CN103954725A - Detection method of aporosa dioica granules - Google Patents
Detection method of aporosa dioica granules Download PDFInfo
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Abstract
The invention relates to a detection method of aporosa dioica granules. The detection method comprises phenotypic traits, identification and detection items, wherein identification comprises the thin-layer identification of menthol, the thin-layer identification of honeysuckle stem, the thin-layer identification of radix bupleuri and the thin-layer identification of bupleurum longiradiatum; as no perfect detection method is developed for detecting active ingredients of the aporosa dioica granules at present, phenomena that related raw materials are not added enough or is not added and fake bupleurum longiradiatum is mixed by illegal manufacturers happen. The detection method is a scientific, reasonable, feasible identification method, the clinical effects of the aporosa dioica granules can be ensured, the medicinal materials have specific quality indexes, the usage of honeysuckle stem, mentha haplocalyx and radix bupleuri in the aporosa dioica granules can be ensured, and therefore, the curative effect of the drug is ensured; besides, the fake bupleurum longiradiatum can be effectively detected, and the harm of radix bupleuri toxins and acetyl radix bupleuri toxins in the bupleurum longiradiatum to the health of patient is avoided.
Description
Technical field:
The present invention relates to a kind of detection method of Yinchai Granules.
Background technology:
Yinchai Granules is the 13 kind of recording of " the Sanitation Ministry medicine standard " Traditional Chinese medicine historical preparation, standard number is WS3-B-2612-97, prescription is caulis lonicerae, reed rhizome, peppermint, radix bupleuri, loguat leaf, it is the granule of pure Chinese medicine, it has heat-clearing, induce sweat, the effect of cough-relieving, being used for the treatment of clinically the disease such as anemopyretic cold, fever and cough, is the common drug that is used for the treatment of in the market the disease such as anemopyretic cold, fever and cough.But up to the present, also do not have a set of perfect detection method to detect accordingly its effective ingredient, may cause so illegal manufacturer not prepared burden in strict accordance with the dosage of writing out a prescription in the time producing medicine, wantonly reduce the raw material that price is high, cause the curative effect of medicine obviously to decline, affect the safe and effective of medicine, grievous injury patient's interests.On the other hand, the prescription of this medicine derives from recipe in " Treatise on Febrile and Miscellaneous Disease " silver bavin reed rhizome soup, and radix bupleuri large usage quantity in prescription accounts for one of 34 of whole recipe quantity, and its effect is mainly harmonizing Sharyang, strengthening vital QI to eliminate pathogenic factors.Because the use amount of radix bupleuri is in recent years larger, but its output is limited, its adulterant bigleaf thorowax root is also had a mind to or is not intended to sneak into use, in bigleaf thorowax root, contain bupleurotoxin and acetylbupleurotoxin, these two kinds of compositions are all noxious materials, repeatedly there is the poisoning Adverse drug events of medicine that is mixed with bigleaf thorowax root because taking, so it is necessary to control bigleaf thorowax root." Shandong medical industry " delivered " to supplementing of the Chinese Pharmacopoeia version radix bupleuri method of inspection in 2000 " literary composition in the 22 the 5th phase of volume in 2003, inquired into the discriminating control problem of bigleaf thorowax root medicinal material in pharmacopeia, but its method has obvious deficiency, in literary composition, disclose and place 24 hours, its detection time is oversize, is unfavorable for drug production process control and drug quality supervision and check; Bupleurotoxin and acetylbupleurotoxin content are relatively low, and point sample is 2 μ l only, and point sample amount is very few, the accuracy of impact inspection; Bupleurotoxin and acetylbupleurotoxin content are relatively low, under uviol lamp, inspect, observe without chromogenic reagent, observing effect is bad, main is many, the contained complicateds of Yinchai Granules prescription flavour of a drug, other composition can produce to be obscured and disturbs, so finding a kind of better way, to control sneaking into of bigleaf thorowax root be the task of top priority.
