CN103543235A - Method for rapidly identifying uncooked and cooked rhizoma corydalis medicinal slices - Google Patents
Method for rapidly identifying uncooked and cooked rhizoma corydalis medicinal slices Download PDFInfo
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- CN103543235A CN103543235A CN201310550242.3A CN201310550242A CN103543235A CN 103543235 A CN103543235 A CN 103543235A CN 201310550242 A CN201310550242 A CN 201310550242A CN 103543235 A CN103543235 A CN 103543235A
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- 241000218176 Corydalis Species 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims abstract description 42
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 140
- 239000000052 vinegar Substances 0.000 claims abstract description 49
- 235000021419 vinegar Nutrition 0.000 claims abstract description 47
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 30
- AEQDJSLRWYMAQI-UHFFFAOYSA-N Tetrahydropalmatine Natural products C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims abstract description 30
- AEQDJSLRWYMAQI-KRWDZBQOSA-N tetrahydropalmatine Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3C[C@H]2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-KRWDZBQOSA-N 0.000 claims abstract description 29
- 239000003814 drug Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000703 high-speed centrifugation Methods 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims description 62
- 239000013558 reference substance Substances 0.000 claims description 43
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 36
- 238000002360 preparation method Methods 0.000 claims description 36
- 239000003795 chemical substances by application Substances 0.000 claims description 35
- 239000000741 silica gel Substances 0.000 claims description 24
- 229910002027 silica gel Inorganic materials 0.000 claims description 24
- 229920006395 saturated elastomer Polymers 0.000 claims description 22
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 19
- 239000000284 extract Substances 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 14
- 238000002137 ultrasound extraction Methods 0.000 claims description 13
- 239000006228 supernatant Substances 0.000 claims description 12
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 7
- 238000012850 discrimination method Methods 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 abstract description 127
- 238000000605 extraction Methods 0.000 abstract description 10
- 239000000843 powder Substances 0.000 abstract description 6
- 239000012925 reference material Substances 0.000 abstract 3
- 239000012085 test solution Substances 0.000 abstract 2
- 239000012153 distilled water Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 239000000523 sample Substances 0.000 description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 11
- 238000004809 thin layer chromatography Methods 0.000 description 11
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 10
- 239000011630 iodine Substances 0.000 description 10
- 229910052740 iodine Inorganic materials 0.000 description 10
- 238000004587 chromatography analysis Methods 0.000 description 9
- 229930013930 alkaloid Natural products 0.000 description 6
- 229940079593 drug Drugs 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- ONBIUAZBGHXJDM-UHFFFAOYSA-J bismuth;potassium;tetraiodide Chemical compound [K+].[I-].[I-].[I-].[I-].[Bi+3] ONBIUAZBGHXJDM-UHFFFAOYSA-J 0.000 description 5
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 5
- 230000000202 analgesic effect Effects 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 241000620709 Corydalis ambigua Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 150000003797 alkaloid derivatives Chemical class 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
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- 230000035945 sensitivity Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- 206010000087 Abdominal pain upper Diseases 0.000 description 1
- 206010013935 Dysmenorrhoea Diseases 0.000 description 1
- 208000007882 Gastritis Diseases 0.000 description 1
- 206010019133 Hangover Diseases 0.000 description 1
- 244000062241 Kaempferia galanga Species 0.000 description 1
- 235000013421 Kaempferia galanga Nutrition 0.000 description 1
- 240000001659 Oldenlandia diffusa Species 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- WQPDQJCBHQPNCZ-UHFFFAOYSA-N cyclohexa-2,4-dien-1-one Chemical compound O=C1CC=CC=C1 WQPDQJCBHQPNCZ-UHFFFAOYSA-N 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
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- 208000014674 injury Diseases 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
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- 210000004185 liver Anatomy 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 239000013642 negative control Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
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Abstract
The invention discloses a method for rapidly identifying uncooked and cooked rhizoma corydalis medicinal slices. The method comprises the following steps: crushing uncooked rhizoma corydalis medicinal slices and vinegar rhizoma corydalis medicinal slices, sieving through a No.4 sieve, finely weighing 2g of uncooked rhizoma corydalis medicinal powder and 2g of vinegar rhizoma corydalis medicinal powder respectively, adding 25ml of distilled water or methyl alcohol, ultrasonically extracting and treating for 40 minutes, performing high-speed centrifugation on an extraction solution, and taking supernate as a test solution; taking a tetrahydropalmatine standard reference material, and adding the methyl alcohol to prepare a solution each 1ml of which contains 1.2mg of tetrahydropalmatine to be used as a reference material solution; and sucking 35 microliters of prepared rhizoma corydalis test solution and 15 microliters of tetrahydropalmatine standard reference material solution, respectively dropping on a same silica gel G thin layer plate, spreading under an alkaline state, taking out, airing, spraying with a 10 percent sulfuric acid alcohol solution, heating for 10 minutes at a temperature of 105 DEG C, and inspecting under an ultraviolet lamp (365nm). The method is capable of rapidly identifying the difference of contents of tetrahydropalmatine in the uncooked rhizoma corydalis medicinal slices and the vinegar rhizoma corydalis medicinal slices, and provides a basis for identifying and evaluating the quality of the rhizoma corydalis medicinal slices in the traditional Chinese medicine industry.
