CN103487546B - Identification method of flower of sunset abelmoschus - Google Patents
Identification method of flower of sunset abelmoschus Download PDFInfo
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- CN103487546B CN103487546B CN201310394319.2A CN201310394319A CN103487546B CN 103487546 B CN103487546 B CN 103487546B CN 201310394319 A CN201310394319 A CN 201310394319A CN 103487546 B CN103487546 B CN 103487546B
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- sunset abelmoschus
- rutin
- hyperoside
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- 241001075517 Abelmoschus Species 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 69
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 claims abstract description 52
- FVQOMEDMFUMIMO-UHFFFAOYSA-N Hyperosid Natural products OC1C(O)C(O)C(CO)OC1OC1C(=O)C2=C(O)C=C(O)C=C2OC1C1=CC=C(O)C(O)=C1 FVQOMEDMFUMIMO-UHFFFAOYSA-N 0.000 claims abstract description 42
- OVSQVDMCBVZWGM-SJWGPRHPSA-N Hyperin Natural products O[C@H]1[C@H](O)[C@@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-SJWGPRHPSA-N 0.000 claims abstract description 40
- OVSQVDMCBVZWGM-DTGCRPNFSA-N quercetin 3-O-beta-D-galactopyranoside Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-DTGCRPNFSA-N 0.000 claims abstract description 40
- BBFYUPYFXSSMNV-UHFFFAOYSA-N quercetin-7-o-galactoside Natural products OC1C(O)C(O)C(CO)OC1OC1=CC(O)=C2C(=O)C(O)=C(C=3C=C(O)C(O)=CC=3)OC2=C1 BBFYUPYFXSSMNV-UHFFFAOYSA-N 0.000 claims abstract description 40
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 claims abstract description 39
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 claims abstract description 39
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 claims abstract description 39
- 235000005493 rutin Nutrition 0.000 claims abstract description 39
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 claims abstract description 39
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 claims abstract description 39
- 229960004555 rutoside Drugs 0.000 claims abstract description 39
- 238000012360 testing method Methods 0.000 claims abstract description 29
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 claims abstract description 26
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 claims abstract description 26
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 claims abstract description 26
- 235000005875 quercetin Nutrition 0.000 claims abstract description 26
- 229960001285 quercetin Drugs 0.000 claims abstract description 26
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 229960000583 acetic acid Drugs 0.000 claims abstract description 12
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 12
- 239000012085 test solution Substances 0.000 claims abstract description 10
- 239000004952 Polyamide Substances 0.000 claims abstract description 9
- 229920002647 polyamide Polymers 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 46
- 239000013558 reference substance Substances 0.000 claims description 43
- NQYPTLKGQJDGTI-FCVRJVSHSA-N hyperoside Natural products OC[C@H]1O[C@@H](OC2=C(Oc3cc(O)cc(O)c3[C@H]2O)c4ccc(O)c(O)c4)[C@H](O)[C@@H](O)[C@H]1O NQYPTLKGQJDGTI-FCVRJVSHSA-N 0.000 claims description 38
- 238000012850 discrimination method Methods 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 12
- 239000004411 aluminium Substances 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
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- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 239000000523 sample Substances 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
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- 235000014290 Artemisia anomala Nutrition 0.000 description 2
- 241000123844 Artemisia anomala Species 0.000 description 2
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- 235000003392 Curcuma domestica Nutrition 0.000 description 2
- OVSQVDMCBVZWGM-IDRAQACASA-N Hirsutrin Natural products O([C@H]1[C@H](O)[C@H](O)[C@H](O)[C@@H](CO)O1)C1=C(c2cc(O)c(O)cc2)Oc2c(c(O)cc(O)c2)C1=O OVSQVDMCBVZWGM-IDRAQACASA-N 0.000 description 2
- 240000001341 Reynoutria japonica Species 0.000 description 2
- 235000018167 Reynoutria japonica Nutrition 0.000 description 2
- 244000153955 Reynoutria sachalinensis Species 0.000 description 2
- 235000003202 Reynoutria sachalinensis Nutrition 0.000 description 2
- 240000008488 Thlaspi arvense Species 0.000 description 2
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- 238000002474 experimental method Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 229930182486 flavonoid glycoside Natural products 0.000 description 2