Summary of the invention:
Object of the present invention, be to provide a kind of detection method of Yinchai Granules, can effectively monitor illegal manufacturer and throw less or do not throw corresponding raw material, monitor sneaking into of adulterant bigleaf thorowax root simultaneously, prevent from taking the generation of rear poisoning Adverse drug events, make this drug safety effective, and ensured the clinical efficacy of Yinchai Granules.
Technical scheme of the present invention is such:
The prescription of this Yinchai Granules is: caulis lonicerae 300g, reed rhizome 300g, peppermint 100g, radix bupleuri 300g, loguat leaf 200g.
The detection method of this Yinchai Granules, comprises proterties, discriminating, inspection item; Wherein, differentiate the discriminating of bupleurotoxin and acetylbupleurotoxin in the discriminating, bigleaf thorowax root of the discriminating, the radix bupleuri that comprise discriminating to the menthol in peppermint medicinal material, caulis lonicerae.
The discriminating of the menthol of peppermint medicinal material: taking menthol as reference substance, taking benzene-ethyl acetate as developping agent, differentiate by thin-layered chromatography;
The discriminating of caulis lonicerae: taking caulis lonicerae control medicinal material as contrast, taking butyl acetate-formic acid-water as developping agent, differentiate by thin-layered chromatography;
The discriminating of radix bupleuri: taking radix bupleuri control medicinal material as contrast, taking ethyl acetate, alcohol and water as developping agent, differentiate by thin-layered chromatography;
The discriminating of bupleurotoxin and acetylbupleurotoxin: taking bupleurotoxin, acetylbupleurotoxin as reference substance, taking normal hexane-ethyl acetate as developping agent, differentiate by thin-layered chromatography;
Detection method is as follows:
(1) discriminating of menthol
Get this product 12g, add 60～90 DEG C of sherwood oil 30ml, close plug, ultrasonic processing 30 minutes, filter, filtrate is as need testing solution, separately get menthol reference substance, add 60～90 DEG C of sherwood oils and make the solution of every 1ml containing 2mg, product solution in contrast, test according to thin-layered chromatography, draw need testing solution 10～20 μ l, reference substance solution 10 μ l, put respectively on same silica gel g thin-layer plate, taking benzene: ethyl acetate=17～21:0.8～1.2 are as developping agent, launch, take out, dry, spray is with the mixed solution of 2% vanillic aldehyde sulfuric acid solution: ethanol=1:4, dry 5～10 minutes at 100 DEG C, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(2) discriminating of caulis lonicerae
Get this product 3g, porphyrize, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, as need testing solution, separately get caulis lonicerae control medicinal material 3g, be ground into meal, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, medicinal material solution in contrast, test according to thin-layer chromatography, draw need testing solution and each 5～10 μ l of control medicinal material solution, put respectively on same silica gel H thin layer plate, taking butyl acetate: formic acid: the upper solution of water=8～12:4～6:3.5～4.5 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of radix bupleuri
Get this product 6g, 20ml adds water, be stirred to dissolve, centrifugal, get supernatant, add polyamide column a, water respectively, the each 100ml wash-out of 20% ethanol and 50% ethanol, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get radix bupleuri control medicinal material 1g, add water appropriate, decoct 1.5 hours, filter, filtrate is concentrated into 10ml, add polyamide column b, water 100ml and 50% ethanol 150ml wash-out respectively, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw need testing solution 2～10ul and control medicinal material solution 2ul, put respectively on same silica gel g thin-layer plate, taking ethyl acetate: ethanol: water=10～14:1.8～2.2:0.9～1.1 are as developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot colour developing, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of bigleaf thorowax root:
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make every 1ml containing bupleurotoxin, the solution of the each 1mg of acetylbupleurotoxin reference substance, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=7～9:0.8～1.2 are as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, must not show the spot of same color.
