CN103940943B - A kind of discrimination method of field pennycress medicinal material - Google Patents
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Abstract
The present invention relates to a kind of discrimination method of field pennycress medicinal material, extract medicinal material to be measured and field pennycress standard medicinal material point respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-glacial acetic acid for developping agent launches, inspect under 365nm uviol lamp, medicinal material to be measured and field pennycress standard medicinal material show the blue-fluorescence spot of same color in same position.Field pennycress medicinal material discrimination method specificity of the present invention is strong, favorable reproducibility, effectively can distinguish three kinds of not equal field pennycress, be applicable to all sources field pennycress medicinal material discriminating and containing the discriminating whether containing field pennycress medicinal material in field pennycress medicinal material manufactured goods.
Description
Technical field
The present invention relates to the qualitative of medicinal material and discrimination method, particularly relate to the discrimination method of field pennycress medicinal material.
Background technology
Field pennycress is a kind of more common Chinese herbal medicine, and clinical practice is wider.Patrinia scaniosaefolia begins to be loaded in Shennong's Herbal, has long medicinal history, excavated before summer, the flowers are in blossom in China, shines to half-dried, is bundled into bundle, then dries in the shade.Tang Materia Medica, Compendium of Material Medica all there is medicinal record.Describe from history tree, field pennycress should be the dry herb of patrinia herb patrinia scabiosaefolia Fiscs (PatriniascabiosaefoliaFisch.) or patrima villosa (PatriniavillosaJuss.).Property pungent, bitter, cool, return stomach, large intestine, Liver Channel, clearing heat and detoxicating, removing blood stasis and expelling pus, to swell furunculosis for appendicitis, dysentery, enteritis, hepatitis, eye conjunctivitis, postpartum blood stasis stomachache, carbuncle.
Record and modern study according to the successive dynasties, the whole nation former plant of Patrinia scaniosaefolia used has tens kinds at present, adheres to composite family (northern Patrinia scaniosaefolia), Valerianaceae (field pennycress) and Cruciferae (HERBA THALASPIS) separately.Three kinds of not equal field pennycress replace use comparatively general mutually, its reason is that history tree record differs, more chaotic, adds each department medication custom difference, in very long evolution and various reasons, create many homonyms, phenomenon that different section is of the same name.Practise as the area such as North China, northwest and Beijing-Tianjin two places and do field pennycress with the herb of feverfew north Patrinia scaniosaefolia and congener thereof, field pennycress is then used as with Cruciferae HERBA THALASPIS in the south of the lower reaches of the Yangtze River, and certified products field pennycress only northeastward, Inner Mongol, Shandong, the some areas such as Yunnan use, and have lost the main flow kind status of field pennycress.Although three kinds of field pennycress all have clearing heat and detoxicating effect, but each medicine is all targeted, its source, proterties, composition, nature and flavor, pharmacology, effect all have obvious difference, if indiscriminate mixed abuse, different effects can be produced in clinical application process, the effectively safe and reliable of clinical application certainly will be affected, unfavorable factor is brought to the development of tcm cause.Therefore, must be standard with pharmacopeia, take effective constituent as foundation, rigorous realistic, strictly distinguishes medication, can not substitute mutually.
Chinese Pharmacopoeia one (1977 editions), Shandong Province's Chinese crude drug standard (version in 2002) and Hunan Province's Chinese crude drug standard (version in 2009) etc. have all recorded field pennycress medicinal material, but it differentiates that item is except microscopical characters, what adopt is foaming phenomena and Ultraluminescence phenomenon discrimination method, concrete operations are for " getting the meal 0.5g of this product leaf; add water 10ml; put in water-bath and heat 10 minutes, filter.Filtrate is put in test tube with ground stopper, powerful jolting 1 minute, produces persistent foam, does not disappear in 10 minutes." " get above-mentioned filtered fluid point on filter paper, after dry, observe under putting ultraviolet lamp, aobvious hyacinthine fluorescence, then add 1% sodium hydroxide solution 1, then aobvious greenish yellow fluorescent ".Said method is simple to operate, but specificity is poor, and except field pennycress, northern Patrinia scaniosaefolia and HERBA THALASPIS can occur above-mentioned reaction too, three kinds of not equal field pennycress differences can not be come, to confirm the true and false of field pennycress medicinal material.
