CN107576751A - The discrimination method of ginseng in ginseng antler medical liquor - Google Patents
The discrimination method of ginseng in ginseng antler medical liquor Download PDFInfo
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- CN107576751A CN107576751A CN201710625119.1A CN201710625119A CN107576751A CN 107576751 A CN107576751 A CN 107576751A CN 201710625119 A CN201710625119 A CN 201710625119A CN 107576751 A CN107576751 A CN 107576751A
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- ginseng
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- butanol
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- 241000208340 Araliaceae Species 0.000 title claims abstract description 92
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 title claims abstract description 92
- 235000003140 Panax quinquefolius Nutrition 0.000 title claims abstract description 92
- 235000008434 ginseng Nutrition 0.000 title claims abstract description 92
- 210000003056 antler Anatomy 0.000 title claims abstract description 46
- 238000012850 discrimination method Methods 0.000 title claims abstract description 39
- 239000013558 reference substance Substances 0.000 claims abstract description 94
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229930182494 ginsenoside Natural products 0.000 claims abstract description 24
- 229940089161 ginsenoside Drugs 0.000 claims abstract description 20
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 97
- 238000012360 testing method Methods 0.000 claims description 75
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 60
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 52
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 37
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- 238000002360 preparation method Methods 0.000 claims description 20
- 239000000047 product Substances 0.000 claims description 15
- 239000007921 spray Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000000741 silica gel Substances 0.000 claims description 13
- 229910002027 silica gel Inorganic materials 0.000 claims description 13
- 235000019640 taste Nutrition 0.000 claims description 13
- 238000009835 boiling Methods 0.000 claims description 11
- 238000011161 development Methods 0.000 claims description 11
- 238000002474 experimental method Methods 0.000 claims description 11
- 238000000605 extraction Methods 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000292 calcium oxide Substances 0.000 claims description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- NJUISRMVIKYYCN-UHFFFAOYSA-N acetic acid;chloroform;methanol;hydrate Chemical compound O.OC.CC(O)=O.ClC(Cl)Cl NJUISRMVIKYYCN-UHFFFAOYSA-N 0.000 claims description 5
- 239000002021 butanolic extract Substances 0.000 claims description 3
- GGISZLOBBISXOZ-UHFFFAOYSA-N acetic acid;chloroform Chemical compound CC(O)=O.ClC(Cl)Cl GGISZLOBBISXOZ-UHFFFAOYSA-N 0.000 claims description 2
- ROAYSRAUMPWBQX-UHFFFAOYSA-N ethanol;sulfuric acid Chemical compound CCO.OS(O)(=O)=O ROAYSRAUMPWBQX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000284 extract Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 239000000523 sample Substances 0.000 claims 6
- 238000010521 absorption reaction Methods 0.000 claims 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 238000005984 hydrogenation reaction Methods 0.000 claims 1
- 239000012488 sample solution Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 239000013642 negative control Substances 0.000 abstract description 6
- 239000000470 constituent Substances 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 238000007689 inspection Methods 0.000 abstract description 2
- 230000006641 stabilisation Effects 0.000 abstract description 2
- 238000011105 stabilization Methods 0.000 abstract description 2
- HYGYSIDIKIGPJA-UHFFFAOYSA-N chloroform;ethyl acetate;methanol Chemical compound OC.ClC(Cl)Cl.CCOC(C)=O HYGYSIDIKIGPJA-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 77
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 9
- 229930182490 saponin Natural products 0.000 description 9
- 150000007949 saponins Chemical class 0.000 description 9
- 239000003814 drug Substances 0.000 description 5
- YEZWWUMWIFKEQM-UHFFFAOYSA-N O.OC.ClC(Cl)Cl.CCOC(C)=O Chemical compound O.OC.ClC(Cl)Cl.CCOC(C)=O YEZWWUMWIFKEQM-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229940026314 red yeast rice Drugs 0.000 description 4
- 210000000582 semen Anatomy 0.000 description 4
- 241000427159 Achyranthes Species 0.000 description 3
- 239000009636 Huang Qi Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000004809 thin layer chromatography Methods 0.000 description 3
- 235000014101 wine Nutrition 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 241000005787 Cistanche Species 0.000 description 2
- 241000208966 Polygala Species 0.000 description 2
- 241000405414 Rehmannia Species 0.000 description 2
- 240000006079 Schisandra chinensis Species 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 210000003734 kidney Anatomy 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 210000004072 lung Anatomy 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 210000000952 spleen Anatomy 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000020097 white wine Nutrition 0.000 description 2
- 235000002722 Dioscorea batatas Nutrition 0.000 description 1
- 235000006536 Dioscorea esculenta Nutrition 0.000 description 1
- 240000001811 Dioscorea oppositifolia Species 0.000 description 1
- 235000003416 Dioscorea oppositifolia Nutrition 0.000 description 1
