water (5: 5: 0.5) for developping agent, launch, take out, dry, spray is with 5% vanillin-sulfuric acid solution, and it is clear that hot blast blows to spot development.In test sample chromatogram, on the position corresponding to Paeoniflorin reference substance chromatogram, the spot of aobvious same color.
(4) get corydalis tuber control medicinal material 0.2g, add methyl alcohol 10ml, ultrasonic process 15 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 4ml makes dissolving, as corydalis tuber control medicinal material solution.Get tetrahydropalmatine reference substance again, add methyl alcohol and make the solution of every 1ml containing 0.2mg, as corydalis tuber reference substance solution.Get indigo naturalis control medicinal material 0.lg, add methyl alcohol 10ml, ultrasonic process 15 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 0.2ml makes dissolving, as indigo naturalis control medicinal material solution.Test according to thin-layered chromatography (annex VIB), each 2 μ 1 of above-mentioned corydalis tuber control medicinal material solution, indigo naturalis control medicinal material solution and corydalis tuber reference substance solution under need testing solution, (4) item under absorption (1) item, put respectively on same silica gel g thin-layer plate, with toluene-acetone (15: 5) for developping agent, launch, take out, dry, in test sample chromatogram, on the position corresponding to indigo naturalis control medicinal material chromatogram, the spot of aobvious same color; Put and take out in iodine cylinder smoked about 3 minutes, after waving the iodine that most plate adsorbs, inspect under putting ultraviolet lamp (365nm), in test sample chromatogram, on the position corresponding with tetrahydropalmatine reference substance chromatogram to corydalis tuber control medicinal material, the fluorescence spot of aobvious same color.
Embodiment 3
(1) get Jianwei Yuyang capsule 10g, porphyrize, add methyl alcohol 100ml, ultrasonic process 15 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 10ml, and heating makes dissolving, 2 times are extracted with water saturated normal butyl alcohol jolting, each 50ml, merges normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as need testing solution.Separately get radix bupleuri control medicinal material 1.0g, add water 250ml, decocts 2 hours, let cool, filter, filtrate evaporate to dryness, adds methyl alcohol 100ml, ultrasonic process 15 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 10ml, and heating makes dissolving, extract 2 times with water saturated normal butyl alcohol jolting, each 50ml, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as radix bupleuri control medicinal material solution.Extracting Radix Glycyrrhizae control medicinal material 0.2g, adds water-saturated n-butanol 30ml, and jolting 1.5 hours, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 5ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution.Test according to thin-layered chromatography (annex VIB), above-mentioned need testing solution, radix bupleuri control medicinal material solution, each 10 μ 1 of Radix Glycyrrhizae control medicinal material solution under absorption (1) item, put respectively on same silica gel g thin-layer plate, with ethyl acetate, alcohol and water (15: 2: 0.6) for developping agent, launch, take out, dry, spray with 40% sulfuric acid solution containing 2% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot development.In test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the spot of aobvious same color.Inspect under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the fluorescence spot of aobvious same color.
(2) get Radix Codonopsis control medicinal material 0.5g, add methyl alcohol 30ml, ultrasonic process 60 minutes, let cool, filter, filtrate evaporate to dryness, residue adds water 30ml, heating makes dissolving, extracts 2 times, each 50ml with water saturated normal butyl alcohol jolting, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 0.2ml makes dissolving, as Radix Codonopsis control medicinal material solution.Test according to thin-layered chromatography (annex VIB), to draw under (1) item each 2 μ 1 of above-mentioned Radix Codonopsis control medicinal material solution under need testing solution and (2) item, put respectively on same silica gel g thin-layer plate, with normal butyl alcohol-alcohol-water (5: 3: 0.2) for developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear, inspects under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to Radix Codonopsis control medicinal material chromatogram, the spot of aobvious same color.