Just (the just positive cloud such as positive cloud, Jiang Hong, Kang Tingguo, Deng. patrinia scabiosaefolia Fiscs capsule quality standard research (II). time precious traditional Chinese medical science traditional Chinese medicines, 2003,14 (10): 593 ~ 594) patrinia scabiosaefolia Fiscs herb rubber capsule TLC distinguish and assay research was carried out, its with oleanolic acid-3-0-β-D-Glucose (1 → 3)-α-L-rhamnose-(1 → 2)-β-D-wood sugar for reference substance, adopt chloroform-methanol-water to be developping agent, 10% ethanol solution of sulfuric acid is that developer carries out differentiating and assay.We are with reference to the method, and select field pennycress control medicinal material (middle inspection is made) to differentiate for contrast, find that three kinds of field pennycress medicinal materials all show same phenomenon, the method still cannot distinguish three kinds of field pennycress medicinal materials.
Summary of the invention
The object of this invention is to provide a kind of discrimination method of field pennycress medicinal material, discrimination method specificity provided by the invention is strong, effectively can distinguish three kinds of not equal field pennycress, differentiate rapidly and accurately to field pennycress medicinal material.
Field pennycress medicinal material discrimination method provided by the invention is: respectively with C
1 ~ 4monohydroxy alcohol extracts medicinal material to be measured and field pennycress standard medicinal material, after extracting liquid filtering, point is on same silica gel g thin-layer plate, launch with developping agent, inspect under 365nm uviol lamp, medicinal material to be measured and field pennycress standard medicinal material show the blue-fluorescence spot of same color in same position, wherein, described developping agent is cyclohexane-ethyl acetate-glacial acetic acid, and its volume ratio is 5 ~ 8:5:0.1.
The above-mentioned discrimination method of the present invention is only positive to patrinia herb field pennycress, and other feverfew north Patrinia scaniosaefolias, the equal unstressed configuration display of crucifer HERBA THALASPIS, accurately can distinguish not equal field pennycress.
The concrete discrimination method of field pennycress medicinal material of the present invention is:
1), need testing solution preparation
Get field pennycress medicinal powder 1 ~ 4g, add C
1 ~ 4monohydroxy alcohol 50ml, after fully dissolving, filters, gets filtrate as need testing solution;
2), reference substance solution preparation
Get field pennycress standard medicinal material product in contrast, add C
1 ~ 4monohydroxy alcohol 50ml, after fully dissolving, filters, gets filtrate 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 respectively on same silica gel g thin-layer plate, with volume ratio be the cyclohexane-ethyl acetate-glacial acetic acid of 5 ~ 8:5:0.1 for developping agent, launch, take out, inspect under putting 365nm uviol lamp; In test sample chromatogram, on the position corresponding to reference substance chromatogram, the blue-fluorescence spot of aobvious same color.
In said method of the present invention, step 1) described in abundant dissolving can adopt the dissolving means of various routine, as stirred, vibrating, add hot reflux, ultrasonic process etc., to impel C
1 ~ 4effective constituent in field pennycress 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 30min.
The discrimination method of above-mentioned field pennycress 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, to obtaining best test findings, convenient discriminating.
Preferably, take volume ratio as the cyclohexane-ethyl acetate-glacial acetic acid of 5:5:0.1 be developping agent.According to actual conditions, the ratio of developping agent suitably can be adjusted.
Field pennycress medicinal material discrimination method of the present invention is applicable to single (comprising dry product, fresh goods, Different sources) medicinal material of patrinia herb field pennycress, can be used for the differentiation of patrinia herb field pennycress medicinal material and other section homonym field pennycress.Field pennycress medicinal material discrimination method of the present invention is equally also applicable to the discriminating whether containing field pennycress medicinal material in the various manufactured goods (comprising folk prescription, compound manufactured goods) such as human drugs, food, health products, cosmetics, veterinary drug containing patrinia herb field pennycress medicinal material.
The field pennycress standard medicinal material used in the present invention is prepared by Nat'l Pharmaceutical & Biological Products Control Institute.Differentiate that field pennycress carries out according to the respective specified of Pharmacopoeia of People's Republic of China (version in 2010) with thin-layered chromatography.