Description
Technical field
The invention belongs to that the prepared slices of Chinese crude drugs are qualitative, quantitative measurement technical field, more specifically say a kind of method of differentiating fast the raw ripe medicine materical crude slice of traditional Chinese medicine corydalis tuber by qualitative, semi-quantitative analysis.
Background technology
Corydalis tuber is papaveraceae plant corydalis
corydalis yanhusuow.T.Wang. dry tuber.Nature and flavor acrid, bitter, warm, returns liver, the spleen channel.Have invigorate blood circulation, the effect of sharp gas and pain relieving, clinically cure mainly the chest side of body and epigastric pain, through closing dysmenorrhoea, postpartum stasis blocking and treating swelling and pain by traumatic injury.Show after deliberation at present, in corydalis tuber, alkaloid has good analgesic activity, wherein stronger with the analgesic activity of tetrahydropalmatine again, stability is best, but water-soluble poor, corydalis tuber can make its alkaloids composition stripping quantity increase after vinegar system, to strengthen analgesic effect, therefore often select it as index.In 2010 editions Chinese Pharmacopoeias, use thin-layered chromatography, high-efficient liquid phase technique, chemoluminescence method, capillary electrophoresis to differentiate and assay corydalis tuber.And than additive method, thin-layered chromatography has quick, easy feature.At present, existing thin-layer chromatography test method mainly comprises:
1, the method for 2010 editions Chinese Pharmacopoeias:
(1) need testing solution preparation: described in 2010 editions Chinese Pharmacopoeia methods, get Yanhusuo 1g, add methyl alcohol 50ml, ultrasonic processing 30 minutes, filter, filtrate evaporate to dryness, residue adds water 10ml to be made to dissolve, add strong ammonia solution and be adjusted to alkalescence, with ether jolting, extract 3 times, each 10ml merges ether solution, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution.Separately get corydalis tuber control medicinal material 1g, be made in the same way of control medicinal material solution.
(2) reference substance solution preparation: get again tetrahydropalmatine reference substance, add methyl alcohol and make 1ml containing the solution of 0.5mg, in contrast product solution.
(3) chromatographic condition: according to thin-layered chromatography (appendix VI B) test, draw each 2～3 μ l of above-mentioned three kinds of solution, put respectively on the silica gel g thin-layer plate of preparing in same use 1% sodium hydroxide solution, toluene one acetone (9:2) of take is developping agent, launches, and takes out, dry, put in iodine cylinder and take out after approximately 3 minutes, wave after the iodine adsorbing on most thin layer plate, put under ultraviolet lamp (365nm) and inspect.In test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color.