- UFNDONGOJKNAES-UHFFFAOYSA-N Ginsenoside Rb1 Natural products CC(=CCCC(C)(OC1OC(COC2OC(CO)C(O)C(O)C2O)C(O)C(O)C1O)C3CCC4(C)C3C(O)CC5C6(C)CCC(OC7OC(CO)C(O)C(O)C7OC8OC(CO)C(O)C(O)C8O)C(C)(C)C6CC(O)C45C)C UFNDONGOJKNAES-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- -1 Methane-acetate-methanol-water Chemical compound 0.000 description 1
- 244000197580 Poria cocos Species 0.000 description 1
- 235000008599 Poria cocos Nutrition 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- GZYPWOGIYAIIPV-JBDTYSNRSA-N ginsenoside Rb1 Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)O[C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(CC[C@H]4C(C)(C)[C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O)CC[C@]4(C)[C@H]3C[C@H]2O)C)(C)CC1)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O GZYPWOGIYAIIPV-JBDTYSNRSA-N 0.000 description 1
- TXEWRVNOAJOINC-UHFFFAOYSA-N ginsenoside Rb2 Natural products CC(=CCCC(OC1OC(COC2OCC(O)C(O)C2O)C(O)C(O)C1O)C3CCC4(C)C3C(O)CC5C6(C)CCC(OC7OC(CO)C(O)C(O)C7OC8OC(CO)C(O)C(O)C8O)C(C)(C)C6CCC45C)C TXEWRVNOAJOINC-UHFFFAOYSA-N 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000012372 quality testing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 235000015961 tonic Nutrition 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
- 229960000716 tonics Drugs 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of discrimination method of ginseng in ginseng antler medical liquor, is with ginsenoside Rb1Reference substance is control, with chloroform ethyl acetate methanol water=10~20 placed at 10 DEG C:30~50:18~25:5~15 subnatant is the thin-layered chromatography of solvent.The discrimination method of ginseng in a kind of ginseng antler medical liquor provided by the invention, operation possibility is stronger, can realize and efficiently and accurately differentiate constituent of ginseng in ginseng antler medical liquor.The method controllability of the present invention is higher, simple to operate, separating degree is high, favorable reproducibility, and negative control is noiseless, and different manufacturers lamellae and temperature, damp condition do not influence.Discrimination method of the present invention constituent of ginseng in ginseng antler medical liquor can be carried out it is accurate, comprehensive, scientifical it is effective differentiate, improve quality inspection standard, further ensure that the stabilization, safely, effectively of product quality.
Description
Technical field
The present invention relates to the discrimination method of ginseng in ginseng antler medical liquor, particularly belongs to Chinese medicine detection technique field.
Background technology
Ginseng antler medical liquor is by Semen Cuscutae, the root of bidentate achyranthes, prepared rhizome of rehmannia, saline cistanche, pilose antler, ginseng, gun tab, the Radix Astragali, the fruit of Chinese magnoliavine, mountain
Made of medicine, Radix Angelicae Sinensis, keel, polygala (system) and red yeast rice.Function is strengthening by means of tonics, helps gas-solid smart.Ginseng in side, based on Semen Cuscutae
Medicine, play and reinforce vital energy, benefiting qi for promoting production of blood, tonify the liver and kidney, the effect of astringent sperm contracting urine, be equipped with the root of bidentate achyranthes, pilose antler, the Radix Astragali, Radix Angelicae Sinensis, the five tastes
The tonifying kidney and benefiting sperm blood-nourishing such as son, strengthen drug effect.The discriminating of ginseng is not directed in the quality standard of existing ginseng antler medical liquor, therefore, is ground
Study carefully a kind of method that can efficiently, accurately differentiate ginseng in ginseng antler medical liquor, lift the quality standard of ginseng antler medical liquor, be advantageous to ginseng antler medical liquor
Quality testing, it appears particularly necessary.
The content of the invention
, can it is an object of the invention to a kind of discrimination method of ginseng in ginseng antler medical liquor to solve the deficiencies in the prior art
Efficiently and accurately ginseng in discriminating ginseng antler medical liquor, separating degree are good.
The ginseng antler medical liquor of the present invention, is by Semen Cuscutae 6g, root of bidentate achyranthes 4g, prepared rhizome of rehmannia 4g, saline cistanche 4g, pilose antler 2g, ginseng 2g, big gun
Tag 2g, Radix Astragali 2g, fruit of Chinese magnoliavine 2g, Poria cocos 2g, Chinese yam 2g, Radix Angelicae Sinensis 2g, keel 2g, polygala (system) 2g and red yeast rice 1g are made.With
Upper ten five tastes, pilose antler, ginseng are ground into coarse powder, standby.In addition to red yeast rice, the taste of Semen Cuscutae etc. 12 is cataclasm for remaining, add white wine 800g,
With putting in tank, capping water proof heating is stewed to being poured into during boiling in cylinder and sealed, and is soaked for sucrose 80g and the coarse powder such as red yeast rice and above-mentioned pilose antler
Leaching wine liquid after 30 days, dregs of a decoction recovery white wine, press juice merge with the wine liquid of recovery wine liquid and leaching after residue squeezing, filter,
800mL is made, it is filling, produce.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that：
The discrimination method of ginseng in ginseng antler medical liquor, it is with ginsenoside Rb1Reference substance is control, with the trichlorine placed at 10 DEG C
Methane-acetate-methanol-water=10~20:30~50:18~25:5~15 subnatant is the thin-layer chromatography of solvent
Method.