- 150000007955 flavonoid glycosides Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- GXMWXESSGGEWEM-UHFFFAOYSA-N isoquercitrin Natural products OCC(O)C1OC(OC2C(Oc3cc(O)cc(O)c3C2=O)c4ccc(O)c(O)c4)C(O)C1O GXMWXESSGGEWEM-UHFFFAOYSA-N 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000013642 negative control Substances 0.000 description 2
- OVSQVDMCBVZWGM-QSOFNFLRSA-N quercetin 3-O-beta-D-glucopyranoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-QSOFNFLRSA-N 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 235000013976 turmeric Nutrition 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 201000006474 Brain Ischemia Diseases 0.000 description 1
- 206010007191 Capillary fragility Diseases 0.000 description 1
- 206010008120 Cerebral ischaemia Diseases 0.000 description 1
- 241001573881 Corolla Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 241000522190 Desmodium Species 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 240000005717 Dioscorea alata Species 0.000 description 1
- 244000192024 Euphorbia helioscopia Species 0.000 description 1
- 235000012043 Euphorbia helioscopia Nutrition 0.000 description 1
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- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- 241000801118 Lepidium Species 0.000 description 1
- 241000219071 Malvaceae Species 0.000 description 1
- IKMDFBPHZNJCSN-UHFFFAOYSA-N Myricetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC(O)=C(O)C(O)=C1 IKMDFBPHZNJCSN-UHFFFAOYSA-N 0.000 description 1
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- 244000228293 Persicaria perfoliata Species 0.000 description 1
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- 241000304432 Sedum sarmentosum Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- FOGVNFMUZXDMTR-UHFFFAOYSA-N [Mg].Cl Chemical compound [Mg].Cl FOGVNFMUZXDMTR-UHFFFAOYSA-N 0.000 description 1
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- PCOBUQBNVYZTBU-UHFFFAOYSA-N myricetin Natural products OC1=C(O)C(O)=CC(C=2OC3=CC(O)=C(O)C(O)=C3C(=O)C=2)=C1 PCOBUQBNVYZTBU-UHFFFAOYSA-N 0.000 description 1
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- Saccharide Compounds (AREA)
- Cosmetics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to an identification method of flower of sunset abelmoschus, which comprises the following steps of: by taking rutin, hyperin and quercetin as contrast substances or taking rutin and hyperin as contrast substances, spotting test product solution and contrast drug solution on the same polyamide film, by taking 60-75% glacial acetic acid as the developing agent, developing through aluminium trichloride test solution, viewing under an ultraviolet lamp (365 nm), and developing fluorescent spots of the same colour at the position corresponding to a contrast substance chromatograph in a test product chromatograph. The identification method of flower of sunset abelmoschus provided by the invention has the advantages of being strong in specificity, few in use amounts of drugs and chemical reagents, simple and convenient for operation and good in reproducibility and is applied to identifying all flowers of sunset abelmoschus and identifying whether finished products containing flower of sunset abelmoschus contain flower of sunset abelmoschus.
Description
Technical field
The present invention relates to qualitative, the discrimination method of medicinal material, particularly relate to the discrimination method of sunset abelmoschus flower medicinal material.
Background technology
Sunset abelmoschus flower is the dry corolla of Malvaceae plant Sunset Abelmoschus Root, has long medicinal history in China, and " Jiayou Bencao ", Compendium of Material Medica all have medicinal record.Property sweet, cold, return kidney, urinary bladder channel, hold back for damp and hot heap soil or fertilizer over and around the roots, stranguria with turbid discharge oedema; Control swollen ulcer drug outward, scald.
The principal ingredient of sunset abelmoschus flower comprises Hyperoside, isoquercitrin, Quercetin, myricetin, rutin etc.Wherein Determination of Hyperoside is the highest, has significant topical pain relief effect, shields, shield, and have spasmolysis and analgesia and the effect such as reducing blood lipid, enhancing immunologic function to liver gastric mucosa cardiac muscle, cerebral ischemia.Quercetin can be used as medicine, have eliminate the phlegm preferably, cough-relieving and antiasthmatic effect, reduce blood pressure in addition in addition, strengthen capillary resistance, reduce the effect such as capillary fragility, reducing blood lipid.Rutin has anti-inflammatory, antiviral and maintain VAR, reduce its permeability, reduce the effect such as fragility of blood vessels.