2, Wei Liangbing, the Meng lintel, journey Fan, etc. different vinegar is processed the content of terahydropalmalin in corydalis ambigua cham. Chinese crude drug, 2008,31 (4): 494-495 method:
(1) need testing solution preparation: precision takes test sample 2g, puts in round-bottomed flask, and precision adds the weighed weight of strong ammonia solution one methyl alcohol (1:20) mixed solution 100ml, cold soaking 1h, adds hot reflux 1h, lets cool, weighed weight again, supplies the weight of less loss with strong ammonia solution one methyl alcohol (1:20), shake up, filter, get subsequent filtrate 25ml evaporate to dryness, residue adds methyl alcohol and dissolves, be transferred in 10ml volumetric flask, and be diluted to scale, shake up, filter, get subsequent filtrate, obtain need testing solution.
(2) reference substance solution preparation: precision takes tetrahydropalmatine reference substance, adds methyl alcohol and makes every 1ml containing the solution of 0.10mg, obtains reference substance solution.
(3) chromatographic condition: take silica G plate as adsorbent, toluene one acetone (9:2) is developping agent, saturated 30min, launches, and takes out, and dries, and puts in iodine cylinder and takes out after approximately 3 minutes, waves the iodine adsorbing on most plate.Maximum absorption wavelength is determined in spectral scan: according to thin-layered chromatography (appendix VI B of Chinese Pharmacopoeia version in 2005) test, draw reference substance solution, each 1 μ l point of need testing solution on silica gel g thin-layer plate, launch in accordance with the law; At the wavelength coverage interscan tetrahydropalmatine spot of 200～700nm, selected 280nm is for detecting wavelength, and at 650nm place, all without absorbing, selected 650nm is reference wavelength.
3, Tan Yonghong, Wu Sucheng, Jiang Yunping, etc. gastritis is stopped the thin-layer chromatography of oldenlandia diffusa in capsule, corydalis tuber, galangal and is differentiated [J]. West China pharmaceutical journal, and 1998,13 (4): 265～266 method:
(1) need testing solution preparation: get test sample 5g and add ammoniacal liquor 5ml infiltration, 80ml adds diethyl ether, ultrasonic extraction lh, 10% acetic acid extraction for extract (20ml * 3), combining extraction liquid, adds ammoniacal liquor and adjusts PH10～11, then add chloroform extraction (20ml * 3), combined chloroform extract, water washing is to neutral; Add appropriate anhydrous sodium sulfate dehydration, fling to chloroform, residue adds methyl alcohol lml and dissolves to obtain need testing solution.Separately get the negative control sample 5g that lacks corydalis tuber, be made in the same way of negative sample test liquid.
(2) reference substance solution preparation: get tetrahydropalmatine reference substance and add methyl alcohol and make every milliliter containing the reference substance solution of lmg.
(3) chromatographic condition: draw each 10 μ l of above-mentioned 3 kinds of solution, put respectively on same silica gel g thin-layer plate, take (I) normal hexane one chloroform one methyl alcohol one diethylamine (10:6:1:1 drips) and (II) benzene one acetone one diethylamine (8:2:1 drips) as developping agent expansion, taking-up is dried, spray, with improvement bismuth potassium iodide solution, is inspected under daylight.In test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color, negative sample is without this spot.
4, Zheng Hong, Xu Hongwei. the thin-layer chromatography of the different concocting methods of corydalis tuber is differentiated comparative study [J]. traditional Chinese medical science journal, 2013,28 (5): the method for 695-696:
(1) need testing solution preparation: get corydalis tuber sample and pulverize, get powder 1g, add methyl alcohol 50ml, ultrasonic processing 15 minutes, filter, filtrate evaporate to dryness, residue adds water 10ml to be made to dissolve, add strong ammonia solution and be adjusted to alkalescence, with ether jolting, extract 3 times, each 10ml merges ether solution, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution.
(2) reference substance solution preparation: get tetrahydropalmatine reference substance and add methyl alcohol and make 1ml containing the solution of 1.5mg, in contrast product solution.
(3) chromatographic condition: test sample and reference substance are put on the silica gel g thin-layer plate of preparing in same 1% sodium hydroxide solution, take toluene one acetone (9:2) as developping agent expansion 6～7cm, take out thin layer plate, dry, put in iodine cylinder and take out after approximately 3 minutes, wave the iodine adsorbing on most thin layer plate, put under ultraviolet lamp (365nm) and inspect.In visible test sample chromatogram, with reference substance chromatogram relevant position on, the fluorescence spot of aobvious same color.