In foregoing ginseng antler medical liquor in the discrimination method of ginseng, specific discrimination method comprises the following steps：
(1) preparation of need testing solution：This product is taken, in evaporating into no alcohol taste in water-bath, calcium oxide is hydrogenated with, stirs evenly, put boiling
Heat, take out, room temperature natural cooling in water-bath, filtration, filtrate, which adds diethyl ether, shakes extraction, discards ether layer, water layer water saturation
N-butanol extraction, merge n-butanol liquid；Washed with ammonia solution, merge n-butanol liquid；The water washing of n-butanol saturation is used again, is closed
And n-butanol liquid, it is evaporated, residue adds methanol to make its dissolving, as need testing solution；
(2) preparation of reference substance solution：Take ginsenoside Rb1Reference substance, add methanol to be made in every 1mL and contain 0.5mg people
Join saponin(e Rb1The solution of reference substance, as reference substance solution；
(3) differentiate：According to《Chinese Pharmacopoeia》Four thin-layered chromatography of general rule 0502 experiments of version in 2015, it is molten to draw reference substance
Liquid, need testing solution, put respectively on same silica gel g thin-layer plate, with place at 10 DEG C chloroform-acetate-methanol-
Water=10~20:30~50:18~25:5~15 subnatant is solvent, is deployed, and takes out, dries, spray the sulfuric acid with 10%
Ethanol solution, it is clear to be heated to spot development at 105 DEG C, puts and is inspected under daylight, in test sample chromatogram, with reference substance chromatogram
On relevant position, show the spot of same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, with reference substance chromatogram
On relevant position, show the fluorescence spot of same color.
Further, in foregoing ginseng antler medical liquor in the discrimination method of ginseng, specific discrimination method comprises the following steps：
(1) preparation of need testing solution：90~110mL of this product is taken, in evaporating into no alcohol taste in water-bath, is hydrogenated with calcium oxide
0.3~0.8g, stir evenly, put and 15min is heated in boiling water bath, take out, room temperature natural cooling, filtration, filtrate add diethyl ether 30mL~
50mL, shaking extraction, ether layer is discarded, water layer is extracted 2~4 times with water saturated n-butanol, every time using water saturated positive fourth
Alcohol 30mL~50mL, merge n-butanol liquid；Washed 2~3 times, each 45mL~55mL with ammonia solution, merge n-butanol liquid；Use again
The water washing of n-butanol saturation 2~4 times, each 45mL~55mL, merge n-butanol liquid, be evaporated, residue adds methanol 0.5mL to make it
Dissolving, as need testing solution；
(2) preparation of reference substance solution：Take ginsenoside Rb1Reference substance, add methanol to be made in every 1mL and contain 0.5mg people
Join saponin(e Rb1The solution of reference substance, as reference substance solution；
(3) differentiate：According to《Chinese Pharmacopoeia》Four thin-layered chromatography of general rule 0502 experiments of version in 2015, draw reference substance solution
5~10 μ L, the μ L of need testing solution 5~10, put respectively on same silica gel g thin-layer plate, with the chloroform-second placed at 10 DEG C
Acetoacetic ester-methanol-water=10~20:30~50:18~25:5~15 subnatant is solvent, is deployed, and takes out, dries, and is sprayed
With 10% ethanol solution of sulfuric acid, it is clear to be heated to spot development at 105 DEG C, puts and is inspected under daylight, in test sample chromatogram,
With on reference substance chromatogram relevant position, showing the spot of same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram,
With on reference substance chromatogram relevant position, showing the fluorescence spot of same color.
