CN102914498A - Yanling Changchun capsule detection method - Google Patents
Yanling Changchun capsule detection method Download PDFInfo
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- CN102914498A CN102914498A CN2012103907789A CN201210390778A CN102914498A CN 102914498 A CN102914498 A CN 102914498A CN 2012103907789 A CN2012103907789 A CN 2012103907789A CN 201210390778 A CN201210390778 A CN 201210390778A CN 102914498 A CN102914498 A CN 102914498A
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Abstract
The invention provides a Yanling Changchun capsule detection method. The Yanling Changchun capsule detection method includes steps of A), observing characters of contents; B), checking under a microscope; C), identifying fructus cnidi and ginseng in formula by the thin-layer chromatography method; D), checking Yanling Changchun capsules to comply with related various regulations under capsule items according to an appendix IL of Chinese Pharmacopoeia of 2010 version; and E), measuring contents of polygonum multiflorum active components by the high-performance liquid chromatography method. By the Yanling Changchun capsule detection method, ingredients and contents of the Yanling Changchun capsule can be qualitatively and quantitatively detected, quality of the capsules is guaranteed, and accordingly, safety and effectiveness in use of the capsules are improved.
Description
Technical field
The present invention relates to the drug inspection technical field.Specifically, the present invention relates to a kind of detection method of Chinese patent drug.
Background technology
Tradition Chinese patent drug detection method can only qualitative explanation Chinese patent drug composition, the composition of efficient and quantitative detection Chinese patent drug is the technical matters that modern TCM industry is badly in need of solution.
Prolong age Changchun capsule and made through series of process such as pulverizing, extract, decoct, filter, be dry by 17 kinds of natural drugs, have good tonifying kidney and strengthening yang, Tianjing Busuiye medicinal, the effect of promoting inspiration to relieve asthma.For the insufficiency of the kidney yang, blood and essence asthenia, soreness of waist and knee joint, four limbs are cold, fatigue and asthenia, impotence and premature ejaculation, poliosis, refreshing tired win is thin to wait disease that preferably curative effect is arranged.
Prolonging age Changchun capsule is hard shell capsules, and content is for being chocolate brown powder; The gas raw meat, it is salty to distinguish the flavor of.
The prescription that prolongs Changchun capsule in age is as follows:
Pilose antler (unhairing) 8.7g deer whip 2.5g dog whip 5g
Pig testis 51.3g Penaeus seu panulirus 42g dog bone 60g
Hippocampus 53.3g gekko (foot of decaptitating) 2g prepared rhizome of rehmannia 30.7g
Colla carapacis et plastri testudinis 30g sealwort (wine system) 62g prepared fleece flower root 92g
Fruit of medicinal cornel 60g ginseng 20g frutus cnidii 46.7g
Barrenwort (processing) 30.7g stalactite (forging) 44g
The method for making of prolonging Changchun capsule in age is as follows: above 17 flavors, pilose antler, colla carapacis et plastri testudinis, ginseng, the fleece-flower root, sealwort, stalactite are ground into fine powder.Dog whip, deer whip, pig testis, gekko, Penaeus seu panulirus, hippocampus add 40% alcohol reflux and extract secondary, and each 5 hours, filter, merging filtrate, filtrate recycling ethanol also is concentrated into the clear cream of relative density 1.32～1.35 (50 ° of C).The five tastes boiling secondaries such as all the other prepared rhizomes of rehmannia, 3 hours for the first time, 2 hours for the second time, collecting decoction filtered, and filtrate is concentrated into the clear cream that relative density is 1.32～1.35 (50 ° of C).Two clear cream merge, and add above-mentioned powder mixing, and drying is pulverized, and sieves, and is encapsulated, makes 1000, and get final product.
The method for making of prolonging Changchun capsule in age is complicated, and its curative effect is subjected to the manufacture craft of quality, content and the medicament of medicinal material to affect larger.Yet existing detection method, qualitative and quantitative analysis are not comprehensive, can't better guarantee the quality of medicine, and then security and validity that medicine is used constitute a threat to.
Summary of the invention
The present invention provides one to overlap comprehensively and effectively detection method for solving above-mentioned the deficiencies in the prior art, the quality stability that Changchun capsule in age is prolonged in strict control.
