CN101690748A - Identification method of traditional Chinese medicine Shenfu cardiotonic pill - Google Patents
Identification method of traditional Chinese medicine Shenfu cardiotonic pill Download PDFInfo
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Abstract
The invention relates to an identification method of traditional Chinese medicine Shenfu cardiotonic pills, which comprises the following steps of microscopically identifying Shenfu cardiotonic pill, and identifying ginseng, rhubarb and white mulberry root-bark in Shenfu cardiotonic pills. In the ginseng identification step of the identification method, the time for heating and refluxing in water bath is shortened from 1h to 30min; the developing solvent in the identification step of rhubarb in Shenfu cardiotonic pills is replaced with benzene-acetic ether-formic acid from petroleum ether-ethyl formate-formic acid; and the steps of white mulberry root-bark identification and aconitine checking are added. The method has simple operation, can ensure the safety of usage, shorten identification time, increase identification efficiency, and can rapidly and accurately identify the traditional Chinese medicine Shenfu cardiotonic pills.
Description
Technical field
The invention belongs to the field of Chinese medicines, especially a kind of discrimination method of Chinese medicine Shenfu cardiotonic pill.
Background technology
Shenfu cardiotonic pill is cut out by the yellow Pelleting of the own green pepper Li of the shenfu decoction of " married woman's good recipe " and " Medical Treasures of the Golden Chamber ", produces through Ministry of Public Health approval in 1989, and now quality standard records in the Sanitation Ministry medicine standard new drug is become a full member the 6th of standard.Shenfu cardiotonic pill, is sieved through being ground into fine powder by Radix Ginseng, Radix Aconiti Lateralis Preparata (system), Cortex Mori, Polyporus, Semen Lepidii (Semen Descurainiae), the above Six-element Chinese medicine of Radix Et Rhizoma Rhei, mixing, and every 100g powder adds refined honey 130～150g, makes big honeyed pills, promptly; This product is tan big honeyed pills, sweet, little hardship of distinguishing the flavor of; The discrimination method of prior art Shenfu cardiotonic pill is: " (1) gets this product, puts microscopically and observes: mycelia bonds agglomerating or is dispersed in, and is colourless mostly; Prism of calcium oxalate regular octahedron shape, diameter 32～60 μ m; Fiber is colourless, and is how cataclasm, diameter 13～31 μ m, and wall thickness, cell is linear, stone cell yellow or yellowish-brown, similar round, Long Circle or class polygon, diameter 24～52 μ m; Plant subcutaneous chrotoplast yellow, polygon or long polygon, wall is thick slightly; Calcium oxalate cluster crystal is big, diameter 60～140 μ m; (2) get this product 4 balls, add kieselguhr 10g, grind well, add chloroform 50ml, put in the water-bath reflux 1 hour, filter, discard filtrate, residue adds methanol 80ml, puts in the water-bath reflux 1 hour, filter, filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, add neutral alumina post (100～120 orders that fill in advance, 15g, internal diameter 10～15mm) tops are with methanol solution (4 → 10) 150ml eluting, collect eluent, evaporate to dryness, residue add water 30ml makes dissolving, extracts 2 times with water saturated butanol solution, each 25ml, merge extractive liquid,, with 2% sodium hydroxide solution 25ml washing once, reuse is washed to neutrality; Get n-butanol layer, evaporate to dryness, residue add methanol 0.5ml makes dissolving, as need testing solution; Other gets ginsenoside Rb1 ReRg1, adds methanol and makes the mixed solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography (57 pages of appendix of Chinese Pharmacopoeia nineteen ninety version), draw each 1～2 μ l of above-mentioned two kinds of solution, put respectively on same high-efficient silica gel G lamellae, with chloroform-ethyl acetate-formic acid-water (15: 40: 21: 10) be developing solvent, launch, take out, dry, spray is with ethanol solution of sulfuric acid (1 → 10), 105 ℃ of bakings 3～5 minutes; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; Put