Shandong Province's Chinese crude drug standard (version in 2002) has recorded sunset abelmoschus flower medicinal material, it differentiates that item selects hydrochloric acid magnesium powder to react, differentiate flavonoid glycoside wherein, there is redness to aubergine reaction for index, operate relatively simple, but specificity is poor, as long as the different medicinal materials containing flavonoid glycoside composition all can present positive reaction.
Newly record sunset abelmoschus flower in Pharmacopoeia of People's Republic of China (version in 2010), improve the discrimination method of sunset abelmoschus flower medicinal material.Its operating process is: " get this product powder 1g, add 0.18% ethanol solution hydrochloride 20ml, put in water-bath and add hot reflux 1 hour, filter while hot, filtrate is concentrated into 5ml, as need testing solution.Separately get Quercetin reference substance, add ethanol and make the solution of every 1ml containing 0.5mg, product solution in contrast.Draw each 1 μ l of above-mentioned two kinds of solution, put on the silica gel g thin-layer plate prepared in same use 0.5% sodium hydroxide solution respectively, with toluene-ethyl acetate-formic acid 5:4:1 for developping agent, launch, take out, dry, spray is with aluminium choride test solution, inspect under putting ultraviolet lamp 365nm, on the position corresponding to reference substance chromatogram, the fluorescence spot in same color ".The method is reacted by hydrochloric acid hydrolysis, effective constituent Hyperoside, Q3Glc, isoquercitrin etc. in sunset abelmoschus flower removed substituting group and is converted to Quercetin, then using Quercetin reference substance as reference, differentiates the medicinal material true and false.Its method specificity is relatively strong, but there is the deficiencies such as operating process is cumbersome, use chemical reagent kind is many, the discriminating time is long, is not suitable for the requirement of quick test in production run.
In addition, adulterated, shoddy phenomenon of Market of Chinese Materia Medica adulterating is innumerable.Chinese medicine, for curing the disease, if treatment uses counterfeit drug material or medicinal material inferior, not only can not play result for the treatment of, possibility delay treatment, even life threatening on the contrary, therefore reinforcement Chinese crude drug and Quality of Chinese Traditional Proprietary Medicine management become more and more important work.The discriminating of Chinese crude drug is always difficult point, and method specificity directly determines the value of discrimination method.Although adopt single reference substance to carry out differentiating to have certain specificity, due to Chinese crude drug complicated component, a lot of Chinese crude drug all contains same effective constituent, therefore usually there will be misjudgment phenomenon.Such as, the Chinese crude drug containing Quercetin of including in pharmacopeia just has Orostachys fimbriatus, wolf's milk, stringy stonecrop, polygonum perfoliatum, desmodium, cacumen biotae, ginkgo leaf, lepidium seed, sunset abelmoschus flower etc., when using the discrimination method of sunset abelmoschus flower medicinal material to differentiate these medicinal materials, all there will be Quercetin unique point, cause false positive results.
Summary of the invention
The object of this invention is to provide a kind of discrimination method of sunset abelmoschus flower medicinal material, method provided by the invention is easy and simple to handle, specificity is stronger, favorable reproducibility, can differentiate sunset abelmoschus flower medicinal material rapidly and accurately.
The discrimination method of sunset abelmoschus flower medicinal material provided by the invention is with rutin, Hyperoside and Quercetin for reference substance, and adopt thin-layered chromatography to differentiate, concrete grammar comprises:
1), need testing solution preparation
Get sunset abelmoschus flower medicinal powder 0.1 ~ 0.5g, add C
1 ~ 4monohydroxy alcohol 10ml, after fully dissolving, filters, gets filtrate as need testing solution;
2), reference substance solution preparation
Get rutin, Hyperoside, Quercetin reference substance respectively, with C
1 ~ 4monohydroxy alcohol makes the solution of every 1ml containing rutin 0.05 ~ 0.1mg, Hyperoside 0.1 ~ 0.3mg, Quercetin 0.05 ~ 0.1mg, as control substance of Rutin solution, Hyperoside reference substance solution and Quercetin reference substance solution;
Or,
Rutin, Hyperoside and Quercetin reference substance are dissolved in C simultaneously
1 ~ 4in monohydroxy alcohol, make the solution of every 1ml containing rutin 0.05 ~ 0.1mg, Hyperoside 0.1 ~ 0.3mg, Quercetin 0.05 ~ 0.1mg, product solution in contrast;
3), thin-layered chromatography is differentiated
Draw above-mentioned need testing solution and each 2 ~ 10 μ L of reference substance solution respectively, put on same polyamide film, with 60 ~ 75% glacial acetic acid for developping agent, exhibition, apart from 6cm, is taken out, is dried, spray with aluminium choride test solution, hot blast drying, inspect under putting 365nm ultraviolet lamp; In test sample chromatogram, on the position corresponding to each reference substance chromatogram, the fluorescence spot of aobvious same color.