5, Liu Xin, woods what, Chen Yun, etc. tetrahydropalmatine thin layer chromatography scanning systematic study in Chinese patent drug. Chinese patent drug, 2006,26(1): the method for 19-23:
(1) need testing solution preparation: get the crude drug powder preparation of corydalis tuber, add appropriate amount of ethanol refluxing extraction 3 times, each 30min, obtains ethanol extract.Decompressing and extracting ethanol, residue dissolves with 0.2mol dilute sulfuric acid or hydrochloric acid gradation, and with appropriate ether washing, obtains acid water extracting liquid.Regulate pH9～10, by appropriate extracted with diethyl ether 4～5 times, obtain after ether extracted liquid, evaporate to dryness ether, by residue gradation dissolving, obtains need testing solution with ethanol.
(2) chromatographic condition: adopted the manual plate of high-efficient silica gel G prefabricated board and silica G and added Diethylamine method alkalescence developping agent system.The selected improvement of Color Appearance System bismuth potassium iodide, iodine smoke 2 kinds of modes and develop the color, and adopt visible ray, ultraviolet light and 3 kinds of modes of fluorescence to detect.Through test findings, show, it is poor that bismuth potassium iodide color stability smokes colour developing compared with iodine, should after colour developing, in 5h, detect.Consider that in Chinese patent drug, THP content is micro-, requiring has good Sensitivity, stability and sweep velocity, with iodine smoke colour developing, the detection of fluorescence list wavelength is comparatively suitable.
In sum, there is following problem in the test method of existing corydalis tuber thin-layer chromatography:
(1) problems such as in the thin-layered chromatography that prior art is used, the extraction of corydalis tuber exists complicated operation, and solvent-oil ratio is large, and extraction ratio is not high;
(2) what in prior art, use is special silica gel g thin-layer plate or high-efficient silica gel G prefabricated board and the manual plate of silica G prepared by 1% sodium hydroxide solution;
(3) the various irritant solvents such as toluene, acetone, chloroform, diethylamine of using of the preparation solvent species of developping agent in prior art, easily damage human body;
(4) multiplex iodine cylinder when the method for prior art develops the color, or use the little improvement bismuth potassium iodide of the colour developing scope of application, and the visible spot that can develop the color in thin-layer chromatography is inspected is few or not obvious.
Summary of the invention
The object of the invention is to overcome the shortcoming and the not enough a kind of device for thin-layer chromatography test method providing after improvement of prior art.The thin layer chromatography of the raw ripe medicine materical crude slice of quick discriminating traditional Chinese medicine corydalis tuber disclosed by the invention, is characterized in that being undertaken by following step:
A method for the raw ripe medicine materical crude slice of quick discriminating corydalis tuber, is characterized in that being undertaken by following step:
(1) preparation of need testing solution: get respectively raw corydalis tuber, each 2g of vinegar corydalis tuber of pulverizing, adding distil water or methyl alcohol 25ml, ultrasonic extraction process 40-60min, to give birth to corydalis tuber, vinegar corydalis tuber extract high speed centrifugation 10-20min, 4000r/s, gets raw corydalis tuber, vinegar corydalis tuber supernatant as need testing solution;
(2) preparation of reference substance solution: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution;
(3) chromatographic condition: get respectively raw corydalis tuber, vinegar corydalis tuber need testing solution 30-35 μ l, reference substance solution 12-15 μ l, put respectively on same silica gel g thin-layer plate, using developping agent ether: cyclohexane: the volume ratio of methyl alcohol is (3 ~ 6): (2 ~ 4): (0.5 ~ 2) is as developping agent, under alkaline state, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, at 105 ℃, heat 10min, under 365nm uviol lamp, detect.Preferred developping agent ether: cyclohexane: the volume ratio of methyl alcohol is 5:3:1, under alkaline state, launch, take out, to dry, spray, with 10% ethanol solution of sulfuric acid, is heated 10min at 105 ℃, under 365nm uviol lamp, detects.