Detection method of prolonging Changchun capsule in age provided by the invention comprises the steps:
A) content character observation;
B) test under microscope;
C) frutus cnidii, ginseng in the thin-layered chromatography discriminating side;
D) according to appendix IL of Chinese Pharmacopoeia version in 2010, inspection should meet every regulation relevant under the capsule item; With
E) content of fleece-flower root active component in the high effective liquid chromatography for measuring side.
In the present invention, steps A) observation is that characters powder is observed, and namely observes prolonging age Changchun capsule pharmaceutical, and its content should be chocolate brown powder; The gas raw meat, it is salty to distinguish the flavor of.
Step B) observation is test under microscope, should be irregular shape fragment, faint yellow or light gray, and bone lacuna similar round or class prismatic, size and arrangement differ, and the marginal bone tubule is radial rill.The class square crystal is numerous, and is transparent, and there are many group oblique cleavage textures on the surface that has, drips watery hydrochloric acid, produces bubble.Mucilage cell includes the needle-like calcium oxalate crystal bundle.
Step C) discriminating comprises:
(1) gets and prolong Changchun capsule 's content 3g in age, add methenyl choloride 40ml, added hot reflux 1 hour, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, filters, filtrate is extracted 2 times with methenyl choloride, each 10ml merges the methenyl choloride extract, evaporate to dryness, residue adds ethanol 0.5ml makes dissolving, as need testing solution.Other gets frutus cnidii control medicinal material 1g, adds water 20ml, adds hot reflux 1 hour, filters, and filtrate is extracted with methenyl choloride 10ml, and evaporate to dryness, residue add ethanol 1ml makes dissolving, in contrast medicinal material solution.Draw each 2 μ l of mentioned solution, put respectively on same silica gel g thin-layer plate toluene-ethyl acetate take volume ratio 12:4:0.5 ratio-glacial acetic acid solution as developping agent, launch, take out, dry, put that (365nm) inspects under the ultraviolet lamp; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color;
(2) get the residue after methenyl choloride extraction under above-mentioned (1) item, add methyl alcohol 30ml, added hot reflux 1 hour, filter, the filtrate evaporate to dryness adds water 10ml dissolving, extract 2 times with water-saturated n-butanol, each 10ml merges n-butanol extracting liquid, with 0.5% sodium hydroxide solution washing 2 times, each 10ml washes with water to neutrality again, discard washing lotion, normal butyl alcohol liquid evaporate to dryness, residue add methyl alcohol 0.5ml makes dissolving, as need testing solution.Other gets ginseng control medicinal material 1g, is made in the same way of control medicinal material solution.Other gets ginsenoside Rb
1, Re and Rg1 reference substance, add methyl alcohol and make the mixed solution that every 1ml contains 2mg, in contrast product solution.Draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, take the normal butyl alcohol-ethyl acetate of volume ratio 4:1:5 ratio-water as developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ° of C bakings several minutes, put respectively under daylight and the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, respectively spot or the fluorescence spot of aobvious same color; With the corresponding position of reference substance chromatogram on, aobvious three identical aubergine spots under the daylight, the lower aobvious yellow of ultraviolet lamp (365nm) and two fluorescent orange spots;
Step D) inspection: according to appendix IL of Chinese Pharmacopoeia version in 2010, inspection should meet every regulation relevant under the capsule item.That is, moisture, content uniformity, disintegration time limited, heavy metal inspection, arsenic salt check, limit test of microbe should be up to specification.
Step e) assay comprises:
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Acetonitrile-water (volume ratio 22:78) is mobile phase; The detection wavelength is 320nm; Number of theoretical plate by 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-Glucose glycosides peak calculates and should be not less than 3000;
The preparation precision of reference substance solution takes by weighing 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-Glucose glycosides reference substance is an amount of, adds Diluted Alcohol (20 ℃ time concentration be 19.5% ~ 50.5%) and makes the solution that every 1ml contains 0.05mg, and shake up, and get final product;
The preparation of need testing solution is got and prolonged the about 0.8g of content under the Changchun capsule content uniformity in age, and is accurately weighed, puts in the 100ml conical flask, accurate Diluted Alcohol (20 ℃ time concentration be 19.5% ~ 50.5%) 50ml that adds, weighed weight was soaked ultrasonic processing 30 minutes 1 hour, be cooled to room temperature, supply weight with Diluted Alcohol (20 ℃ time concentration be 19.5% ~ 50.5%), shake up, filter, get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product;
Prolong age every of Changchun capsule and contain prepared fleece flower root with 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides meter, must not be less than 0.08mg.。
By above-mentioned detection method, can do good qualitative detection and quantitatively detect the quality of assurance medicine, thereby security and validity that the raising medicine uses the composition and the content that prolong Changchun capsule in age.