under the ultra-violet lamp (365nm) and inspect, show identical fluorescence speckle; (3) get this product 1g, add methanol 20ml, soaked 10 minutes, grind diffusingly, supersound extraction 15 minutes filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml, put in the water-bath heating 30 minutes, put coldly, add diethyl ether and extract twice, each 10ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (57 pages of appendix of Chinese Pharmacopoeia nineteen ninety version), draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same high-efficient silica gel G lamellae, with benzene-ethyl acetate-formic acid (10: 1: 0.1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on show identical orange-yellow fluorescence speckle; Put in the ammonia smoked after, speckle becomes redness." in the above-mentioned discrimination method, differentiate that required time is longer, identification efficiency is lower, and for example: 1. the fibrous tissue feature of Cortex Mori more obviously can be replenished without its stone cell feature; 2. reflux 1 hour in the water-bath in the step (2), overlong time has influenced the efficient of differentiating; 3. the developing solvent effect in the step (3) is relatively poor, differentiates that required time is longer; In addition, also one of important indicator of differentiating at the discrimination process mesaconitine, not record in the prior art.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of discrimination method of Chinese medicine Shenfu cardiotonic pill is provided, this discrimination method has shortened the time of differentiating, has improved the efficient of differentiating, and is simple to operate, can differentiate the Chinese medicine Shenfu cardiotonic pill quickly and accurately.
The present invention is achieved through the following technical solutions:
Advantage of the present invention and beneficial effect are:
1. the fibrous tissue feature of Cortex Mori is more obvious in this discrimination method, has deleted in the prior art stone cell feature and has replenished, and is convenient to observe and differentiates, improves identification efficiency.
2. this discrimination method shortened to 30 minutes to the time of reflux in the water-bath in the Radix Ginseng discriminating step by 1 hour, had improved speed of experiment when guaranteeing to differentiate quality, had shortened the time of differentiating.
3. this discrimination method differentiates that to the Radix Et Rhizoma Rhei in the Shenfu cardiotonic pill developing solvent in the step replaces with petroleum ether-Ethyl formate-formic acid by benzene-ethyl acetate of the prior art-formic acid, and it is better to launch effect, has improved identification efficiency.
4. increase Cortex Mori in this discrimination method and differentiated step, ensured the accuracy of identification result, improved the safety in using.
5. increase aconitine in this discrimination method and checked step, guaranteed the safety that this product is used.
6. the present invention is simple to operate, has shortened the time of differentiating, has improved the efficient of differentiating, can differentiate the Chinese medicine Shenfu cardiotonic pill quickly and accurately.
Description of drawings
Fig. 1 is that the microscopically of Polyporus mycelia in the Chinese medicine Shenfu cardiotonic pill is observed figure;
Fig. 2 is that the microscopically of Chinese medicine Shenfu cardiotonic pill mesoxalic acid calcium prismatic crystal is observed figure;
Fig. 3 is that the microscopically of Cortex Mori fiber in the Chinese medicine Shenfu cardiotonic pill is observed figure;
Fig. 4 is that the microscopically of Cortex Mori stone cell in the Chinese medicine Shenfu cardiotonic pill is observed figure;
Fig. 5 is that the microscopically of Semen Lepidii (Semen Descurainiae) kind Intradermal epidermis cell in the Chinese medicine Shenfu cardiotonic pill is observed figure;
Fig. 6 is that the microscopically of Radix Et Rhizoma Rhei calcium oxalate cluster crystal in the Chinese medicine Shenfu cardiotonic pill is observed figure;