Detection method is as follows more specifically:
(1) discriminating of menthol
Get this product 12g, add 60～90 DEG C of sherwood oil 30ml, close plug, ultrasonic processing 30 minutes, filter, filtrate is as need testing solution, separately get menthol reference substance, add 60～90 DEG C of sherwood oils and make the solution of every 1ml containing 2mg, product solution in contrast, test according to thin-layered chromatography, draw need testing solution 10～20 μ l, reference substance solution 10 μ l, put respectively on same silica gel g thin-layer plate, taking benzene: ethyl acetate=19:1 as developping agent, launch, take out, dry, spray is with the mixed solution of 2% vanillic aldehyde sulfuric acid solution: ethanol=1:4, dry 5～10 minutes at 100 DEG C, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(2) discriminating of caulis lonicerae
Get this product 3g, porphyrize, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, as need testing solution, separately get caulis lonicerae control medicinal material 3g, be ground into meal, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, medicinal material solution in contrast, test according to thin-layer chromatography, draw need testing solution and each 5～10 μ l of control medicinal material solution, put respectively on same silica gel H thin layer plate, taking butyl acetate: the upper solution of formic acid: water=10:5:4 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of radix bupleuri
Get this product 6g, 20ml adds water, be stirred to dissolve, centrifugal, get supernatant, add polyamide column a, water respectively, the each 100ml wash-out of 20% ethanol and 50% ethanol, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get radix bupleuri control medicinal material 1g, add water appropriate, decoct 1.5 hours, filter, filtrate is concentrated into 10ml, add polyamide column b, water 100ml and 50% ethanol 150ml wash-out respectively, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw need testing solution 2～10ul and control medicinal material solution 2ul, put respectively on same silica gel g thin-layer plate, taking ethyl acetate: ethanol: water=12:2:1 is as developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot colour developing, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of bigleaf thorowax root:
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make every 1ml containing bupleurotoxin, the solution of the each 1mg of acetylbupleurotoxin reference substance, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=8:1 as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, must not show the spot of same color.
Described polyamide column a is that polyamide is crossed 100～200 mesh sieves, takes the polyamide 8g after sieving, and selects the chromatographic column that internal diameter is 2.5～3cm, wet method dress post.
Described polyamide column b is that polyamide is crossed 100～200 orders, takes the polyamide 4g after sieving, and selects the chromatographic column that internal diameter is 2cm, wet method dress post.
Proterties: this product is tan particle; Gas perfume (or spice), taste is micro-sweet, slightly bitter.
Check: should meet every regulation relevant under granule item (annex I C of " Chinese Pharmacopoeia " version in 2010).
The ratio of developping agent of the present invention is in volume ratio.
Technique effect of the present invention:
The present invention is by the discriminating to menthol in Yinchai Granules, the discriminating of caulis lonicerae, the discriminating of radix bupleuri, the discriminating of bigleaf thorowax root, allow several medicinal materials have clear and definite quality index, guarantee the use of caulis lonicerae, peppermint, radix bupleuri in Yinchai Granules, thereby ensured the curative effect of medicine; On the other hand, the adulterant bigleaf thorowax root of radix bupleuri also can effectively detect, and has avoided these two kinds of toxic substances harm patients' of the bupleurotoxin that contains in bigleaf thorowax root and acetylbupleurotoxin health.The present invention can monitor the quality of Yinchai Granules better and more comprehensively, and can effectively control illegal manufacturers produce Yinchai Granules of poor quality, thereby has ensured curative effect and the safety of medicine, has ensured patient's interests, and the present invention is scientific and reasonable, practical.