(3) get Paeoniflorin reference substance, add methyl alcohol and make every 1ml containing 0.2mg solution, as Paeoniflorin reference substance solution.Test according to thin-layered chromatography (annex VIB), to draw under (1) item each 3 μ 1 of above-mentioned Paeoniflorin reference substance solution under need testing solution and (3) item, put respectively on same silica gel g thin-layer plate, with ethyl acetate, alcohol and water (15: 2: 0.6) for developping agent, launch, take out, dry, spray is with 5% vanillin-sulfuric acid solution, and it is clear that hot blast blows to spot development.In test sample chromatogram, on the position corresponding to Paeoniflorin reference substance chromatogram, the spot of aobvious same color.
(4) get corydalis tuber control medicinal material 1.0g, add methyl alcohol 50ml, ultrasonic process 15 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as corydalis tuber control medicinal material solution.Get tetrahydropalmatine reference substance again, add methyl alcohol and make the solution of every 1ml containing 1.0mg, as corydalis tuber reference substance solution.Get indigo naturalis control medicinal material 1.0g, add methyl alcohol 50ml, ultrasonic process 15 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as indigo naturalis control medicinal material solution.Test according to thin-layered chromatography (annex VIB), each 2 μ 1 of above-mentioned corydalis tuber control medicinal material solution, indigo naturalis control medicinal material solution and corydalis tuber reference substance solution under need testing solution, (4) item under absorption (1) item, put respectively on same silica gel g thin-layer plate, with toluene-acetone (5: 3) for developping agent, launch, take out, dry, put and take out in iodine cylinder smoked about 2 minutes, in test sample chromatogram, on the position corresponding to indigo naturalis control medicinal material chromatogram, the spot of aobvious same color; Put and take out in iodine cylinder smoked about 5 minutes, after waving the iodine that most plate adsorbs, inspect under putting ultraviolet lamp (365nm), in test sample chromatogram, on the position corresponding with tetrahydropalmatine reference substance chromatogram to corydalis tuber control medicinal material, the fluorescence spot of aobvious same color.
Claims (3)
1. a TLC distinguish chromatographic process for Jianwei Yuyang preparation, is characterized in that: comprise the following steps:
(1) get this product 0.5 ~ 10g, porphyrize, add methyl alcohol 30 ~ 100ml, ultrasonic process 15 ~ 60 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 10 ~ 30ml, and heating makes dissolving, 2 times are extracted with water saturated normal butyl alcohol jolting, each 15 ~ 50ml, merges normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as need testing solution; Separately get radix bupleuri control medicinal material 0.2 ~ 1.0g, add water 50 ~ 250ml, decocts 0.5 ~ 2 hour, let cool, filter, filtrate evaporate to dryness, adds methyl alcohol 30 ~ 100ml, ultrasonic process 15 ~ 60 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 10 ~ 30ml, and heating makes dissolving, extract 2 times with water saturated normal butyl alcohol jolting, each 15 ~ 50ml, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as radix bupleuri control medicinal material solution; Extracting Radix Glycyrrhizae control medicinal material 0.2 ~ 1.0g, adds water-saturated n-butanol 10 ~ 30ml, and jolting 0.5 ~ 1.5 hour, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution; Test according to thin-layered chromatography, above-mentioned need testing solution, radix bupleuri control medicinal material solution, each 3 ~ 10 μ 1 of Radix Glycyrrhizae control medicinal material solution under absorption (1) item, put respectively on same silica gel g thin-layer plate, be that the ethyl acetate, alcohol and water of 5 ~ 15: 1 ~ 5: 0.2 ~ 2 is for developping agent with volume ratio, launch, take out, dry, spray with 40% sulfuric acid solution containing 2% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot development; In test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the spot of aobvious same color; Inspect under putting 365nm ultraviolet lamp, in test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the fluorescence spot of aobvious same color;