Field pennycress standard medicinal material used in the present invention is provided by Nat'l Pharmaceutical & Biological Products Control Institute.Differentiate that operating basis Pharmacopoeia of People's Republic of China (version in the 2010) respective specified of field pennycress is carried out with thin-layered chromatography.
The discrimination method being reference substance with field pennycress standard medicinal material provided by the invention compares with field pennycress medicinal material discrimination method in existing standard and list of references, has the following advantages.
1. specificity is strong, highly sensitive.Adopting discrimination method of the present invention respectively to three kinds of kinds---composite family (northern Patrinia scaniosaefolia), Valerianaceae (field pennycress), Cruciferae (HERBA THALASPIS) plant are differentiated, except patrinia herb field pennycress is positive, all the other comprise northern Patrinia scaniosaefolia and HERBA THALASPIS all shows without blue-fluorescence, accurately can distinguish not equal field pennycress, and reflecting the quality information of medicinal material comparatively all sidedly, method is highly sensitive.And method all cannot distinguish this three kinds of medicinal materials in existing standard and list of references.Therefore, the inventive method can ensure to purchase the accuracy of medicinal material, can in process of production more comprehensively, rapidly inspection judge product quality, ensure the reliable and clinical safety of constant product quality, curative effect.
2. discrimination method is ripe.Differentiate through different experimental conditions and carry out discriminating contrast to many batches of Different sources, dry wet field pennycress medicinal material, the inventive method favorable reproducibility, all accurately can differentiate medicinal material.And then, discrimination method of the present invention is applied to manufactured goods containing field pennycress as the discriminating of Baijiang Tablets, compound ambrette particle, Fu Xue-Ning, Fuyankangfu capsules etc., negative noiseless, there is good identification result equally, the manufactured goods quality containing field pennycress medicinal material and clinical efficacy can be controlled better.
3. discrimination method is simple.The inventive method sample preparation is easy, and testing cost is low, and the running time is short, and whole operating process can complete in 1 hour, chemical reagent used and standard price of medicinal material all very low, can be used for the daily production control of product.
4. discrimination method agents useful for same toxicity is low, consumption is few, and methenyl choloride in list of references selected by field pennycress discrimination method and the equal toxicity of sulfuric acid large, corrosivity is strong.
Embodiment
Embodiment 1
Get each 1g of medicinal powder of feverfew north Patrinia scaniosaefolia, patrinia herb field pennycress, crucifer HERBA THALASPIS respectively, add methyl alcohol 50ml, ultrasound wave process 30min, filter, get filtrate as need testing solution; Get field pennycress standard medicinal material product in contrast, add methyl alcohol 50ml, ultrasound wave process 30min, filter, get filtrate product solution in contrast.Draw above-mentioned need testing solution and each 2 μ L of reference substance solution respectively, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-glacial acetic acid (5:5:0.1) for developping agent, launch, take out, inspect under putting 365nm ultraviolet lamp.On the position corresponding to reference substance chromatogram, feverfew north Patrinia scaniosaefolia and crucifer HERBA THALASPIS unstressed configuration spot, patrinia herb field pennycress shows the blue-fluorescence spot of same color, can distinguish thus judge differentiate medicinal material whether as patrinia herb field pennycress.
Embodiment 2
The present embodiment field pennycress medicinal material derives from Shandong, Jilin, ground, Hunan three respectively.
Get three kinds of each 4g of medicinal powder respectively, add normal butyl alcohol 50ml, ultrasound wave process 30min, filter, get filtrate as need testing solution; Get field pennycress standard medicinal material product in contrast, add normal butyl alcohol 50ml, ultrasound wave process 30min, filter, get filtrate product solution in contrast.Draw above-mentioned need testing solution and each 10 μ L of reference substance solution respectively, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-glacial acetic acid (8:5:0.1) for developping agent, launch, take out, inspect under putting 365nm ultraviolet lamp.On the position corresponding to reference substance chromatogram, the fluorescence spot of all aobvious same color of three ground field pennycress, can judge differentiated medicinal material thus whether as patrinia herb field pennycress.
Embodiment 3
The present embodiment is differentiated the field pennycress medicinal material in Baijiang Tablets, and field pennycress crude drug source used is in Shandong.
Prescription: field pennycress 1000g.
Method for making: get field pennycress 1000g, be ground into meal, after 24 hours, carries out diacolation by 60% alcohol dipping, collects percolate, is condensed into paste, adds right amount of auxiliary materials, make particle, be pressed into 1000, sugar coating, obtain final product below 70 DEG C.