Embodiment:
Embodiment 1:
[prescription] caulis lonicerae 300g reed rhizome 300g peppermint 100g radix bupleuri 300g loguat leaf 200g
[method for making] above five tastes, peppermint is extracted volatile oil, and the another device of aqueous solution after distillation is preserved, the four taste boiling secondaries such as the dregs of a decoction and all the other caulis loniceraes, each 2 hours, collecting decoction, filter, leave standstill, the aqueous solution after getting supernatant and distilling merges, at 50～55 DEG C of temperature, be condensed into relative density and be 1.33～1.36 clear cream, add appropriate cane sugar powder and dextrin, with ethanol particle processed, dry, add peppermint oil, mix, make 650g, to obtain final product.
[proterties] this product is tan particle; Gas perfume (or spice), taste is micro-sweet, slightly bitter.
The discriminating of [discriminating] (1) menthol
Get this product 12g, add 60～90 DEG C of sherwood oil 30ml, close plug, ultrasonic processing 30 minutes, filter, filtrate is as need testing solution, separately get menthol reference substance, add 60～90 DEG C of sherwood oils and make the solution of every 1ml containing 2mg, product solution in contrast, test according to thin-layered chromatography, draw need testing solution 10～20 μ l, reference substance solution 10 μ l, put respectively on same silica gel g thin-layer plate, taking benzene: ethyl acetate=17:0.8 as developping agent, launch, take out, dry, spray is with the mixed solution of 2% vanillic aldehyde sulfuric acid solution: ethanol=1:4, dry 5～10 minutes at 100 DEG C, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(2) discriminating of caulis lonicerae
Get this product 3g, porphyrize, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, as need testing solution, separately get caulis lonicerae control medicinal material 3g, be ground into meal, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, medicinal material solution in contrast, test according to thin-layer chromatography, draw need testing solution and each 5～10 μ l of control medicinal material solution, put respectively on same silica gel H thin layer plate, taking butyl acetate: the upper solution of formic acid: water=8:4:3.5 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of radix bupleuri
Get this product 6g, 20ml adds water, be stirred to dissolve, centrifugal, get supernatant, (polyamide is crossed 100～200 mesh sieves to add polyamide column a, take the polyamide 8g after sieving, select the chromatographic column that internal diameter is 2.5～3cm, wet method dress post), water respectively, the each 100ml wash-out of 20% ethanol and 50% ethanol, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get radix bupleuri control medicinal material 1g, add water appropriate, decoct 1.5 hours, filter, filtrate is concentrated into 10ml, (polyamide is crossed 100～200 orders to add polyamide column b, take the polyamide 4g after sieving, select the chromatographic column that internal diameter is 2cm, wet method dress post), water 100ml and 50% ethanol 150ml wash-out respectively, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw need testing solution 2～10ul and control medicinal material solution 2ul, put respectively on same silica gel g thin-layer plate, taking ethyl acetate: ethanol: water=10:1.8:0.9 is as developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot colour developing, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of bigleaf thorowax root:
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make every 1ml containing bupleurotoxin, the solution of the each 1mg of acetylbupleurotoxin reference substance, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=7:0.8 as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, must not show the spot of same color.
[inspection] should meet every regulation relevant under granule item (annex I C of " Chinese Pharmacopoeia " version in 2010).
Embodiment 2:
[prescription] caulis lonicerae 300g reed rhizome 300g peppermint 100g radix bupleuri 300g loguat leaf 200g
[method for making] above five tastes, peppermint is extracted volatile oil, and the another device of aqueous solution after distillation is preserved, the four taste boiling secondaries such as the dregs of a decoction and all the other caulis loniceraes, each 2 hours, collecting decoction, filter, leave standstill, the aqueous solution after getting supernatant and distilling merges, at 50～55 DEG C of temperature, be condensed into relative density and be 1.33～1.36 clear cream, add appropriate cane sugar powder and dextrin, with ethanol particle processed, dry, add peppermint oil, mix, make 650g, to obtain final product.
[proterties] this product is tan particle; Gas perfume (or spice), taste is micro-sweet, slightly bitter.
