CN101269097A - Alstonia-leaf medicinal materials and medicament testing method for its preparation - Google Patents
Alstonia-leaf medicinal materials and medicament testing method for its preparation Download PDFInfo
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Abstract
The invention relates to a medicinal material of alstonia-leaf and the drug detecting method of the pharmaceutical preparations of alstonia-leaf. The invention is characterized in that a thin-layer chromatography is adopted to detect the effective ingredients of kaempferol-3-O-Beta-D-galactose-(2-1)-O-Beta-D-xylopyranoside and quercetin-3-O-Beta-D-galactose-(2--1)-O-Beta-D- xylopyranoside of the alstonia-leaf and the pharmaceutical preparations of alstonia-leaf qualitatively. Spectrophotometry is adopted to realize a quality analysis and control of the alstonia-leaf and the pharmaceutical preparations of alstonia-leaf. The invention overcomes the deficiencies that the prior art can only detect the alkaloid components yet fail to detect a type of more important active ingredient flavonoid glycoside in the alstonia-leaf and the pharmaceutical preparations of alstonia-leaf . The method of the invention can precisely detect flavonoid glycoside active-ingredient compound 1, flavonoid glycoside active-ingredient compound 2 and the contents in the alstonia-leaf and the pharmaceutical preparations of alstonia-leaf. The method can be used for evaluating the quality of alstonia-leaf and detecting the quality analysis of the pharmaceutical preparations of various types adopting alstonia-leaf as the medicinal ingredient, such as granules, tablets, capsules, oral liquid and so on. The method is directly applicable to an actual production process and a quality analysis of the product.
Description
Technical field
The present invention relates to pharmaceutical analysis detection technique field, specifically the drug detection method of Folium Alstoniae Scholaris medical material and preparation thereof.
Background technology
Cornus controversa Alstonia Scholaris (L.) R.Bro. is an apocynaceae plant, the south of Yunnan that mainly distributes, aboundresources.Folium Alstoniae Scholaris is the natural drug of multi-national use, is used for the treatment of respiratory system diseases such as cough due to lung-heat, abundant expectoration, bronchitis, and medical material has been " Yunnan Province's drug standard ", " Chinese pharmacopoeia is recorded.Utilize Folium Alstoniae Scholaris to be raw material, developed formulation products such as Folium Alstoniae Scholaris granule, tablet, capsule, oral liquid.
Chemical research for Folium Alstoniae Scholaris, the bright thesis for the doctorate of Zhu Wei " preliminary study of five kinds of resources of medicinal plant chemistry ", Zhu Hua thesis for the doctorate " chemistry of five kinds of medicinal plants and active component research " has carried out systematic study and literature review to alkaloid component in (Kunming Inst. of Botany, Chinese Academy of Sciences, calendar year 2001,2006).Aspect the drug quality analysis, " Yunnan Province's drug standard " only differentiated with simple alkaloid precipitation the Folium Alstoniae Scholaris medical material, no assay project; Health Chinese medicine standard promulgated by the ministries or commissions of the Central Government Folium Alstoniae Scholaris granule does not have the physics and chemistry test item, and the lamp-stand blade adopts acid-base titrations to survey alkaloid, and conversion is index components picrinine content, but the specificity of assay method is poor, can not adapt to the specification requirement of the modernization of Chinese medicine.
For improving Folium Alstoniae Scholaris medical material and quality of the pharmaceutical preparations analytical technique thereof, some research report or related application have been arranged.Zhu Guangrong application " application of picrinine in the control Folium Alstoniae Scholaris medical material and the quality of the pharmaceutical preparations thereof " patent (is authorized, CN100356172C); Kunming Zhenhua Pharmacy Co., Ltd. is studied the detection method of Folium Alstoniae Scholaris main alkaloid composition picrinine, patent (open, CN 1975412A) that application " is measured the efficient liquid-phase chromatography method of alkali picrinine content "; The Kunming plant research is applied for " medicine of treatment diseases concerned with respiratory and its production and application " (openly, CN101084951A), " medicine and the application thereof of treatment diseases concerned with respiratory " patent (open, CN 101084894A); Nat'l Pharmaceutical ﹠ Biological Products Control Institute's application " a kind of Chinese medicine composition for the treatment of cough, asthma " patent (open, CN101028323A).Research and patent that these are relevant all just relate to the alkaloids composition that contains in the Folium Alstoniae Scholaris, especially the analytical method of main component alkali picrinine and application in drug quality control thereof.
Summary of the invention
The purpose of this invention is to provide a kind of analyzing and testing Folium Alstoniae Scholaris medical material and be effective ingredient chemical compound 1 and 2 method in the various preparations of raw material production with the Folium Alstoniae Scholaris.This method is with chemical compound 1,2 in thin layer chromatography qualitative detection Folium Alstoniae Scholaris medical material and the preparation thereof, and realizes quality analysis and control to Folium Alstoniae Scholaris medical material and preparation thereof with its content of spectrophotometry.