Fig. 7 and Fig. 8, these two parts of accompanying drawings are the chromatogram (wherein Fig. 7 develops the color under the 365nm uviol lamp at daylight and Fig. 8) of sample (lot number 2008001), sample (lot number 2008002), sample (lot number E508003), sample (lot number 5080001), sample (lot number 5080002), sample (lot number 5080003), ginsenoside Rb1, Re, Rg1 reference substance (middle inspection institute) (merk plate) from left to right;
Fig. 9, Figure 10, these two parts of accompanying drawings are the chromatogram (wherein Fig. 9 develops the color under the 365nm uviol lamp at daylight and Figure 10) of negative sample, sample (lot number 2008001), sample (lot number 2008002), sample (lot number E508003), sample (lot number 5080001), sample (lot number 5080002), sample (lot number 5080003), Radix Et Rhizoma Rhei control medicinal material (middle inspection institute) from left to right;
Figure 11, Figure 12, these two parts of accompanying drawings are the chromatogram of negative sample, sample (lot number 2008001), sample (lot number 2008002), sample (lot number E508003), sample (lot number 5080001), sample (lot number 5080002), sample (lot number 5080003), Cortex Mori control medicinal material (middle inspection institute) from left to right, 19.2 ℃ of room temperatures, humidity 22%, wherein Figure 11 is that Merk plate, Figure 12 are the Yantai plate;
Figure 13 is from left to right: the chromatogram (Yantai plate) of negative sample, sample (lot number 2008001), sample (lot number 2008002), sample (lot number E508003), Cortex Mori control medicinal material (middle inspection institute), 9 ℃ of low temperature;
Figure 14 is from left to right: the chromatogram (Yantai plate) of negative sample, sample (lot number 2008001), sample (lot number 2008002), sample (lot number E508003), Cortex Mori control medicinal material (middle inspection institute), high humidity 74%;
Figure 15 is from left to right: negative sample, the chromatogram of sample (lot number 2008001), sample (lot number 2008002), sample (lot number E508003), sample (lot number 5080001), sample (lot number 5080002), sample (lot number 5080003), aconitine reference substance 2 μ g, 0.2 μ g, 0.5 μ g, 1 μ g, 2 μ g, 4 μ g, 6 μ g.
The specific embodiment
The present invention is described in further detail by following examples.Need to prove: following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1
A kind of discrimination method of Chinese medicine Shenfu cardiotonic pill comprises microscopical identification to Shenfu cardiotonic pill, the Radix Ginseng in the Shenfu cardiotonic pill is differentiated, the Radix Et Rhizoma Rhei in the Shenfu cardiotonic pill is differentiated, the Cortex Mori in the Shenfu cardiotonic pill is differentiated.Wherein the microscopical identification step to Shenfu cardiotonic pill is as follows:
Get Shenfu cardiotonic pill and put the microscopically observation:
Cortex Mori: fiber is colourless, and is how cataclasm, diameter 13 μ m, and wall thickness, cell is linear;
Polyporus: mycelia is cohered agglomerating, and is colourless mostly; Prism of calcium oxalate regular octahedron shape, diameter 32 μ m;
Semen Lepidii (Semen Descurainiae): plant Intradermal epidermis cell yellow, polygon or long polygon, wall is thick slightly;
Radix Et Rhizoma Rhei: calcium oxalate cluster crystal is big, diameter 60 μ m.
Wherein the Radix Ginseng in the Shenfu cardiotonic pill is differentiated that step is as follows:
The preparation of need testing solution: get Shenfu cardiotonic pill 4 balls, add kieselguhr 10g, grind well, add chloroform 50ml, reflux 30 minutes filters, discard filtrate, residue adds methanol 80ml, reflux 30 minutes, filter, filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, put neutral alumina post 100 orders, 15g is on the internal diameter 10mm, with 40% methanol 150ml eluting, collect eluent, evaporate to dryness, residue add water 30ml makes dissolving, with water saturated n-butanol extraction 2 times, each 25ml merges n-butyl alcohol liquid, washs with 2% sodium hydroxide solution 25ml, discard sodium hydroxide solution, n-butyl alcohol liquid reuse is washed to neutrality, divides and gets n-butanol layer, evaporate to dryness, residue adds methanol 0.5ml makes dissolving, as need testing solution.