Preferably, in foregoing ginseng antler medical liquor in the discrimination method of ginseng, specific discrimination method comprises the following steps：
(1) preparation of need testing solution：This product 100mL is taken, in evaporating into no alcohol taste in water-bath, is hydrogenated with calcium oxide 0.5g,
Stir evenly, put and 15min is heated in boiling water bath, take out, room temperature natural cooling, filtration, filtrate adds diethyl ether 40mL, shaking extraction, discards
Ether layer, water layer with water saturated n-butanol extract 3 times, every time using water saturated n-butanol be respectively 50mL, 40mL,
30mL, merge n-butanol liquid；Washed 2 times, each 50mL with ammonia solution, merge n-butanol liquid；The washing of n-butanol saturation is used again
Wash 2 times, each 50mL, merge n-butanol liquid, be evaporated, residue adds methanol 0.5mL to make its dissolving, as need testing solution；
(2) preparation of reference substance solution：Take ginsenoside Rb1Reference substance, add methanol to be made in every 1mL and contain 0.5mg people
Join saponin(e Rb1The solution of reference substance, as reference substance solution；
(3) differentiate：According to《Chinese Pharmacopoeia》Four thin-layered chromatography of general rule 0502 experiments of version in 2015, draw reference substance solution
8 μ L, the μ L of need testing solution 8, put respectively on same silica gel g thin-layer plate, with place at 10 DEG C chloroform-ethyl acetate-
Methanol-water=15:40:22:10 subnatant is solvent, is deployed, and takes out, dries, spray the ethanol solution of sulfuric acid with 10%,
It is clear that spot development is heated at 105 DEG C, puts and is inspected under daylight, in test sample chromatogram, with reference substance chromatogram relevant position,
The spot of aobvious same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, with reference substance chromatogram relevant position,
The fluorescence spot of aobvious same color.
In order to ensure discrimination method science of the present invention, reasonable, feasible, the discrimination method of the present invention is studied and examined
Examine.Ginseng, nature and flavor：Sweet, slight bitter, it is warm-natured, flat.Returns spleen, lung channel, the heart channel of Hang-Shaoyin.Reinforce vital energy, veins takes off admittedly, reinforce the spleen to benefit the lung, it is raw
Tianjin, calm the nerves.Ginseng is main ingredient in side, ginsenoside Rb1It is its specificity composition in side.Therefore, this experiment will choose people
Join saponin(e Rb1Reference substance extracts the ginsenoside Rb of ginseng in this product by water saturated n-butanol as compareing1Composition, to people
Join medicinal material and carry out thin layer discriminating, and investigate different point sample amounts, different manufacturers lamellae, different temperatures, different humidity in this product
The influence of ginseng crude drug's thin-layer chromatography.Result of the test shows：With ginsenoside Rb1Reference substance is control, with what is placed at 10 DEG C
Chloroform-acetate-methanol-water=10~20:30~50:18~25:5~15 subnatant is solvent, to ginseng
The thin-layered chromatography feature differentiated is obvious, and specificity is strong, can be as the discrimination method of ginseng in this product.
1st, instrument and reagent
MS304s/01 electronic balances, METTLER TOLEDO (plum Teller-support benefit), ammoniacal liquor (Chongqing Chuanjiang River chemical reagent
Factory), ether (Tianjin Ke Miou chemical reagent Co., Ltd, analysis are pure), n-butanol (Xilong Chemical Co., Ltd, analysis
It is pure), calcium hydroxide (Xilong Chemical Co., Ltd), P-1 types thin layer chromatograph developing cylinder (the limited public affairs of Xinyi Instrument Factory, Shanghai
Department), silica gel g thin-layer plate (Qingdao Haiyang chemical industry), 5 μ L point samples capillaries (Tianjin Si Lida Science and Technology Ltd.s), SLD-1 is thin
Layer chromatography photographic apparatus (Tianjin Si Lida chromatographic techniques development company).
Ginseng antler medical liquor (20150101,20150102,20150103, Guizhou Xinbang Pharmacy Stock Co., Ltd), ginsenoside
Rb1 reference substances (Nat'l Pharmaceutical ＆ Biological Products Control Institute).
2nd, specificity is investigated
Draw need testing solution, ginsenoside Rb1Reference substance solution, ginseng negative control solution each 8 μ L, it is molten by test sample
Liquid, reference substance solution, negative control solution, respectively at same silica gel g thin-layer plate point sample, deploy, take out, dry, spray with 10%
Ethanol solution of sulfuric acid colour developing, it is clear to be heated to colour developing under the conditions of 105 DEG C, puts examined under daylight and uviol lamp (365nm) respectively
Depending on.In test sample chromatogram, put and inspected under daylight, with reference substance chromatogram relevant position, showing the spot of same color；Put
Inspected under 365nm ultraviolet lamps, with reference substance chromatogram relevant position, showing the fluorescence spot of same color.In negative control
Spot or fluorescence spot of the corresponding position without same color, as shown in Figure 1.Illustrate that the specificity of the inventive method is good.