The discriminating of [discriminating] (1) menthol
Get this product 12g, add 60～90 DEG C of sherwood oil 30ml, close plug, ultrasonic processing 30 minutes, filter, filtrate is as need testing solution, separately get menthol reference substance, add 60～90 DEG C of sherwood oils and make the solution of every 1ml containing 2mg, product solution in contrast, test according to thin-layered chromatography, draw need testing solution 10～20 μ l, reference substance solution 10 μ l, put respectively on same silica gel g thin-layer plate, taking benzene: ethyl acetate=19:1 as developping agent, launch, take out, dry, spray is with the mixed solution of 2% vanillic aldehyde sulfuric acid solution: ethanol=1:4, dry 5～10 minutes at 100 DEG C, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(2) discriminating of caulis lonicerae
Get this product 3g, porphyrize, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, as need testing solution, separately get caulis lonicerae control medicinal material 3g, be ground into meal, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, medicinal material solution in contrast, test according to thin-layer chromatography, draw need testing solution and each 5～10 μ l of control medicinal material solution, put respectively on same silica gel H thin layer plate, taking butyl acetate: the upper solution of formic acid: water=10:5:4 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of radix bupleuri
Get this product 6g, 20ml adds water, be stirred to dissolve, centrifugal, get supernatant, (polyamide is crossed 100～200 mesh sieves to add polyamide column a, take the polyamide 8g after sieving, select the chromatographic column that internal diameter is 2.5～3cm, wet method dress post), water respectively, the each 100ml wash-out of 20% ethanol and 50% ethanol, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get radix bupleuri control medicinal material 1g, add water appropriate, decoct 1.5 hours, filter, filtrate is concentrated into 10ml, (polyamide is crossed 100～200 orders to add polyamide column b, take the polyamide 4g after sieving, select the chromatographic column that internal diameter is 2cm, wet method dress post), water 100ml and 50% ethanol 150ml wash-out respectively, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw need testing solution 2～10ul and control medicinal material solution 2ul, put respectively on same silica gel g thin-layer plate, taking ethyl acetate: ethanol: water=12:2:1 is as developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot colour developing, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of bigleaf thorowax root:
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make every 1ml containing bupleurotoxin, the solution of the each 1mg of acetylbupleurotoxin reference substance, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=8:1 as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, must not show the spot of same color.
[inspection] should meet every regulation relevant under granule item (annex I C of " Chinese Pharmacopoeia " version in 2010).
Embodiment 3:
[prescription] caulis lonicerae 300g reed rhizome 300g peppermint 100g radix bupleuri 300g loguat leaf 200g
[method for making] above five tastes, peppermint is extracted volatile oil, and the another device of aqueous solution after distillation is preserved, the four taste boiling secondaries such as the dregs of a decoction and all the other caulis loniceraes, each 2 hours, collecting decoction, filter, leave standstill, the aqueous solution after getting supernatant and distilling merges, at 50～55 DEG C of temperature, be condensed into relative density and be 1.33～1.36 clear cream, add appropriate cane sugar powder and dextrin, with ethanol particle processed, dry, add peppermint oil, mix, make 650g, to obtain final product.
[proterties] this product is tan particle; Gas perfume (or spice), taste is micro-sweet, slightly bitter.