(2) get Radix Codonopsis control medicinal material 0.5 ~ 2.0g, add methyl alcohol 30 ~ 100ml, ultrasonic process 15 ~ 60 minutes, let cool, filter, filtrate evaporate to dryness, residue adds water 10 ~ 30ml, heating makes dissolving, extracts 2 times, each 15 ~ 50ml with water saturated normal butyl alcohol jolting, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as Radix Codonopsis control medicinal material solution; Test according to thin-layered chromatography, to draw under (1) item each 2 ~ 10 μ 1 of above-mentioned Radix Codonopsis control medicinal material solution under need testing solution and (2) item, put respectively on same silica gel g thin-layer plate, with volume ratio be the normal butyl alcohol-alcohol-water of 5 ~ 15: 1 ~ 5: 0.2 ~ 2 for developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear, inspects under putting 365nm ultraviolet lamp; In test sample chromatogram, on the position corresponding to Radix Codonopsis control medicinal material chromatogram, the spot of aobvious same color;
(3) get Paeoniflorin reference substance, add methyl alcohol and make every 1ml containing 0.2 ~ 1.0mg solution, as Paeoniflorin reference substance solution; Test according to thin-layered chromatography, to draw under (1) item each 3 ~ 10 μ 1 of above-mentioned Paeoniflorin reference substance solution under need testing solution and (3) item, put respectively on same silica gel g thin-layer plate, be that the ethyl acetate, alcohol and water of 5 ~ 15: 1 ~ 5: 0.2 ~ 2 is for developping agent with volume ratio, launch, take out, dry, spray is with 5% vanillin-sulfuric acid solution, and it is clear that hot blast blows to spot development; In test sample chromatogram, on the position corresponding to Paeoniflorin reference substance chromatogram, the spot of aobvious same color;
(4) get corydalis tuber control medicinal material 0.2 ~ 1.0g, add methyl alcohol 10 ~ 50ml, ultrasonic process 15 ~ 60 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as corydalis tuber control medicinal material solution; Get tetrahydropalmatine reference substance again, add methyl alcohol and make the solution of every 1ml containing 0.2 ~ 1.0mg, as corydalis tuber reference substance solution; Get indigo naturalis control medicinal material 0.l ~ 1.0g, add methyl alcohol 10 ~ 50ml, ultrasonic process 15 ~ 60 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 0.2 ~ 5ml makes dissolving, as indigo naturalis control medicinal material solution; Test according to thin-layered chromatography, each 2 ~ 10 μ 1 of above-mentioned corydalis tuber control medicinal material solution, indigo naturalis control medicinal material solution and corydalis tuber reference substance solution under need testing solution, (4) item under absorption (1) item, put respectively on same silica gel g thin-layer plate, with volume ratio be the toluene-acetone of 5 ~ 15: 1 ~ 5 for developping agent, launch, take out, dry, in test sample chromatogram, on the position corresponding to indigo naturalis control medicinal material chromatogram, the spot of aobvious same color; Put and take out in iodine cylinder smoked about 1 ~ 5 minute, after waving the iodine that most plate adsorbs, inspect under putting 365nm ultraviolet lamp, in test sample chromatogram, on the position corresponding with tetrahydropalmatine reference substance chromatogram to corydalis tuber control medicinal material, the fluorescence spot of aobvious same color.
2. the TLC distinguish chromatographic process of Jianwei Yuyang preparation according to claim 1, is characterized in that: the TLC distinguish chromatographic process of described Jianwei Yuyang preparation comprises the following steps:
(1) get this product 1.5g, porphyrize, add methyl alcohol 40ml, ultrasonic process 40 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 20ml, and heating makes dissolving, 2 times are extracted with water saturated normal butyl alcohol jolting, each 30ml, merges normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Separately get radix bupleuri control medicinal material 0.5g, add water 100ml, decocts 1 hour, let cool, filter, filtrate evaporate to dryness, adds methyl alcohol 40ml, ultrasonic process 40 minutes, lets cool, and filters, filtrate evaporate to dryness, residue adds water 20ml, and heating makes dissolving, extract 2 times with water saturated normal butyl alcohol jolting, each 30ml, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as radix bupleuri control medicinal material solution; Extracting Radix Glycyrrhizae control medicinal material 0.2g, adds water-saturated n-butanol 20ml, and jolting 1 hour, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution; Test according to thin-layered chromatography, above-mentioned need testing solution, radix bupleuri control medicinal material solution, each 5 μ 1 of Radix Glycyrrhizae control medicinal material solution under absorption (1) item, put respectively on same silica gel g thin-layer plate, be that the ethyl acetate, alcohol and water of 12: 2: 1 is for developping agent with volume ratio, launch, take out, dry, spray with 40% sulfuric acid solution containing 2% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot development, in test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the spot of aobvious same color; Inspect under putting 365nm ultraviolet lamp, in test sample chromatogram, on the position corresponding to radix bupleuri control medicinal material, Radix Glycyrrhizae control medicinal material chromatogram, the fluorescence spot of aobvious same color;