3rd, the investigation of optimal point sample amount
Respectively need testing solution and reference substance solution 2 in aspiration step (1) and step (2), 3,4,5,6,7,8,10,12,
16 μ L, put on different silica gel g thin-layer plates, investigated respectively, deploy, take out, dry, spray the ethanol solution of sulfuric acid with 10%
Colour developing, colour developing is heated under the conditions of 105 DEG C clearly, puts inspected under daylight and uviol lamp (365nm) respectively.Wherein, test sample 8
μ L point sample amount best results, when point sample amount is more than 10 μ L, there is conditions of streaking in need testing solution position spot, and point sample amount is less than
During 5 μ L, need testing solution position spot unobvious；Effect is good during reference substance solution point sample 5~10 μ L of amount, especially in 8 μ L
Best results, therefore it is 5~10 μ L, the optimal μ L of point sample amount 8 to select need testing solution point sample amount；The μ of reference substance solution point sample amount 5~10
L, the optimal μ L of point sample amount 8.
4th, tolerance is investigated
4.1st, the lamellae of different brands
Draw need testing solution, ginsenoside Rb1Each 8 μ L point samples of reference substance solution, the lamellae of different brands is changed, opened up
Open, take out, dry, spray the ethanol solution of sulfuric acid colour developing with 10%, colour developing is heated under the conditions of 105 DEG C clearly, puts day respectively
Inspected under light and uviol lamp (365nm).As shown in Figures 2 and 3.Put and inspected under daylight, in test sample chromatogram, with reference substance color
Compose on relevant position, show the spot of same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, with reference substance color
Compose on relevant position, show the fluorescence spot of same color.And after changing different lamellaes, without significant difference, table between each lamellae
Bright different brands lamellae of changing differentiates without influence on the thin layer of ginseng.
4.2nd, temperature
Draw need testing solution, ginsenoside Rb1Each 8 μ L point samples of reference substance solution, convert different temperature conditionss, exhibition
Open, take out, dry, spray the ethanol solution of sulfuric acid colour developing with 10%, colour developing is heated under the conditions of 105 DEG C clearly, puts day respectively
Inspected under light and uviol lamp (365nm).As shown in Figure 4 and Figure 5.Put and inspected under daylight, in test sample chromatogram, with reference substance color
Compose on relevant position, show the spot of same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, with reference substance color
Compose on relevant position, show the fluorescence spot of same color.And after conversion different temperatures, without significant difference between each lamellae, show
Different temperatures is converted to differentiate without influence the thin layer of ginseng.
4.3rd, humidity
Draw need testing solution, ginsenoside Rb1Each 8 μ L point samples of reference substance solution, convert different damp conditions, exhibition
Open, take out, dry, spray the ethanol solution of sulfuric acid colour developing with 10%, colour developing is heated under the conditions of 105 DEG C clearly, puts day respectively
Inspected under light and uviol lamp (365nm).As shown in Figure 6 and Figure 7.Put and inspected under daylight, in test sample chromatogram, with reference substance color
Compose on relevant position, show the spot of same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, with reference substance color
Compose on relevant position, show the fluorescence spot of same color.And after conversion different humidity, without significant difference between each lamellae, show
Different humidity is converted to differentiate without influence the thin layer of ginseng.
5th, with the comparison of existing discrimination method
The inventive method differentiates that object is ginseng in ginseng antler medical liquor, and ginseng antler medical liquor prescription includes the high medicinal material of many sugar contents.
With《Chinese Pharmacopoeia》The discrimination method of the two middle ginseng crude drugs of version in 2015 compares, inventive process have the advantage that the system of sample
Desugar processing is carried out during standby, appropriate calcium hydroxide is added and removes most of sugar in test sample, so as to ensure final expansion
Effect.In order to prove that the superiority of ability is sweetened off in the inventive method, take differentiated with a batch of ginseng antler medical liquor with the present invention respectively
Method and the discrimination method of existing ginseng are tested, the results showed that the expansion of this programme works well and do not trailed, existing
Ginseng discrimination method separating effect is poor.
The present invention is advantageous in that：The discrimination method of ginseng in a kind of ginseng antler medical liquor provided by the invention, operation are feasible
Property it is stronger, can realize efficiently and accurately differentiate ginseng antler medical liquor in constituent of ginseng.The method controllability of the present invention is higher, operation letter
It is single, separating degree is high, favorable reproducibility, and negative control is noiseless, different manufacturers lamellae and temperature, damp condition not shadow
Ring.Discrimination method of the present invention can carry out accurate, comprehensive, scientifical effective discriminating to constituent of ginseng in ginseng antler medical liquor, improve matter
Examination criteria is measured, further ensure that the stabilization, safely, effectively of product quality.