The discrimination method of sunset abelmoschus flower medicinal material provided by the invention can also be that adopt thin-layered chromatography to differentiate, concrete grammar comprises with rutin and Hyperoside for reference substance:
1), need testing solution preparation
Get sunset abelmoschus flower medicinal powder 0.1 ~ 0.5g, or be equivalent to 0.1 ~ 0.5g sunset abelmoschus flower medicinal material containing sunset abelmoschus flower medicinal material manufactured goods powder, add C
1 ~ 4monohydroxy alcohol 10ml, after fully dissolving, filters, gets filtrate as need testing solution;
2), reference substance solution preparation
Get rutin, Hyperoside reference substance respectively, with C
1 ~ 4monohydroxy alcohol makes the solution of every 1ml containing rutin 0.05 ~ 0.1mg, Hyperoside 0.1 ~ 0.3mg, as control substance of Rutin solution, Hyperoside reference substance solution;
Or,
Rutin, Hyperoside reference substance are dissolved in C simultaneously
1 ~ 4in monohydroxy alcohol, make the solution of every 1ml containing rutin 0.05 ~ 0.1mg, Hyperoside 0.1 ~ 0.3mg, product solution in contrast;
3), thin-layered chromatography is differentiated
Draw above-mentioned need testing solution and each 2 ~ 10 μ L of reference substance solution respectively, put on same polyamide film, with 60 ~ 75% glacial acetic acid for developping agent, exhibition, apart from 6cm, is taken out, is dried, spray with aluminium choride test solution, hot blast drying, inspect under putting 365nm ultraviolet lamp; In test sample chromatogram, on the position corresponding to each reference substance chromatogram, the fluorescence spot of aobvious same color.
In said method of the present invention, step 1) described in abundant dissolving be the dissolving means taking various routine, as stirring, vibration, heating etc., use C
1 ~ 4effective constituent in sunset abelmoschus flower medicinal material is dissolved out by monohydroxy alcohol as much as possible.Wherein the most simple and effective dissolving method solution is placed in ultrasound wave process 20min.
The discrimination method of above-mentioned sunset abelmoschus flower medicinal material provided by the invention is a typical method for qualitative analysis.Under different experimental situations and test condition, the experimental result obtained may have difference slightly.In practical operation, allow to carry out suitable adjustment to the experiment condition in above-mentioned discrimination method, obtain best test findings, to facilitate discriminating with it.
Usually, preferably with 70% glacial acetic acid for developping agent.According to actual conditions, the concentration of developping agent suitably can be adjusted.
If because above-mentioned experiment condition changes, or be subject to the impact of experimental situation, sample point developed the color bad, suitably can also heat thin layer plate, be beneficial to colour developing.
Percentage concentration of the present invention is concentration expressed in percentage by volume.
Sunset abelmoschus flower discrimination method of the present invention is not only applicable to all sources, single (comprising dry product, fresh goods, Different sources) sunset abelmoschus flower medicinal material, to be equally applicable in the various manufactured goods (comprising folk prescription, compound manufactured goods) such as human drugs, food, health products, cosmetics, veterinary drug prepared with all sources sunset abelmoschus flower medicinal material the discriminating whether containing sunset abelmoschus flower medicinal material yet.
Rutin used in the present invention, Hyperoside, Quercetin standard items are prepared by Nat'l Pharmaceutical & Biological Products Control Institute.Differentiate that sunset abelmoschus flower carries out according to the respective specified of Pharmacopoeia of People's Republic of China (version in 2010) with thin-layered chromatography.