(2) get Radix Codonopsis control medicinal material 1g, add methyl alcohol 40ml, ultrasonic process 40 minutes, let cool, filter, filtrate evaporate to dryness, residue adds water 20ml, heating makes dissolving, extracts 2 times, each 30ml with water saturated normal butyl alcohol jolting, merge normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as Radix Codonopsis control medicinal material solution; According to thin-layered chromatography test, to draw under (1) item each 2 μ 1 of above-mentioned Radix Codonopsis control medicinal material solution under need testing solution and (2) item, put respectively on same silica gel g thin-layer plate, be that the normal butyl alcohol-alcohol-water of 7: 2: 1 is for developping agent with volume ratio, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to spot development at 105 DEG C clear, inspect under putting 365nm ultraviolet lamp, in test sample chromatogram, on the position corresponding to Radix Codonopsis control medicinal material chromatogram, the spot of aobvious same color;
(3) get Paeoniflorin reference substance, add methyl alcohol and make every 1ml containing 0.5mg solution, as Paeoniflorin reference substance solution; Test according to thin-layered chromatography, to draw under (1) item each 5 μ 1 of above-mentioned Paeoniflorin reference substance solution under need testing solution and (3) item, put respectively on same silica gel g thin-layer plate, be that the ethyl acetate, alcohol and water of 12: 2: 1 is for developping agent with volume ratio, launch, take out, dry, spray is with 5% vanillin-sulfuric acid solution, and it is clear that hot blast blows to spot development; In test sample chromatogram, on the position corresponding to Paeoniflorin reference substance chromatogram, the spot of aobvious same color;
(4) get corydalis tuber control medicinal material 0.2g, add methyl alcohol 30ml, ultrasonic process 15 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as corydalis tuber control medicinal material solution; Get tetrahydropalmatine reference substance again, add methyl alcohol and make the solution of every 1ml containing 0.5mg, as corydalis tuber reference substance solution; Get indigo naturalis control medicinal material 0.lg, add methyl alcohol 20ml, ultrasonic process 40 minutes, lets cool, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as indigo naturalis control medicinal material solution; Test according to thin-layered chromatography, each 5 μ 1 of above-mentioned corydalis tuber control medicinal material solution, indigo naturalis control medicinal material solution and corydalis tuber reference substance solution under need testing solution, (4) item under absorption (1) item, put respectively on same silica gel g thin-layer plate, with volume ratio be the toluene-acetone of 9: 2 for developping agent, launch, take out, dry, in test sample chromatogram, on the position corresponding to indigo naturalis control medicinal material chromatogram, the spot of aobvious same color; Put and take out in iodine cylinder smoked about 3 minutes, after waving the iodine that most plate adsorbs, inspect under putting 365nm ultraviolet lamp, in test sample chromatogram, on the position corresponding with tetrahydropalmatine reference substance chromatogram to corydalis tuber control medicinal material, the fluorescence spot of aobvious same color.
3. the TLC distinguish chromatographic process of Jianwei Yuyang preparation as claimed in claim 1 or 2, is characterized in that, described Jianwei Yuyang preparation formulation is any one in capsule, tablet, granule.
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| CN102120021A (en) * | 2011-03-11 | 2011-07-13 | 雷允上药业有限公司 | Detection method of concentrated pills for treating hyperplastic disease of breast |
| CN102233097A (en) * | 2010-05-07 | 2011-11-09 | 郑州福瑞堂制药有限公司 | Quality control method for Zengguang capsules |
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| CN102233097A (en) * | 2010-05-07 | 2011-11-09 | 郑州福瑞堂制药有限公司 | Quality control method for Zengguang capsules |
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