Brief description of the drawings
Fig. 1 is that the specificity of ginseng in ginseng antler medical liquor of the invention differentiates collection of illustrative plates；
Fig. 2 is using the chromatogram of Qingdao Haiyang lamellae when ginseng differentiates in ginseng antler medical liquor；
Fig. 3 is using the chromatogram of Yantai Chemical Industry Research Inst.'s lamellae when ginseng differentiates in ginseng antler medical liquor；
Fig. 4 is the chromatogram that temperature is 25 DEG C when ginseng differentiates in ginseng antler medical liquor；
Fig. 5 is the chromatogram that temperature is 8 DEG C when ginseng differentiates in ginseng antler medical liquor；
Fig. 6 is the chromatogram that humidity is 32% when ginseng differentiates in ginseng antler medical liquor；
Fig. 7 is the chromatogram that humidity is 72% when ginseng differentiates in ginseng antler medical liquor；
The implication of reference in figure：Fig. 1:1- test sample lot number 20150101,2- test sample lot number 20150102,3- people
Join saponin(e Rb1Reference substance, 4- negative controls, 5- test samples lot number 20150103, A- daylight is inspected, B- uviol lamps (365nm) inspection
Depending on；Fig. 2~Fig. 7：1- test sample lot number 20150101,2- test sample lot number 20150102,3- ginsenosides Rb1Reference substance, 4-
Test sample lot number 20150103, A- daylight are inspected, and B- uviol lamps (365nm) are inspected.
Embodiment
The present invention is further introduced below in conjunction with specific embodiment.
Embodiment 1
The discrimination method of ginseng in ginseng antler medical liquor, specific discrimination method comprise the following steps：
(1) preparation of need testing solution：This product 90mL is taken, in evaporating into no alcohol taste in water-bath, calcium oxide 0.3g is hydrogenated with, stirs
It is even, put and 15min is heated in boiling water bath, take out, room temperature natural cooling, filtration, filtrate adds diethyl ether 30mL, shaking extraction, discards second
Ether layer, water layer are extracted 2 times with water saturated n-butanol, every time using water saturated n-butanol 30mL, merge n-butanol liquid；Use ammonia
Test solution washs 2 times, each 45mL, merges n-butanol liquid；Again with the water washing 2 times of n-butanol saturation, each 55mL, merge positive fourth
Alcohol liquid, is evaporated, and residue adds methanol 0.5mL to make its dissolving, as need testing solution；
(2) preparation of reference substance solution：Take ginsenoside Rb1Reference substance, add methanol to be made in every 1mL and contain 0.5mg people
Join saponin(e Rb1The solution of reference substance, as reference substance solution；
(3) differentiate：According to《Chinese Pharmacopoeia》Four thin-layered chromatography of general rule 0502 experiments of version in 2015, draw reference substance solution
5 μ L, the μ L of need testing solution 5, put respectively on same silica gel g thin-layer plate, with place at 10 DEG C chloroform-ethyl acetate-
Methanol-water=10:30:18:5 subnatant is solvent, is deployed, and takes out, dries, spray the ethanol solution of sulfuric acid with 10%,
It is clear that spot development is heated at 105 DEG C, puts and is inspected under daylight, in test sample chromatogram, with reference substance chromatogram relevant position,
The spot of aobvious same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, with reference substance chromatogram relevant position,
The fluorescence spot of aobvious same color.
Embodiment 2
The discrimination method of ginseng in ginseng antler medical liquor, specific discrimination method comprise the following steps：
(1) preparation of need testing solution：This product 110mL is taken, in evaporating into no alcohol taste in water-bath, is hydrogenated with calcium oxide 0.8g,
Stir evenly, put and 15min is heated in boiling water bath, take out, room temperature natural cooling, filtration, filtrate adds diethyl ether 50mL, shaking extraction, discards
Ether layer, water layer are extracted 4 times with water saturated n-butanol, every time using water saturated n-butanol 50mL, merge n-butanol liquid；With
Ammonia solution washs 3 times, each 55mL, merges n-butanol liquid；The water washing 4 times, each 45mL of n-butanol saturation is used again, is merged just
Butanol liquid, is evaporated, and residue adds methanol 0.5mL to make its dissolving, as need testing solution；
(2) preparation of reference substance solution：Take ginsenoside Rb1Reference substance, add methanol to be made in every 1mL and contain 0.5mg people
Join saponin(e Rb1The solution of reference substance, as reference substance solution；
(3) differentiate：According to《Chinese Pharmacopoeia》Four thin-layered chromatography of general rule 0502 experiments of version in 2015, draw reference substance solution
10 μ L, the μ L of need testing solution 10, put respectively on same silica gel g thin-layer plate, with the chloroform-acetic acid second placed at 10 DEG C
Ester-methanol-water=20:50:25:15 subnatant is solvent, is deployed, and takes out, dries, spray molten with 10% sulfuric acid ethanol
Liquid, it is clear to be heated to spot development at 105 DEG C, puts and is inspected under daylight, in test sample chromatogram, with reference substance chromatogram corresponding positions
Put, show the spot of same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, with reference substance chromatogram corresponding positions
Put, show the fluorescence spot of same color.