Discrimination method of the present invention is ripe, differentiates and the sunset abelmoschus flower medicinal material of many batches of Different sources, separate sources is carried out to discriminatings contrast, all accurately can differentiate medicinal material through different experimental conditions, specificity by force, favorable reproducibility.And then the manufactured goods be applied to by discrimination method of the present invention containing sunset abelmoschus flower are as the discriminating of sunset abelmoschus flower in compound ambrette particle, negative noiseless, specificity is good, has good identification result equally.
Compare with the discrimination method of sunset abelmoschus flower medicinal material in existing pharmacopeia, discrimination method of the present invention has the following advantages.
1. specificity is stronger.The inventive method adopts rutin, Hyperoside two kinds of reference substances or rutin, Hyperoside, Quercetin three kinds of reference substances as reference material simultaneously, differentiate sunset abelmoschus flower medicinal material and contain sunset abelmoschus flower medicinal material manufactured goods, quality of medicinal material information can be reflected more all sidedly, more effectively avoid false positive results, improve discriminating specificity.Can check in process of production more comprehensively, rapidly and judge product quality, control the clinical safety of sunset abelmoschus flower medicinal material and preparation thereof better, ensure stable and reliable product quality.
2. need testing solution preparation method is easy.Directly add C
1 ~ 4the one of monohydroxy alcohol, adopting the methods such as ultrasonic or backflow to extract can obtain, and needs to prepare ethanol solution hydrochloride, add hot reflux to have made hydrolysis reaction completely easy much with ethanol solution hydrochloride relative to official method.
3. differentiate time shorten.Whole operating process can complete in 1 hour, and official method then at least needs more than 2 hours.
4. medicinal material, using amount of reagent are few.Discrimination method of the present invention only needs medicinal material 0.1 ~ 0.5g, and whole detection only needs C
1 ~ 4a few reagent of monohydroxy alcohol, glacial acetic acid, aluminium choride can complete, official method then needs at least 1g medicinal material, whole detection relates to hydrochloric acid, ethanol, toluene, ethyl acetate, formic acid, aluminium choride plurality of reagents, and using amount of reagent is large, and organic solvent toxicity is large.
5. method is highly sensitive.Only need minute quantity reference substance namely can develop the color obviously, highly sensitive.
Accompanying drawing explanation
Fig. 1 is the Development of Thin-Layer Chromatography design sketch of embodiment 1.
Fig. 2 is the Development of Thin-Layer Chromatography design sketch of embodiment 2.
Fig. 3 is the Development of Thin-Layer Chromatography design sketch of embodiment 3.
Fig. 4 is the Development of Thin-Layer Chromatography design sketch of embodiment 4.
Embodiment
Embodiment 1
The present embodiment sunset abelmoschus flower crude drug source is in Hui nationality.
Get sunset abelmoschus flower medicinal powder 0.1g, add methyl alcohol 10ml, put in ultrasound wave and process 20min and fully dissolve, filter, get filtrate as need testing solution; Get rutin, Hyperoside, Quercetin reference substance respectively, add methyl alcohol and make the solution of every 1ml containing rutin 0.05mg, Hyperoside 0.1mg, Quercetin 0.05mg respectively, product solution in contrast.
Draw each 10 μ L of above-mentioned four kinds of solution, put respectively on same polyamide film, with 60% glacial acetic acid for developping agent, exhibition, apart from 6cm, is taken out, is dried, spray with aluminium choride test solution, hot blast drying, inspect under putting 365nm ultraviolet lamp.Chromatogram is as Fig. 1, and in test sample chromatogram, on the position corresponding to reference substance chromatogram, the fluorescence spot of aobvious same color, can judge that differentiated medicinal material is as sunset abelmoschus flower thus.
Embodiment 2
The present embodiment sunset abelmoschus flower crude drug source is in Xinghua, Jiangsu.
Get sunset abelmoschus flower medicinal powder 0.5g, add ethanol 10ml, put in ultrasound wave and process 20min and fully dissolve, filter, get filtrate as need testing solution; Get rutin, Hyperoside and Quercetin reference substance to add in ethanol simultaneously, make the solution of every 1ml containing rutin 0.05mg, Hyperoside 0.1mg, Quercetin 0.05mg, product solution in contrast; The sunset abelmoschus flower medicinal material that another Example 1 derives from Hui nationality is made in the same way of control medicinal material solution.