The preparation of reference substance solution: get ginsenoside Rb1's reference substance, ginsenoside Re's reference substance, ginsenoside Rg1's reference substance, add methanol and make the mixed solution that every 1ml contains 1mg, in contrast product solution;
The employing thin layer chromatography is differentiated: adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, draw each 2 μ l of need testing solution and reference substance solution, put respectively on same high-efficient silica gel G lamellae, with chloroform-ethyl acetate-formic acid-water (15: 40: 21: 10) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; Put under the ultra-violet lamp (365nm) and inspect, show the fluorescence speckle of same color.
Wherein the Radix Et Rhizoma Rhei in the Shenfu cardiotonic pill is differentiated that step is as follows:
The preparation of need testing solution: get Shenfu cardiotonic pill 2.5g, shred, add methanol 20ml, soaked 10 minutes, supersound process 15 minutes filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml, put in the water-bath heating 30 minutes, put cold, with ether extraction 2 times, each 10ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.
The preparation of control medicinal material solution: get Radix Et Rhizoma Rhei control medicinal material 0.1g, shine medical material solution in pairs with legal system;
The employing thin layer chromatography is differentiated: adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, each 2 μ l of need testing solution and control medicinal material solution in the absorption, put respectively on same high-efficient silica gel G lamellae, upper solution with 30 ℃-Ethyl formate-formic acid of petroleum ether (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical orange-yellow fluorescence speckle; Put in the ammonia steam smoked after, speckle becomes redness.
Wherein the Cortex Mori in the Shenfu cardiotonic pill is differentiated that step is as follows:
The preparation of need testing solution: get Shenfu cardiotonic pill 3 balls, shred, add saturated sodium carbonate liquor 30ml, supersound process 30 minutes, filter, get filtrate or supernatant and add dilute hydrochloric acid adjusting pH value to 1, left standstill 30 minutes, extract 2 times with the ethyl acetate jolting, each 30ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.
The preparation of control medicinal material solution: get Cortex Mori control medicinal material 2g, add saturated sodium carbonate liquor 15ml, supersound process 30 minutes filters, get filtrate or supernatant and add dilute hydrochloric acid adjusting pH value to 1, left standstill 30 minutes, and extracted 2 times, each 15ml with the ethyl acetate jolting, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.
The employing thin layer chromatography is differentiated: adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, each 5～10 μ l of need testing solution and control medicinal material solution in the absorption, put respectively on same high-efficient silica gel G lamellae, with 60 ℃-ethyl acetate of petroleum ether (6: 4) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
Wherein this discrimination method comprises that also aconitine inspection step is as follows:
The preparation of need testing solution: it is an amount of to get Shenfu cardiotonic pill, shreds, and gets 14g, the accurate title, decide, and it is an amount of to add kieselguhr, grinds well, add ammonia solution 10ml, carefully mix thoroughly, placed 2 hours, the 100ml that adds diethyl ether again, supersound process 5 minutes left standstill 24 hours, divide and get ether solution, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution;
The preparation of reference substance solution: it is an amount of to get the aconitine reference substance, and accurate the title decides, and adds dehydrated alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution;
The employing thin layer chromatography is differentiated: adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, accurate need testing solution 16 μ l, the reference substance solution 2 μ l of drawing, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-diethylamine (14: 4: 1) is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution and sodium nitrite ethanol test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on the speckle that occurs should or speckle appear less than the speckle of reference substance.