Get Baijiang Tablets 1, add methyl alcohol 50ml, put in ultrasound wave and process 30min and fully dissolve, filter, get filtrate as need testing solution; Get field pennycress standard medicinal material product in contrast, add methyl alcohol 50ml, put in ultrasound wave and process 30min, filter, get filtrate product solution in contrast; By Baijiang Tablets prescription and method for making, get the Baijiang Tablets negative sample 1 except field pennycress, add methyl alcohol 50ml, put in ultrasound wave and process 30min, filter, get filtrate as negative control solution.Draw each 10 μ L of above-mentioned three kinds of solution respectively, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-glacial acetic acid (5:5:0.1) for developping agent, launch, take out, inspect under putting 365nm ultraviolet lamp.On the position corresponding to reference substance chromatogram, the blue-fluorescence spot of aobvious same color, negative control sample, without corresponding spot, can judge Baijiang Tablets medicinal material used thus whether as field pennycress.
Embodiment 4
The present embodiment is differentiated the field pennycress medicinal material in compound ambrette particle, and field pennycress crude drug source used is in Shandong.
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 6g, add methyl alcohol 50ml, put in ultrasound wave and process 30min, filter, get filtrate as need testing solution; Get field pennycress standard medicinal material product in contrast, add methyl alcohol 50ml, put in ultrasound wave and process 30min, filter, get filtrate product solution in contrast; Separately get the compound ambrette particle negative sample 6g except field pennycress medicinal material, add methyl alcohol 50mL, put in ultrasound wave and process 30min, filter, using filtrate as negative control solution.
Draw above-mentioned need testing solution and each 10 μ L of reference substance solution respectively, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-glacial acetic acid (5:5:0.1) for developping agent, launch, take out, inspect under putting 365nm ultraviolet lamp.On the position corresponding to reference substance chromatogram, the blue-fluorescence spot of aobvious same color, negative control sample, without corresponding spot, can judge compound ambrette particle medicinal material used thus whether as field pennycress.
Claims (4)
1. a discrimination method for field pennycress medicinal material is respectively with same C
1 ~ 4monohydroxy alcohol extracts medicinal material to be measured and field pennycress standard medicinal material, after extracting liquid filtering, point is on same silica gel g thin-layer plate, launch with developping agent, inspect under 365nm uviol lamp, medicinal material to be measured and field pennycress standard medicinal material show the blue-fluorescence spot of same color in same position, wherein, described developping agent is cyclohexane-ethyl acetate-glacial acetic acid, and its volume ratio is 5 ~ 8:5:0.1.
2. the discrimination method of field pennycress medicinal material according to claim 1, is characterized in that:
1), need testing solution preparation
Get field pennycress medicinal powder 1 ~ 4g, add a kind of C
1 ~ 4monohydroxy alcohol 50ml, after fully dissolving, filters, gets filtrate as need testing solution;
2), reference substance solution preparation
Get field pennycress standard medicinal material product in contrast, add the C identical with step 1)
1 ~ 4monohydroxy alcohol 50ml, after fully dissolving, filters, gets filtrate 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 respectively on same silica gel g thin-layer plate, with volume ratio be the cyclohexane-ethyl acetate-glacial acetic acid of 5 ~ 8:5:0.1 for developping agent, launch, take out, inspect under putting 365nm uviol lamp; In test sample chromatogram, on the position corresponding to reference substance chromatogram, the blue-fluorescence spot of aobvious same color.
3. the discrimination method of field pennycress medicinal material according to claim 2, is characterized in that, in described abundant dissolving step, solution being placed in ultrasound wave and processing 30min.
4. the discrimination method of field pennycress medicinal material according to claim 1 and 2, is characterized in that the volume ratio of described developping agent cyclohexane-ethyl acetate-glacial acetic acid is 5:5:0.1.
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Effective date of registration: 20160706 Address after: 038300 hi tech Industrial Zone, Huairen County, Shanxi, Shuozhou Patentee after: Shanxi Huayuan Pharmaceutical Biotechnology Co., Ltd. Address before: 030001, No. 1, unit 1, building 26, 5 Xiguan Street, Yingze District, Shanxi, Taiyuan Patentee before: Wang Zhimin |