Draw each 5 μ L of above-mentioned three kinds of solution, put respectively on same polyamide film, with 75% glacial acetic acid for developping agent, exhibition, apart from 6cm, is taken out, is dried, spray with aluminium choride test solution, hot blast drying, inspect under putting ultraviolet lamp (365nm).Chromatogram, as Fig. 2, in test sample chromatogram, on the position corresponding to reference substance chromatogram, shows the fluorescence spot of same color, and with control medicinal material chromatogram without obvious difference, can judge that differentiated medicinal material is as sunset abelmoschus flower thus.
Embodiment 3
The present embodiment sunset abelmoschus flower crude drug source is in Hebei punishment platform.
Get sunset abelmoschus flower medicinal powder 0.5g, add normal butyl alcohol 10ml, put in ultrasound wave and process 20min and fully dissolve, filter, get filtrate as need testing solution; Get rutin, Hyperoside reference substance respectively, add normal butyl alcohol respectively and make the solution of every 1ml containing rutin 0.1mg, Hyperoside 0.3mg, product solution in contrast.
Draw each 2 μ L of above-mentioned three kinds of solution, put respectively on same polyamide film, with 75% glacial acetic acid for developping agent, exhibition, apart from 6cm, is taken out, is dried, spray with aluminium choride test solution, hot blast drying, inspect under putting ultraviolet lamp (365nm).Chromatogram is as Fig. 3, and in test sample chromatogram, on the position corresponding to reference substance chromatogram, the fluorescence spot of aobvious same color, can judge that differentiated medicinal material is as sunset abelmoschus flower thus.
Embodiment 4
The present embodiment is differentiated the sunset abelmoschus flower medicinal material in compound ambrette particle, and sunset abelmoschus flower crude drug source used is in Xinghua, Jiangsu.
Prescription: sunset abelmoschus flower 1000g, field pennycress 500g, Fen Bi Hu 240g, giant knotweed 400g, Artemisia anomala 350g, turmeric 250g, radix bupleuri 250g, prepared RADIX ET RHIZOMA RHEI with wine 250g, bighead atractylodes rhizome 250g, prepared fleece flower root 200g.
Method for making: sunset abelmoschus flower, turmeric, alcohol heating reflux extracts 1 hour, and filter, filtrate recycling ethanol, is condensed into thick paste; Field pennycress, hypoglaucous collett yam rhizome, giant knotweed, Artemisia anomala, radix bupleuri, prepared RADIX ET RHIZOMA RHEI with wine, the bighead atractylodes rhizome, prepared fleece flower root eight taste, boiling secondary, each 1 hour, collecting decoction, added ethanol cold heavy 24 hours, filters, filtrate recycling ethanol, concentrated; Merge above-mentioned two kinds of medicinal extract, add lactose 100g, DEXTRIN 0g, mixing, dry, make 1000g, to obtain final product.
Get compound ambrette particle 5g, add methyl alcohol 10ml, put in ultrasound wave and process 20min and fully dissolve, filter, get filtrate as need testing solution; Get rutin, Hyperoside reference substance adds in methyl alcohol simultaneously, make the solution of every 1ml containing rutin 0.1mg, Hyperoside 0.3mg, product solution in contrast; Separately get the compound ambrette particle negative sample 5g except sunset abelmoschus flower medicinal material, add methyl alcohol 10mL, put in ultrasound wave and process 20min and fully dissolve, filter, get filtrate as negative control solution.
Draw each 5 μ L of above-mentioned three kinds of solution, put respectively on same polyamide film, with 70% glacial acetic acid for developping agent, exhibition, apart from 6cm, is taken out, is dried, spray with aluminium choride test solution, hot blast drying, inspect under putting ultraviolet lamp (365nm).Chromatogram is as Fig. 4, and in test sample chromatogram, on the position corresponding to reference substance chromatogram, the fluorescence spot of aobvious same color, negative control sample, without corresponding spot, can judge in differentiated finished drug product thus containing sunset abelmoschus flower medicinal material.