Embodiment 2
A kind of discrimination method of Chinese medicine Shenfu cardiotonic pill, its method comprises the microscopical identification to Shenfu cardiotonic pill, and the Radix Ginseng in the Shenfu cardiotonic pill is differentiated, the Radix Et Rhizoma Rhei in the Shenfu cardiotonic pill is differentiated, Cortex Mori in the Shenfu cardiotonic pill is differentiated that wherein the microscopical identification step to Shenfu cardiotonic pill is as follows:
Get Shenfu cardiotonic pill and put the microscopically observation:
Cortex Mori: fiber is colourless, and is how cataclasm, diameter 26 μ m, and wall thickness, cell is linear;
Polyporus: mycelia is cohered agglomerating, and is colourless mostly; Prism of calcium oxalate regular octahedron shape, diameter 60 μ m;
Semen Lepidii (Semen Descurainiae): plant Intradermal epidermis cell yellow, polygon or long polygon, wall is thick slightly;
Radix Et Rhizoma Rhei: calcium oxalate cluster crystal is big, diameter 140 μ m.
Wherein the Radix Ginseng in the Shenfu cardiotonic pill is differentiated that step is as follows:
The preparation of need testing solution: get Shenfu cardiotonic pill 4 balls, add kieselguhr 10g, grind well, add chloroform 50ml, reflux 30 minutes filters, discard filtrate, residue adds methanol 80ml, reflux 30 minutes, filter, filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, put neutral alumina post 120 orders, 15g is on the internal diameter 15mm, with 40% methanol 150ml eluting, collect eluent, evaporate to dryness, residue add water 30ml makes dissolving, with water saturated n-butanol extraction 2 times, each 25ml merges n-butyl alcohol liquid, washs with 2% sodium hydroxide solution 25ml, discard sodium hydroxide solution, n-butyl alcohol liquid reuse is washed to neutrality, divides and gets n-butanol layer, evaporate to dryness, residue adds methanol 0.5ml makes dissolving, as need testing solution.
The preparation of reference substance solution: get ginsenoside Rb1's reference substance, ginsenoside Re's reference substance, ginsenoside Rg1's reference substance, add methanol and make the mixed solution that every 1ml contains 1mg, in contrast product solution.
The employing thin layer chromatography is differentiated: adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, draw each 2～5 μ l of need testing solution and reference substance solution, put respectively on same high-efficient silica gel G lamellae, with chloroform-ethyl acetate-formic acid-water (15: 40: 21: 10) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; Put under the ultra-violet lamp (365nm) and inspect, show the fluorescence speckle of same color.
Described as follows to the discriminating of the Radix Et Rhizoma Rhei in Shenfu cardiotonic pill step:
The preparation of need testing solution: get Shenfu cardiotonic pill 2.5g, shred, add methanol 20ml, soaked 10 minutes, supersound process 15 minutes filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml, put in the water-bath heating 30 minutes, put cold, with ether extraction 2 times, each 10ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.
The preparation of control medicinal material solution: get Radix Et Rhizoma Rhei control medicinal material 0.1g, shine medical material solution in pairs with legal system;
The employing thin layer chromatography is differentiated: adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, each 2 μ l of need testing solution and control medicinal material solution in the absorption, put respectively on same high-efficient silica gel G lamellae, upper solution with 60 ℃-Ethyl formate-formic acid of petroleum ether (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical orange-yellow fluorescence speckle; Put in the ammonia steam smoked after, speckle becomes redness.
Described as follows to the discriminating of the Cortex Mori in Shenfu cardiotonic pill step:
The preparation of need testing solution: get Shenfu cardiotonic pill 3 balls, shred, add saturated sodium carbonate liquor 30ml, supersound process 30 minutes, filter, get filtrate or supernatant and add dilute hydrochloric acid adjusting pH value to 2, left standstill 30 minutes, extract 2 times with the ethyl acetate jolting, each 30ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.
The preparation of control medicinal material solution: get Cortex Mori control medicinal material 2g, add saturated sodium carbonate liquor 15ml, supersound process 30 minutes filters, get filtrate or supernatant and add dilute hydrochloric acid adjusting pH value to 2, left standstill 30 minutes, and extracted 2 times, each 15ml with the ethyl acetate jolting, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.