Discrimination method of the present invention, wherein launches to refer to silica gel g thin-layer plate and uses after ammoniacal liquor is saturated under the alkaline state described in step (3).Specifically refer to silica gel g thin-layer plate uses after the saturated 10min of 25% ammoniacal liquor.
Discrimination method of the present invention, wherein launches to refer to silica gel g thin-layer plate and uses after ammoniacal liquor is saturated under the alkaline state described in step (3).Preferably refer to: silica gel g thin-layer plate is used after the saturated 10min of 25% ammoniacal liquor.
Raw corydalis tuber of the present invention refers to corydalis tuber medicinal material and removes impurity, and cleaning, drying, cut sheet.
Vinegar corydalis tuber of the present invention refers to clean corydalis tuber medicine materical crude slice and boils to vinegar exhaustion according to stir-baking with vinegar fried dry or according to vinegar cooking method, cuts sheet.
The invention provides the method for the raw ripe medicine materical crude slice of a kind of quick discriminating traditional Chinese medicine corydalis tuber:
(1) need testing solution preparation: get raw Yanhusuo, vinegar Yanhusuo (No. 4 sieves) 2g, adding distil water 25ml, ultrasonic extraction process 40min, by corydalis tuber extract high speed centrifugation 10min 4000r/s, gets supernatant as need testing solution.
(2) reference substance solution preparation: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution.
(3) chromatographic condition: get above-mentioned need testing solution 35 μ l, reference substance solution 15 μ l, put respectively on same silica gel g thin-layer plate, using developping agent ether-cyclohexane-methyl alcohol (5:3:1) as developping agent, under alkaline state, launch (ammoniacal liquor is saturated), take out, dry, spray is with 10% ethanol solution of sulfuric acid (Chinese Pharmacopoeia appendix), at 105 ℃, heat 10min, under 365nm uviol lamp, inspect as shown in Figure 1.
Another differentiates the method for the raw ripe medicine materical crude slice of traditional Chinese medicine corydalis tuber fast the present invention:
(1) need testing solution preparation: powder (the pulverizing sieve No. 4) 2g that gets raw corydalis tuber, vinegar corydalis tuber medicine materical crude slice, add methyl alcohol 25ml, ultrasonic extraction process 40min, by corydalis tuber extract high speed centrifugation 10min 4000r/s, gets supernatant as need testing solution.
(2) reference substance solution preparation: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution.
(3) chromatographic condition: get above-mentioned need testing solution 30 μ l, reference substance solution 12 μ l, put respectively on same silica gel g thin-layer plate, using developping agent ether-cyclohexane-methyl alcohol (5:3:1) as developping agent, under alkaline state, launch (ammoniacal liquor is saturated), take out, dry, spray is with 10% ethanol solution of sulfuric acid (Chinese Pharmacopoeia appendix), at 105 ℃, heat 10min, under 365nm uviol lamp, inspect as shown in Figure 2.
(4) in the thin-layer chromatography of above two kinds of extracting method is inspected, tetrahydropalmatine spot on raw corydalis tuber and vinegar corydalis tuber correspondence position, vinegar corydalis tuber spot is obviously clear bright than raw corydalis tuber spot colour developing, the stripping quantity that shows can increase after corydalis tuber vinegar system tetrahydropalmatine, has obviously strengthened analgesic effect.