The discriminating of [discriminating] (1) menthol
Get this product 12g, add 60～90 DEG C of sherwood oil 30ml, close plug, ultrasonic processing 30 minutes, filter, filtrate is as need testing solution, separately get menthol reference substance, add 60～90 DEG C of sherwood oils and make the solution of every 1ml containing 2mg, product solution in contrast, test according to thin-layered chromatography, draw need testing solution 10～20 μ l, reference substance solution 10 μ l, put respectively on same silica gel g thin-layer plate, taking benzene: ethyl acetate=21:1.2 as developping agent, launch, take out, dry, spray is with the mixed solution of 2% vanillic aldehyde sulfuric acid solution: ethanol=1:4, dry 5～10 minutes at 100 DEG C, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(2) discriminating of caulis lonicerae
Get this product 3g, porphyrize, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, as need testing solution, separately get caulis lonicerae control medicinal material 3g, be ground into meal, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, medicinal material solution in contrast, test according to thin-layer chromatography, draw need testing solution and each 5～10 μ l of control medicinal material solution, put respectively on same silica gel H thin layer plate, taking butyl acetate: the upper solution of formic acid: water=12:6:4.5 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of radix bupleuri
Get this product 6g, 20ml adds water, be stirred to dissolve, centrifugal, get supernatant, (polyamide is crossed 100～200 mesh sieves to add polyamide column a, take the polyamide 8g after sieving, select the chromatographic column that internal diameter is 2.5～3cm, wet method dress post), water respectively, the each 100ml wash-out of 20% ethanol and 50% ethanol, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get radix bupleuri control medicinal material 1g, add water appropriate, decoct 1.5 hours, filter, filtrate is concentrated into 10ml, (polyamide is crossed 100～200 orders to add polyamide column b, take the polyamide 4g after sieving, select the chromatographic column that internal diameter is 2cm, wet method dress post), water 100ml and 50% ethanol 150ml wash-out respectively, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw need testing solution 2～10ul and control medicinal material solution 2ul, put respectively on same silica gel g thin-layer plate, taking ethyl acetate: ethanol: water=14:2.2:1.1 is as developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot colour developing, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of bigleaf thorowax root:
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make every 1ml containing bupleurotoxin, the solution of the each 1mg of acetylbupleurotoxin reference substance, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=9:1.2 as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, must not show the spot of same color.
[inspection] should meet every regulation relevant under granule item (annex I C of " Chinese Pharmacopoeia " version in 2010).
Claims (4)
1. a detection method for Yinchai Granules, comprises proterties, discriminating, inspection item, it is characterized in that: described discriminating comprises the discriminating of menthol, the discriminating of caulis lonicerae, the discriminating of radix bupleuri, the discriminating of bigleaf thorowax root, and detection method comprises following:
(1) discriminating of menthol
Get this product 12g, add 60～90 DEG C of sherwood oil 30ml, close plug, ultrasonic processing 30 minutes, filter, filtrate is as need testing solution, separately get menthol reference substance, add 60～90 DEG C of sherwood oils and make the solution of every 1ml containing 2mg, product solution in contrast, test according to thin-layered chromatography, draw need testing solution 10～20 μ l, reference substance solution 10 μ l, put respectively on same silica gel g thin-layer plate, taking benzene: ethyl acetate=17～21:0.8～1.2 are as developping agent, launch, take out, dry, spray is with the mixed solution of 2% vanillic aldehyde sulfuric acid solution: ethanol=1:4, dry 5～10 minutes at 100 DEG C, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(2) discriminating of caulis lonicerae
Get this product 3g, porphyrize, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, as need testing solution, separately get caulis lonicerae control medicinal material 3g, be ground into meal, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, medicinal material solution in contrast, test according to thin-layer chromatography, draw need testing solution and each 5～10 μ l of control medicinal material solution, put respectively on same silica gel H thin layer plate, taking butyl acetate: formic acid: the upper solution of water=8～12:4～6:3.5～4.5 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of radix bupleuri
Get this product 6g, 20ml adds water, be stirred to dissolve, centrifugal, get supernatant, add polyamide column a, water respectively, the each 100ml wash-out of 20% ethanol and 50% ethanol, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get radix bupleuri control medicinal material 1g, add water appropriate, decoct 1.5 hours, filter, filtrate is concentrated into 10ml, add polyamide column b, water 100ml and 50% ethanol 150ml wash-out respectively, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw need testing solution 2～10ul and control medicinal material solution 2ul, put respectively on same silica gel g thin-layer plate, taking ethyl acetate: ethanol: water=10～14:1.8～2.2:0.9～1.1 are as developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot colour developing, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of bigleaf thorowax root:
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make every 1ml containing bupleurotoxin, the solution of the each 1mg of acetylbupleurotoxin reference substance, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=7～9:0.8～1.2 are as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, must not show the spot of same color.