Embodiment 3
The discrimination method of ginseng in ginseng antler medical liquor, specific discrimination method comprise the following steps：
(1) preparation of need testing solution：This product 100mL is taken, in evaporating into no alcohol taste in water-bath, is hydrogenated with calcium oxide 0.5g,
Stir evenly, put and 15min is heated in boiling water bath, take out, room temperature natural cooling, filtration, filtrate adds diethyl ether 40mL, shaking extraction, discards
Ether layer, water layer with water saturated n-butanol extract 3 times, every time using water saturated n-butanol be respectively 50mL, 40mL,
30mL, merge n-butanol liquid；Washed 2 times, each 50mL with ammonia solution, merge n-butanol liquid；The washing of n-butanol saturation is used again
Wash 2 times, each 50mL, merge n-butanol liquid, be evaporated, residue adds methanol 0.5mL to make its dissolving, as need testing solution；
(2) preparation of reference substance solution：Take ginsenoside Rb1Reference substance, add methanol to be made in every 1mL and contain 0.5mg people
Join saponin(e Rb1The solution of reference substance, as reference substance solution；
(3) differentiate：According to《Chinese Pharmacopoeia》Four thin-layered chromatography of general rule 0502 experiments of version in 2015, draw reference substance solution
8 μ L, the μ L of need testing solution 8, put respectively on same silica gel g thin-layer plate, with place at 10 DEG C chloroform-ethyl acetate-
Methanol-water=15:40:22:10 subnatant is solvent, is deployed, and takes out, dries, spray the ethanol solution of sulfuric acid with 10%,
It is clear that spot development is heated at 105 DEG C, puts and is inspected under daylight, in test sample chromatogram, with reference substance chromatogram relevant position,
The spot of aobvious same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, with reference substance chromatogram relevant position,
The fluorescence spot of aobvious same color.
Embodiment 4
The discrimination method of ginseng in ginseng antler medical liquor, specific discrimination method comprise the following steps：
(1) preparation of need testing solution：This product 95mL is taken, in evaporating into no alcohol taste in water-bath, calcium oxide 0.6g is hydrogenated with, stirs
It is even, put and 15min is heated in boiling water bath, take out, room temperature natural cooling, filtration, filtrate adds diethyl ether 35mL, shaking extraction, discards second
Ether layer, water layer are extracted 2 times with water saturated n-butanol, the use of water saturated n-butanol are respectively every time 45mL, 35mL, merge just
Butanol liquid；Washed 3 times, each 48mL with ammonia solution, merge n-butanol liquid；Again with the water washing 2 times of n-butanol saturation, every time
52mL, merge n-butanol liquid, be evaporated, residue adds methanol 0.5mL to make its dissolving, as need testing solution；
(2) preparation of reference substance solution：Take ginsenoside Rb1Reference substance, add methanol to be made in every 1mL and contain 0.5mg people
Join saponin(e Rb1The solution of reference substance, as reference substance solution；
(3) differentiate：According to《Chinese Pharmacopoeia》Four thin-layered chromatography of general rule 0502 experiments of version in 2015, draw reference substance solution
6 μ L, the μ L of need testing solution 9, put respectively on same silica gel g thin-layer plate, with place at 10 DEG C chloroform-ethyl acetate-
Methanol-water=12:35:19:13 subnatant is solvent, is deployed, and takes out, dries, spray the ethanol solution of sulfuric acid with 10%,
It is clear that spot development is heated at 105 DEG C, puts and is inspected under daylight, in test sample chromatogram, with reference substance chromatogram relevant position,
The spot of aobvious same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, with reference substance chromatogram relevant position,
The fluorescence spot of aobvious same color.
Claims (4)
1. the discrimination method of ginseng in ginseng antler medical liquor, it is characterised in that：The discrimination method is with ginsenoside Rb1Reference substance is pair
According to chloroform-acetate-methanol-water=10~20 placed at 10 DEG C:30~50:18~25:5~15 lower floor
Liquid is the thin-layered chromatography of solvent.
2. the discrimination method of ginseng in ginseng antler medical liquor according to claim 1, it is characterised in that：Specific discrimination method includes
Following steps：
(1) preparation of need testing solution：This product is taken, in evaporating into no alcohol taste in water-bath, calcium oxide is hydrogenated with, stirs evenly, put boiling water bath
Middle heating, take out, room temperature natural cooling, filtration, filtrate adds diethyl ether shaking extraction, discards ether layer, water layer with it is water saturated just
Butanol extracts, and merges n-butanol liquid；Washed with ammonia solution, merge n-butanol liquid；The water washing of n-butanol saturation is used again, is merged just
Butanol liquid, is evaporated, and residue adds methanol to make its dissolving, as need testing solution；
(2) preparation of reference substance solution：Take ginsenoside Rb1Reference substance, add methanol to be made in every 1mL and contain 0.5mg ginsenosides
Rb1The solution of reference substance, as reference substance solution；
(3) differentiate：According to《Chinese Pharmacopoeia》Four thin-layered chromatography of general rule 0502 experiments of version in 2015, draw reference substance solution, supply
Test sample solution, put respectively on same silica gel g thin-layer plate, with place at 10 DEG C chloroform-acetate-methanol-water=
10~20:30~50:18~25:5~15 subnatant is solvent, is deployed, and takes out, dries, spray the sulfuric acid ethanol with 10%
Solution, it is clear to be heated to spot development at 105 DEG C, puts and is inspected under daylight, in test sample chromatogram, corresponding to reference substance chromatogram
On position, show the spot of same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, corresponding to reference substance chromatogram
On position, show the fluorescence spot of same color.