The thin-layered chromatography comparison that thin-layer method after improvement provided by the invention and prior art are used:
(1) in the thin-layered chromatography that prior art is used, the extraction solvent used of corydalis tuber all needs methyl alcohol to be used in conjunction with the reagent such as ether, strong ammonia solution, chloroform mostly, and the present invention only need use a kind of solvent of methyl alcohol.The problems such as the extraction of corydalis tuber exists complicated operation in addition, and solvent-oil ratio is large, and extraction ratio is not high; And the extracting method of corydalis tuber is simple in experimental technique after the present invention improvement, solvent-oil ratio is few and save time;
(2) what in prior art, use is special silica gel g thin-layer plate or high-efficient silica gel G prefabricated board prepared by 1% sodium hydroxide solution; And what in experimental technique of the present invention, adopt is through the water saturated common silica G plate of 25% ammonia, advantage is to save making sheet step, and the thin layer plate after saturated under alkali condition can promote to form drifting alkaloids in conjunction with alkaloids composition, drifting alkaloids polarity is lower than in conjunction with alkaloid, avoided hangover and Rf value too small, therefore can obtain better expansion effect;
(3) in prior art, the preparation solvent species of thin-layer developing agent is various, and solvents excitatory such as toluene, acetone, chloroform, diethylamine easily damages human body; Developping agent of the present invention is ether, cyclohexane, methyl alcohol, conventional and toxicity is less;
(4) multiplex iodine cylinder when the method for prior art develops the color, or use the little improvement bismuth potassium iodide of the colour developing scope of application, and the visible spot that can develop the color in thin-layer chromatography is inspected is few or not obvious; And of the present invention adopted be wide spectrum developer, applied widely, the high and thin-layer chromatography of the Sensitivity visible blurring and clear that can develop the color in inspecting.
In sum, improvement to the thin-layered chromatography of the content difference of terahydropalmalin in corydalis ambigua cham before and after concocting disclosed by the invention reaches simply, the object of quick, successful, and for thin-layered chromatography, checks the tetrahydropalmatine in corydalis tuber favourable reference is provided.
Accompanying drawing explanation:
Fig. 1 is the detection figure of the embodiment of the present invention 1 corydalis tuber concocting method; Wherein 1: raw corydalis tuber medicine materical crude slice, 2: vinegar corydalis tuber medicine materical crude slice, 3: tetrahydropalmatine reference substance;
Fig. 2 is the detection figure of the embodiment of the present invention 2 corydalis tuber concocting methods; Wherein 1 give birth to corydalis tuber medicine materical crude slice, 2 vinegar corydalis tuber medicine materical crude slice, 3 tetrahydropalmatine reference substances.
Fig. 3 is the water extraction liquid water saturated figure of ammonia; Wherein 1-gives birth to corydalis tuber medicine materical crude slice, 2-vinegar corydalis tuber medicine materical crude slice, 3-tetrahydropalmatine reference substance; Be mainly that corydalis tuber water extraction liquid does not adopt the saturated thin layer plate of 25% ammoniacal liquor, with Fig. 1 comparison, vinegar corydalis tuber separating effect is bad, and detecting spot has obvious conditions of streaking.
Fig. 4 is the alcohol extract water saturated figure of ammonia; Wherein 1-gives birth to corydalis tuber medicine materical crude slice, 2-vinegar corydalis tuber medicine materical crude slice, 3-tetrahydropalmatine reference substance; Be mainly that corydalis tuber methyl alcohol extract does not adopt the saturated thin layer plate of 25% ammoniacal liquor, relatively tetrahydropalmatine spot and R f value is less than normal with Fig. 2, and detecting spot also has conditions of streaking.
Embodiment
Below in conjunction with embodiment, the present invention is described, the scheme of embodiment described here, do not limit the present invention, one of skill in the art can make improvements and change according to spirit of the present invention, these described improvement and variation all should be considered as within the scope of the invention, and scope of the present invention and essence are limited by claim.Wherein various raw material used all has commercially available.
Need testing solution preparation: get respectively raw Yanhusuo, each 2g of vinegar Yanhusuo (No. 4 sieves), adding distil water 25ml, ultrasonic extraction process 40min, will give birth to respectively corydalis tuber, vinegar corydalis tuber extract high speed centrifugation 10min, 4000r/s, gets supernatant as need testing solution.
Reference substance solution preparation: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution.
Chromatographic condition: get respectively raw corydalis tuber, vinegar corydalis tuber need testing solution 35 μ l, reference substance solution 15 μ l, point is on same silica gel g thin-layer plate, using developping agent ether-cyclohexane-methyl alcohol (5:3:1) as developping agent, under alkaline state, launch (25% ammoniacal liquor is saturated), take out, dry, spray is with 10% ethanol solution of sulfuric acid (Chinese Pharmacopoeia appendix), at 105 ℃, heat 10min, under 365nm uviol lamp, inspect as shown in Figure 1.