The employing thin layer chromatography is differentiated: adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, each 10 μ l of need testing solution and control medicinal material solution in the absorption, put respectively on same high-efficient silica gel G lamellae, with 90 ℃-ethyl acetate of petroleum ether (6: 4) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
Described discrimination method comprises that also aconitine inspection step is as follows:
The preparation of need testing solution: it is an amount of to get Shenfu cardiotonic pill, shreds, and gets 14g, the accurate title, decide, and it is an amount of to add kieselguhr, grinds well, add ammonia solution 10ml, carefully mix thoroughly, placed 2 hours, the 100ml that adds diethyl ether again, supersound process 5 minutes left standstill 24 hours, divide and get ether solution, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution.
The preparation of reference substance solution: it is an amount of to get the aconitine reference substance, and accurate the title decides, and adds dehydrated alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution.
The employing thin layer chromatography is differentiated: adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, accurate need testing solution 16 μ l, the reference substance solution 2 μ l of drawing, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-diethylamine (14: 4: 1) is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution and sodium nitrite ethanol test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on the speckle that occurs should or speckle appear less than the speckle of reference substance.
Below in conjunction with accompanying drawing the present invention is described further again:
Get this Chinese medicine preparation, put microscopically and observe: fiber is colourless, and is how cataclasm, diameter 13～26 μ m, wall thickness, cell linear (Cortex Mori).Mycelia is cohered agglomerating, and is colourless mostly; Prism of calcium oxalate regular octahedron shape, diameter 32～60 μ m (Polyporus).Plant Intradermal epidermis cell yellow, polygon or long polygon, wall thick slightly (Semen Lepidii (Semen Descurainiae)).Calcium oxalate cluster crystal is big, and diameter 60～140 μ m (Radix Et Rhizoma Rhei) the results are shown in Figure 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6.
Adopting thin layer chromatography, is reference substance with ginsenoside Rb1, Re, Rg1, differentiates Radix Ginseng in this Chinese medicine preparation.Through check, in the test sample chromatograph, with ginsenoside Rb1, Re, the corresponding position of Rg1 reference substance chromatograph on, all show the speckle of same color, 6 batch samples are all up to specification.The results are shown in Figure 7, Fig. 8.
Adopting thin layer chromatography, is control medicinal material with the Radix Et Rhizoma Rhei, differentiates Radix Et Rhizoma Rhei in this Chinese medicine preparation.Through check, in the test sample chromatograph, with the corresponding position of Radix Et Rhizoma Rhei control medicinal material chromatograph on, all show the speckle of same color, 6 batch samples are all up to specification.The results are shown in Figure 9, Figure 10.
Adopting thin layer chromatography, is control medicinal material with the Cortex Mori, differentiates Cortex Mori in this Chinese medicine preparation.Through check, in the test sample chromatograph, with the corresponding position of Cortex Mori control medicinal material chromatograph on, show the speckle of same color, negative sample is noiseless, the results are shown in Figure 11.In addition this method has been carried out serviceability test, comprised different lamellaes (Merk plate and Yantai plate), low temperature and high humidity environment are investigated Figure 12, Figure 13, Figure 14 as a result to the influence of separation case.The above-mentioned different condition of result does not have influence to this test.
Adopting thin layer chromatography, is reference substance with the aconitine, formulates Radix Aconiti Lateralis Preparata aconitine limit inspection technique in this Chinese medicine preparation.Radix Aconiti Lateralis Preparata accounts for and makes 5.5% of patent medicine total amount in this preparation, and the need testing solution Radix Aconiti Lateralis Preparata content of making is 0.76g/ml, need testing solution point sample amount 16 μ l, and 2 μ l are suitable with aconitine reference substance solution (1mg/ml) point sample amount.The results are shown in Figure 15 and show, aconitine reference substance point sample amount 1 μ g, the energy display dot is lower than this amount, fails to detect.