Claims (3)
1. detection method of prolonging Changchun capsule in age is characterized in that the method is comprised of the following step:
A) content character observation;
B) test under microscope;
C) frutus cnidii, ginseng in the thin-layered chromatography discriminating side;
D) according to appendix IL of Chinese Pharmacopoeia version in 2010, inspection should meet every regulation relevant under the capsule item; With
E) content of fleece-flower root active component in the high effective liquid chromatography for measuring side.
2. detection method of prolonging Changchun capsule in age according to claim 1 is characterized in that, described step C) step as follows:
(1) gets and prolong Changchun capsule 's content 3g in age, add methenyl choloride 40ml, added hot reflux 1 hour, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, filters, filtrate is extracted 2 times with methenyl choloride, each 10ml merges the methenyl choloride extract, evaporate to dryness, residue adds ethanol 0.5ml makes dissolving, as need testing solution; Other gets frutus cnidii control medicinal material 1g, adds water 20ml, adds hot reflux 1 hour, filters, and filtrate is extracted with methenyl choloride 10ml, and evaporate to dryness, residue add ethanol 1ml makes dissolving, in contrast medicinal material solution; According to the thin-layered chromatography test, draw each 2 μ l of mentioned solution, put respectively on same silica gel g thin-layer plate, take the toluene-ethyl acetate of volume ratio 12:4:0.5 ratio-glacial acetic acid solution as developping agent, launch, take out, dry, put under the ultraviolet lamp (365nm) and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color;
(2) get the residue after methenyl choloride extraction under above-mentioned (1) item, add methyl alcohol 30ml, added hot reflux 1 hour, filter, the filtrate evaporate to dryness adds water 10ml dissolving, extract 2 times with water-saturated n-butanol, each 10ml merges n-butanol extracting liquid, with 0.5% sodium hydroxide solution washing 2 times, each 10ml washes with water to neutrality again, discard washing lotion, normal butyl alcohol liquid evaporate to dryness, residue add methyl alcohol 0.5ml makes dissolving, as need testing solution; Other gets ginseng control medicinal material 1g, is made in the same way of control medicinal material solution; Other gets ginsenoside Rb1, Re and Rg1 reference substance, adds methyl alcohol and makes the mixed solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, take the normal butyl alcohol-ethyl acetate of volume ratio 4:1:5 ratio-water as developping agent, launch, take out, dry, spray, is put respectively under daylight and the ultraviolet lamp (365nm) and is inspected 105 ° of C bakings several minutes with 10% ethanol solution of sulfuric acid; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, respectively spot or the fluorescence spot of aobvious same color; With the corresponding position of reference substance chromatogram on, aobvious three identical aubergine spots under the daylight, the lower aobvious yellow of ultraviolet lamp (365nm) and two fluorescent orange spots.
3. detection method of prolonging Changchun capsule in age according to claim 1 and 2 is characterized in that,
Described step e) step is as follows:
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Acetonitrile-water of volume ratio 22:78 is mobile phase; The detection wavelength is 320nm; Number of theoretical plate by 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-Glucose glycosides peak calculates and should be not less than 3000;
The preparation precision of reference substance solution takes by weighing 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-Glucose glycosides reference substance is an amount of, and concentration is that 19.5% ~ 50.5% Diluted Alcohol is made the solution that every 1ml contains 0.05mg when adding 20 ℃, shakes up, and get final product;
The preparation of need testing solution is got and prolonged the about 0.8g of content under the Changchun capsule content uniformity in age, and is accurately weighed, puts in the 100ml conical flask, the accurate Diluted Alcohol 50ml that adds, weighed weight was soaked ultrasonic processing 30 minutes 1 hour, be cooled to room temperature, concentration is that 19.5% ~ 50.5% Diluted Alcohol is supplied weight during with 20 ℃, shakes up, and filters, get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product;
Described age every of the Changchun capsule of prolonging contains prepared fleece flower root with 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides meter, must not be less than 0.08mg.
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Cited By (1)
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| CN108414667A (en) * | 2018-01-19 | 2018-08-17 | 广西中医药大学附属瑞康医院 | The detection method of one seed ginseng osmanthus Yixin granule quality standard |
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Inventor after: Lu Haitao Inventor after: Kang Jian Inventor before: Lu Haitao |
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Application publication date: 20130206 |