Claims (4)
1. a discrimination method for sunset abelmoschus flower medicinal material is with rutin, Hyperoside and Quercetin for reference substance, and adopt thin-layered chromatography to differentiate, concrete grammar comprises:
Get sunset abelmoschus flower medicinal powder 0.1 ~ 0.5g, add C
1 ~ 4monohydroxy alcohol 10ml, after fully dissolving, filters, gets filtrate as need testing solution;
Get rutin, Hyperoside, Quercetin reference substance respectively, with C
1 ~ 4monohydroxy alcohol makes the solution of every 1ml containing rutin 0.05 ~ 0.1mg, Hyperoside 0.1 ~ 0.3mg, Quercetin 0.05 ~ 0.1mg, as control substance of Rutin solution, Hyperoside reference substance solution and Quercetin reference substance solution; Or rutin, Hyperoside and Quercetin reference substance are dissolved in C simultaneously
1 ~ 4in monohydroxy alcohol, make the solution of every 1ml containing rutin 0.05 ~ 0.1mg, Hyperoside 0.1 ~ 0.3mg, Quercetin 0.05 ~ 0.1mg, product solution in contrast;
Draw above-mentioned need testing solution and each 2 ~ 10 μ L of reference substance solution respectively, put on same polyamide film, with 60 ~ 75% glacial acetic acid for developping agent, exhibition, apart from 6cm, is taken out, is dried, spray with aluminium choride test solution, hot blast drying, inspect under putting 365nm ultraviolet lamp; In test sample chromatogram, on the position corresponding to each reference substance chromatogram, the fluorescence spot of aobvious same color.
2. a discrimination method for sunset abelmoschus flower medicinal material is with rutin, Hyperoside for reference substance, and adopt thin-layered chromatography to differentiate, concrete grammar comprises:
Get sunset abelmoschus flower medicinal powder 0.1 ~ 0.5g, or be equivalent to 0.1 ~ 0.5g sunset abelmoschus flower medicinal material containing sunset abelmoschus flower medicinal material manufactured goods powder, add C
1 ~ 4monohydroxy alcohol 10ml, after fully dissolving, filters, gets filtrate as need testing solution;
Get rutin, Hyperoside reference substance respectively, with C
1 ~ 4monohydroxy alcohol makes the solution of every 1ml containing rutin 0.05 ~ 0.1mg, Hyperoside 0.1 ~ 0.3mg, as control substance of Rutin solution, Hyperoside reference substance solution; Or rutin, Hyperoside reference substance are dissolved in C simultaneously
1 ~ 4in monohydroxy alcohol, make the solution of every 1ml containing rutin 0.05 ~ 0.1mg, Hyperoside 0.1 ~ 0.3mg, product solution in contrast;
Draw above-mentioned need testing solution and each 2 ~ 10 μ L of reference substance solution respectively, put on same polyamide film, with 60 ~ 75% glacial acetic acid for developping agent, exhibition, apart from 6cm, is taken out, is dried, spray with aluminium choride test solution, hot blast drying, inspect under putting 365nm ultraviolet lamp; In test sample chromatogram, on the position corresponding to each reference substance chromatogram, the fluorescence spot of aobvious same color.
3. the discrimination method of sunset abelmoschus flower medicinal material according to claim 1 and 2, is characterized in that described abundant dissolving solution is placed in ultrasound wave process 20min.
4. the discrimination method of sunset abelmoschus flower medicinal material according to claim 1 and 2, is characterized in that described developping agent is 70% glacial acetic acid.
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| RU2469316C1 (en) * | 2011-05-06 | 2012-12-10 | Государственное образовательное учреждение высшего профессионального образования "Воронежский государственный университет" (ГОУ ВПО ВГУ) | Method for quantitative determination of rutin via thin-layer chromatography |
| CN103018371A (en) * | 2012-12-24 | 2013-04-03 | 江苏苏中药业集团股份有限公司 | Quality control method of sunset abelmoschus root medicinal material as well as extract and preparation of sunset abelmoschus root |
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| CN103018371A (en) * | 2012-12-24 | 2013-04-03 | 江苏苏中药业集团股份有限公司 | Quality control method of sunset abelmoschus root medicinal material as well as extract and preparation of sunset abelmoschus root |
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