Need testing solution preparation: get respectively raw Yanhusuo, each 2g of vinegar Yanhusuo (No. 4 sieves), add methyl alcohol 25ml, ultrasonic extraction process 40min, will give birth to respectively corydalis tuber, vinegar corydalis tuber extract high speed centrifugation 10min 4000r/s, get supernatant as need testing solution.
Reference substance solution preparation: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution.
Chromatographic condition: get respectively raw corydalis tuber, the molten need testing solution 30 μ l of vinegar corydalis tuber test sample, reference substance solution 12 μ l, put respectively on same silica gel g thin-layer plate, using developping agent ether-cyclohexane-methyl alcohol (5:3:1) as developping agent, under alkaline state, launch (25% ammoniacal liquor is saturated), take out, dry, spray is with 10% ethanol solution of sulfuric acid (Chinese Pharmacopoeia appendix), at 105 ℃, heat 10min, under 365nm uviol lamp, inspect as shown in Figure 2.
(1) preparation of need testing solution: get raw Yanhusuo, vinegar corydalis tuber and cross each 2g of sieve powder No. 4, adding distil water 25ml, ultrasonic extraction process 60min, will give birth to corydalis tuber, vinegar corydalis tuber extract high speed centrifugation 15min, 4000r/s, gets supernatant as need testing solution;
(2) preparation of reference substance solution: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution;
(3) chromatographic condition: get above-mentioned need testing solution 35 μ l, reference substance solution 13.5 μ l, put respectively on same silica gel g thin-layer plate, using developping agent ether: cyclohexane: the volume ratio of methyl alcohol is as 5:3:1 is as developping agent, under alkaline state, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, at 105 ℃, heat 10min, under 365nm uviol lamp, detect.
Embodiment 4
(1) preparation of need testing solution: got and sieve raw Yanhusuo for No. 4, cross each 2g of sieve vinegar Yanhusuo No. 4, add methyl alcohol 25ml, ultrasonic extraction process 40min, will give birth to corydalis tuber, vinegar corydalis tuber extract high speed centrifugation 10min 4000r/s, get supernatant as need testing solution;
(2) preparation of reference substance solution: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution;
(3) chromatographic condition: get above-mentioned need testing solution 30 μ l, reference substance solution 15 μ l, put respectively on same silica gel g thin-layer plate, using developping agent ether: cyclohexane: the volume ratio of methyl alcohol is as 5:3:1 is as developping agent, under alkaline state, launch (25% ammoniacal liquor is saturated), take out, dry, spray is with 10% ethanol solution of sulfuric acid, at 105 ℃, heat 10min, under 365nm uviol lamp, detect.
Embodiment 5
(1) need testing solution preparation: get respectively raw Yanhusuo, each 2g of vinegar Yanhusuo (No. 4 sieves), add water 25ml, ultrasonic extraction process 40min, will give birth to respectively corydalis tuber, vinegar corydalis tuber extract high speed centrifugation 10min 4000r/s, get supernatant as need testing solution.
(2) reference substance solution preparation: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution.
(3) chromatographic condition: get respectively raw corydalis tuber, the molten need testing solution 30 μ l of vinegar corydalis tuber test sample, reference substance solution 12 μ l, put respectively on same silica gel g thin-layer plate, using developping agent ether-cyclohexane-methyl alcohol (5:4:1) as developping agent, under alkaline state, launch (25% ammoniacal liquor is saturated), take out, dry, spray is with 10% ethanol solution of sulfuric acid (Chinese Pharmacopoeia appendix), at 105 ℃, heat 10min, under 365nm uviol lamp, inspect.
Embodiment 6
(1) need testing solution preparation: get respectively raw Yanhusuo, each 2g of vinegar Yanhusuo (No. 4 sieves), add methyl alcohol 25ml, ultrasonic extraction process 40min, will give birth to respectively corydalis tuber, vinegar corydalis tuber extract high speed centrifugation 10min 4000r/s, get supernatant as need testing solution.
(2) reference substance solution preparation: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution.