Claims (6)
1. the discrimination method of a Chinese medicine Shenfu cardiotonic pill, it is characterized in that: the step of discrimination method is:
(1) to the microscopical identification of Shenfu cardiotonic pill;
(2) Radix Ginseng in the Shenfu cardiotonic pill is differentiated;
(3) Radix Et Rhizoma Rhei in the Shenfu cardiotonic pill is differentiated;
(4) Cortex Mori in the Shenfu cardiotonic pill is differentiated.
2. the discrimination method of Chinese medicine Shenfu cardiotonic pill according to claim 1 is characterized in that: described microscopical identification step to Shenfu cardiotonic pill is as follows:
Get Shenfu cardiotonic pill and put the microscopically observation:
Cortex Mori: fiber is colourless, and is how cataclasm, diameter 13～26 μ m, and wall thickness, cell is linear;
Polyporus: mycelia is cohered agglomerating, and is colourless mostly; Prism of calcium oxalate regular octahedron shape, diameter 32～60 μ m;
Semen Lepidii (Semen Descurainiae): plant Intradermal epidermis cell yellow, polygon or long polygon, wall is thick slightly;
Radix Et Rhizoma Rhei: calcium oxalate cluster crystal is big, diameter 60～140 μ m.
3. the discrimination method of Chinese medicine Shenfu cardiotonic pill according to claim 1 is characterized in that: described as follows to the discriminating of the Radix Ginseng in Shenfu cardiotonic pill step:
(1) preparation of need testing solution: get Shenfu cardiotonic pill 4 balls, add kieselguhr 10g, grind well, add chloroform 50ml, reflux 30 minutes filters, discard filtrate, residue adds methanol 80ml, reflux 30 minutes, filter, filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, put the neutral alumina post (100～120 orders, 15g is on the internal diameter 10～15mm), with 40% methanol 150ml eluting, collect eluent, evaporate to dryness, residue add water 30ml makes dissolving, with water saturated n-butanol extraction 2 times, each 25ml merges n-butyl alcohol liquid, washs with 2% sodium hydroxide solution 25ml, discard sodium hydroxide solution, n-butyl alcohol liquid reuse is washed to neutrality, divides and gets n-butanol layer, evaporate to dryness, residue adds methanol 0.5ml makes dissolving, as need testing solution;
(2) preparation of reference substance solution: get ginsenoside Rb1's reference substance, ginsenoside Re's reference substance, ginsenoside Rg1's reference substance, add methanol and make the mixed solution that every 1ml contains 1mg, in contrast product solution;
(3) adopt thin layer chromatography to differentiate: to adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, draw each 2～5 μ l of need testing solution and reference substance solution, put respectively on same high-efficient silica gel G lamellae, with chloroform-ethyl acetate-formic acid-water (15: 40: 21: 10) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; Put under the ultra-violet lamp (365nm) and inspect, show the fluorescence speckle of same color.
4. the discrimination method of Chinese medicine Shenfu cardiotonic pill according to claim 1 is characterized in that: described as follows to the discriminating of the Radix Et Rhizoma Rhei in Shenfu cardiotonic pill step:
(1) preparation of need testing solution: get Shenfu cardiotonic pill 2.5g, shred, add methanol 20ml, soaked 10 minutes, supersound process 15 minutes filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml, put in the water-bath heating 30 minutes, put cold, with ether extraction 2 times, each 10ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution;
(2) preparation of control medicinal material solution: get Radix Et Rhizoma Rhei control medicinal material 0.1g, shine medical material solution in pairs with legal system;
(3) adopt thin layer chromatography to differentiate: to adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, each 2 μ l of need testing solution and control medicinal material solution in the absorption, put respectively on same high-efficient silica gel G lamellae, upper solution with petroleum ether (30～60 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical orange-yellow fluorescence speckle; Put in the ammonia steam smoked after, speckle becomes redness.