2. the detection method of Yinchai Granules according to claim 1, is characterized in that: detection method is as follows more specifically:
(1) discriminating of menthol
Get this product 12g, add 60～90 DEG C of sherwood oil 30ml, close plug, ultrasonic processing 30 minutes, filter, filtrate is as need testing solution, separately get menthol reference substance, add 60～90 DEG C of sherwood oils and make the solution of every 1ml containing 2mg, product solution in contrast, test according to thin-layered chromatography, draw need testing solution 10～20 μ l, reference substance solution 10 μ l, put respectively on same silica gel g thin-layer plate, taking benzene: ethyl acetate=19:1 as developping agent, launch, take out, dry, spray is with the mixed solution of 2% vanillic aldehyde sulfuric acid solution: ethanol=1:4, dry 5～10 minutes at 100 DEG C, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(2) discriminating of caulis lonicerae
Get this product 3g, porphyrize, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, as need testing solution, separately get caulis lonicerae control medicinal material 3g, be ground into meal, add methyl alcohol 15ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1m1 to be made to dissolve, medicinal material solution in contrast, test according to thin-layer chromatography, draw need testing solution and each 5～10 μ l of control medicinal material solution, put respectively on same silica gel H thin layer plate, taking butyl acetate: the upper solution of formic acid: water=10:5:4 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of radix bupleuri
Get this product 6g, 20ml adds water, be stirred to dissolve, centrifugal, get supernatant, add polyamide column a, water respectively, the each 100ml wash-out of 20% ethanol and 50% ethanol, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get radix bupleuri control medicinal material 1g, add water appropriate, decoct 1.5 hours, filter, filtrate is concentrated into 10ml, add polyamide column b, water 100ml and 50% ethanol 150ml wash-out respectively, collect 50% ethanol eluate, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw need testing solution 2～10ul and control medicinal material solution 2ul, put respectively on same silica gel g thin-layer plate, taking ethyl acetate: ethanol: water=12:2:1 is as developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% paradime thylaminobenzaldehyde, it is clear that hot blast blows to spot colour developing, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of bigleaf thorowax root:
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make every 1ml containing bupleurotoxin, the solution of the each 1mg of acetylbupleurotoxin reference substance, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=8:1 as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, must not show the spot of same color.
3. the detection method of Yinchai Granules according to claim 1 and 2, it is characterized in that: the described polyamide column a of step (3) is that polyamide is crossed 100～200 mesh sieves, take the polyamide 8g after sieving, select the chromatographic column that internal diameter is 2.5～3cm, wet method dress post.
4. the detection method of Yinchai Granules according to claim 1 and 2, is characterized in that: the described polyamide column b of step (3) is that polyamide is crossed 100～200 orders, takes the polyamide 4g after sieving, and selects the chromatographic column that internal diameter is 2cm, wet method dress post.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105445385A (en) * | 2014-08-28 | 2016-03-30 | 神威药业集团有限公司 | A quality detecting method for honeysuckle stem formula granules |
| CN105929102A (en) * | 2016-05-18 | 2016-09-07 | 四川逢春制药有限公司 | Detection method of bear gall pills |
| CN108896543A (en) * | 2018-08-15 | 2018-11-27 | 康美保宁（四川）制药有限公司 | A kind of qualitative checking method of FENGRE GANMAO KELI |
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| CN105445385A (en) * | 2014-08-28 | 2016-03-30 | 神威药业集团有限公司 | A quality detecting method for honeysuckle stem formula granules |
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| CN108896543A (en) * | 2018-08-15 | 2018-11-27 | 康美保宁（四川）制药有限公司 | A kind of qualitative checking method of FENGRE GANMAO KELI |
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