(3) chromatographic condition: get respectively raw corydalis tuber, the molten need testing solution 30 μ l of vinegar corydalis tuber test sample, reference substance solution 12 μ l, put respectively on same silica gel g thin-layer plate, using developping agent ether-cyclohexane-methyl alcohol (3:2:0.5) as developping agent, under alkaline state, launch (25% ammoniacal liquor is saturated), take out, dry, spray is with 10% ethanol solution of sulfuric acid (Chinese Pharmacopoeia appendix), at 105 ℃, heat 10min, under 365nm uviol lamp, inspect.
Embodiment 7
(1) need testing solution preparation: get respectively raw Yanhusuo, each 2g of vinegar Yanhusuo (No. 4 sieves), add water 25ml, ultrasonic extraction process 40min, will give birth to respectively corydalis tuber, vinegar corydalis tuber extract high speed centrifugation 10min 4000r/s, get supernatant as need testing solution.
(2) reference substance solution preparation: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution.
(3) chromatographic condition: get respectively raw corydalis tuber, the molten need testing solution 30 μ l of vinegar corydalis tuber test sample, reference substance solution 12 μ l, put respectively on same silica gel g thin-layer plate, using developping agent ether-cyclohexane-methyl alcohol (4:2:1) as developping agent, under alkaline state, launch (25% ammoniacal liquor is saturated), take out, dry, spray is with 10% ethanol solution of sulfuric acid (Chinese Pharmacopoeia appendix), at 105 ℃, heat 10min, under 365nm uviol lamp, inspect.
Embodiment 8
(1) need testing solution preparation: get respectively raw Yanhusuo, each 2g of vinegar Yanhusuo (No. 4 sieves), add methyl alcohol 25ml, ultrasonic extraction process 40min, will give birth to respectively corydalis tuber, vinegar corydalis tuber extract high speed centrifugation 10min 4000r/s, get supernatant as need testing solution.
(2) reference substance solution preparation: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution.
(3) chromatographic condition: get respectively raw corydalis tuber, the molten need testing solution 30 μ l of vinegar corydalis tuber test sample, reference substance solution 12 μ l, put respectively on same silica gel g thin-layer plate, using developping agent ether-cyclohexane-methyl alcohol (4.5:2.5:1.5) as developping agent, under alkaline state, launch (25% ammoniacal liquor is saturated), take out, dry, spray is with 10% ethanol solution of sulfuric acid (Chinese Pharmacopoeia appendix), at 105 ℃, heat 10min, under 365nm uviol lamp, inspect.
Claims (4)
1. differentiate fast a method for the raw ripe medicine materical crude slice of corydalis tuber, it is characterized in that being undertaken by following step:
(1) preparation of need testing solution: get respectively raw corydalis tuber, each 2g of vinegar corydalis tuber of pulverizing, adding distil water or methyl alcohol 25ml, ultrasonic extraction process 40-60min, to give birth to corydalis tuber, vinegar corydalis tuber extract high speed centrifugation 10-20min, 4000r/s, gets raw corydalis tuber, vinegar corydalis tuber supernatant as need testing solution;
(2) preparation of reference substance solution: get again tetrahydropalmatine standard items, add methyl alcohol and make every 1ml containing the solution of 1.2mg, in contrast product solution;
(3) chromatographic condition: get respectively raw corydalis tuber, vinegar corydalis tuber need testing solution 30-35 μ l, reference substance solution 12-15 μ l, put respectively on same silica gel g thin-layer plate, using developping agent ether: cyclohexane: the volume ratio of methyl alcohol as 3 ~ 6:2 ~ 4:0.5 ~ 2 as developping agent, under alkaline state, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, at 105 ℃, heat 10min, under 365nm uviol lamp, detect.
2. discrimination method claimed in claim 1, wherein launches to refer to silica gel g thin-layer plate and uses after ammoniacal liquor is saturated under the alkaline state described in step (3).
3. discrimination method claimed in claim 1, wherein launches to refer to silica gel g thin-layer plate and uses after the saturated 10min of 25% ammoniacal liquor under the alkaline state described in step (3).
4. content assaying method claimed in claim 1, wherein the described developping agent of step (3) refers to ether: cyclohexane: methyl alcohol volume ratio is that 5:3:1 is as developping agent.
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