5. the discrimination method of Chinese medicine Shenfu cardiotonic pill according to claim 1 is characterized in that: described as follows to the discriminating of the Cortex Mori in Shenfu cardiotonic pill step:
(1) preparation of need testing solution: get Shenfu cardiotonic pill 3 balls, shred, add saturated sodium carbonate liquor 30ml, supersound process 30 minutes, filter, get filtrate or supernatant and add dilute hydrochloric acid adjusting pH value to 1～2, left standstill 30 minutes, extract 2 times with the ethyl acetate jolting, each 30ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution;
(2) preparation of control medicinal material solution: get Cortex Mori control medicinal material 2g, add saturated sodium carbonate liquor 15ml, supersound process 30 minutes filters, get filtrate or supernatant and add dilute hydrochloric acid adjusting pH value to 1～2, left standstill 30 minutes, and extracted 2 times, each 15ml with the ethyl acetate jolting, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution;
(3) adopt thin layer chromatography to differentiate: to adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, each 5～10 μ l of need testing solution and control medicinal material solution in the absorption, put respectively on same high-efficient silica gel G lamellae, with petroleum ether (60～90 ℃)-ethyl acetate (6: 4) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
6. the discrimination method of Chinese medicine Shenfu cardiotonic pill according to claim 1 is characterized in that: described discrimination method comprises that also aconitine inspection step is as follows:
(1) preparation of need testing solution: it is an amount of to get Shenfu cardiotonic pill, shreds, and gets 14g, the accurate title, decide, and it is an amount of to add kieselguhr, grinds well, add ammonia solution 10ml, carefully mix thoroughly, placed 2 hours, the 100ml that adds diethyl ether again, supersound process 5 minutes left standstill 24 hours, divide and get ether solution, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution;
(2) preparation of reference substance solution: it is an amount of to get the aconitine reference substance, and accurate the title decides, and adds dehydrated alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution;
(3) adopt thin layer chromatography to differentiate: to adopt thin layer chromatography according to " appendix a VI of Chinese pharmacopoeia version in 2005 B test, accurate need testing solution 16 μ l, the reference substance solution 2 μ l of drawing, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-diethylamine (14: 4: 1) is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution and sodium nitrite ethanol test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on the speckle that occurs should or speckle appear less than the speckle of reference substance.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102707010A (en) * | 2012-06-29 | 2012-10-03 | 天津中新药业集团股份有限公司达仁堂制药厂 | Quality detection method of Chinese medicinal preparation fetal lie pill |
| CN102759600A (en) * | 2012-08-06 | 2012-10-31 | 四川逢春制药有限公司 | Detection method of sufi cough syrup |
| CN106324161A (en) * | 2016-10-24 | 2017-01-11 | 广州康臣药物研究有限公司 | Quality detection method for traditional Chinese medicine composition capable of treating diabetic nephropathy |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102707010A (en) * | 2012-06-29 | 2012-10-03 | 天津中新药业集团股份有限公司达仁堂制药厂 | Quality detection method of Chinese medicinal preparation fetal lie pill |
| CN102707010B (en) * | 2012-06-29 | 2014-03-26 | 天津中新药业集团股份有限公司达仁堂制药厂 | Quality detection method of Chinese medicinal preparation fetal lie pill |
| CN102759600A (en) * | 2012-08-06 | 2012-10-31 | 四川逢春制药有限公司 | Detection method of sufi cough syrup |
| CN106324161A (en) * | 2016-10-24 | 2017-01-11 | 广州康臣药物研究有限公司 | Quality detection method for traditional Chinese medicine composition capable of treating diabetic nephropathy |
| CN106324161B (en) * | 2016-10-24 | 2017-11-14 | 广州康臣药物研究有限公司 | Treat the quality determining method of the Chinese medicine composition of diabetic nephropathy |
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Application publication date: 20100407 |