3. the discrimination method of ginseng in ginseng antler medical liquor according to claim 2, it is characterised in that：Specific discrimination method includes
Following steps：
(1) preparation of need testing solution：90~110mL of this product is taken, in evaporating into no alcohol taste in water-bath, hydrogenation calcium oxide 0.3~
0.8g, stir evenly, put and 15min is heated in boiling water bath, take out, room temperature natural cooling, filtration, filtrate adds diethyl ether 30mL~50mL, shakes
Shake extraction, discard ether layer, water layer extracts 2~4 times with water saturated n-butanol, every time using water saturated n-butanol 30mL~
50mL, merge n-butanol liquid；Washed 2~3 times, each 45mL~55mL with ammonia solution, merge n-butanol liquid；Satisfied again with n-butanol
The water washing of sum 2~4 times, each 45mL~55mL, merge n-butanol liquid, be evaporated, residue adds methanol 0.5mL to make its dissolving, makees
For need testing solution；
(2) preparation of reference substance solution：Take ginsenoside Rb1Reference substance, add methanol to be made in every 1mL and contain 0.5mg ginsenosides
Rb1The solution of reference substance, as reference substance solution；
(3) differentiate：According to《Chinese Pharmacopoeia》Four thin-layered chromatography of general rule 0502 experiments of version in 2015, absorption reference substance solution 5~
10 μ L, the μ L of need testing solution 5~10, put respectively on same silica gel g thin-layer plate, with the chloroform-acetic acid placed at 10 DEG C
Ethyl ester-methanol-water=10~20:30~50:18~25:5~15 subnatant is solvent, deploy, take out, dry, spray with
10% ethanol solution of sulfuric acid, it is clear to be heated to spot development at 105 DEG C, puts and is inspected under daylight, in test sample chromatogram, with
On reference substance chromatogram relevant position, show the spot of same color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, with
On reference substance chromatogram relevant position, show the fluorescence spot of same color.
4. the discrimination method of ginseng in the ginseng antler medical liquor according to Claims 2 or 3, it is characterised in that：Specific discrimination method
Comprise the following steps：
(1) preparation of need testing solution：This product 100mL is taken, in evaporating into no alcohol taste in water-bath, calcium oxide 0.5g is hydrogenated with, stirs evenly,
Put and 15min is heated in boiling water bath, take out, room temperature natural cooling, filtration, filtrate adds diethyl ether 40mL, shaking extraction, discards ether
Layer, water layer are extracted 3 times with water saturated n-butanol, the use of water saturated n-butanol are respectively every time 50mL, 40mL, 30mL, close
And n-butanol liquid；Washed 2 times, each 50mL with ammonia solution, merge n-butanol liquid；Again with the water washing 2 times of n-butanol saturation, often
Secondary 50mL, merge n-butanol liquid, be evaporated, residue adds methanol 0.5mL to make its dissolving, as need testing solution；
(2) preparation of reference substance solution：Take ginsenoside Rb1Reference substance, add methanol to be made in every 1mL and contain 0.5mg ginsenosides
Rb1The solution of reference substance, as reference substance solution；
(3) differentiate：According to《Chinese Pharmacopoeia》Four thin-layered chromatography of general rule 0502 experiments of version in 2015, absorption reference substance solution 8 μ L,
The μ L of need testing solution 8, put respectively on same silica gel g thin-layer plate, with place at 10 DEG C chloroform-acetate-methanol-
Water=15:40:22:10 subnatant is solvent, is deployed, and takes out, dries, spray the ethanol solution of sulfuric acid with 10%, at 105 DEG C
Under to be heated to spot development clear, put and inspected under daylight, in test sample chromatogram, with reference substance chromatogram relevant position, showing phase
With the spot of color；Put and inspected under 365nm ultraviolet lamps, in test sample chromatogram, with reference substance chromatogram relevant position, showing phase
With the fluorescence spot of color.
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| CN116355717A (en) * | 2023-04-20 | 2023-06-30 | 江西大自然制药有限公司 | Ginseng and pilose antler wine and preparation method thereof |
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| CN101306082A (en) * | 2008-06-26 | 2008-11-19 | 广州奇星药业有限公司 | Houkangsan quality control method |
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| CN116355717A (en) * | 2023-04-20 | 2023-06-30 | 江西大自然制药有限公司 | Ginseng and pilose antler wine and preparation method thereof |
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