The inventor further studies confirm that Folium Alstoniae Scholaris, Folium Alstoniae Scholaris also contains more flavonoid glycoside composition except that alkaloid component, and find there are two flavonoid glycoside compositions that content is higher first: kaempferol-3-O-β-D-galactose-(2--1)-O-β-D-xyloside, Quercetin-3-O-β-D-galactose-(2--1)-O-β-D-xyloside (to call chemical compound 1,2 in the following text, its structure is seen accompanying drawing 1).Through pharmacological testing proof chemical compound 1 and 2 is Folium Alstoniae Scholaris and preparation antiinflammatory thereof, cough-relieving, analgesic effective ingredient.Existence and content to chemical compound 1 and 2 are analyzed and are detected, and can be used as the important indicator of the control Folium Alstoniae Scholaris and the quality of the pharmaceutical preparations thereof.
(1) detect chemical compound 1 and 2 in Folium Alstoniae Scholaris medical material and the preparation thereof with thin layer chromatography: with the silica gel G is adsorbent, is developing solvent with the mixed solution of ethyl acetate-butanone-formic acid-water; The volume ratio of the contained four kinds of solvents of developing solvent is an ethyl acetate: butanone: formic acid: water=5: 3～5: 0.5～1: 0.5～1.Its best proportioning is an ethyl acetate: butanone: formic acid: water=5: 3: 1: 1.
Wherein, the ethyl acetate in the developing solvent can be used C
1-C
4Fatty acid and C
1-C
4The ester that forms of aliphatic alcohol substitute, butanone can be used C
3-C
6Lower aliphatic ketone substitute, formic acid can be used C
2-C
6Lower fatty acid substitute.
(2) with the content of chemical compound 1 in spectrophotometry Folium Alstoniae Scholaris medical material and the preparation thereof and 2: in the presence of sodium nitrite, be developer with the aluminum nitrate, absorption value is measured in 510nm in the colour developing back in diluted sodium hydroxide solution, and its content is relatively determined with the absorption value of 2 blended standard solution under identical color condition with chemical compound 1 with absorption value.
Above-described preparation is to be the various preparations of raw material production with the Folium Alstoniae Scholaris, comprises Folium Alstoniae Scholaris granule, tablet, capsule, oral liquid etc.
Table one chemical compound 1 and 2 main spectroscopic data
(1) influence of chemical compound 1 and 2 pairs of ammonia induced mice coughs
Choose 18～22g mice, on glass plate, push 25% strong aqua ammonia 0.04mL with 300mL glass beaker left-hand thread simultaneously rapidly in vessel, observe the cough number of times in the mice 2min, typical case's cough actor is the qualified animal of screening more than 3 times to occur in the 2min.Get 60 of the qualified mices of screening, male and female half and half are divided into 6 groups at random by sex, body weight, 10 every group.Each treated animal is pressed table two dosage respectively and is irritated stomach 1 time, and pure water is held in blank group filling etc.30min puts into mice one by one and uses 300mL glass beaker left-hand thread on the glass plate after irritating stomach, pushes 25% strong aqua ammonia 0.04mL simultaneously in vessel rapidly, the cough number of times of mice in the record 2min, and result and statistical analysis see Table two.
The result shows that the high dose of codeine phosphate group (positive drug), chemical compound 1,2 all can obviously reduce the cough number of times that strong aqua ammonia causes mice; Chemical compound 1,2 has antitussive action.
Table two chemical compound 1 and the 2 pairs of strong aqua ammonia cause the influence of mouse cough
(2) influence of chemical compound 1 and 2 xylol induced mice auricle edemas
Choose 60 of 18～22g mices, male and female half and half are divided into 6 groups at random by sex and body weight, 10 every group.Each treated animal is pressed table three dosage respectively and is irritated stomach 1 time, and pure water is held in blank group filling etc., and 30min evenly smears the caused by dimethylbenzene xylene inflammation by 0.1mL/ amount only in the mouse right ear two sides after administration.Mice is put to death in dislocation behind the 1h, cuts ears along the auricle baseline, and two ears are stacked alignment,, weighs in downcutting auricle with the position homalographic with the 9mm card punch, calculates swelling degree and suppression ratio according to following formula, and result and statistical analysis see Table three.
Swelling degree=auris dextra sheet weight (causing scorching side)-left auricle weight (normal side)
Suppression ratio=[(blank group auricle swelling degree-other respectively organize auricle swelling degree)/blank group auricle swelling degree] * 100%
The result shows, aspirin (positive drug), chemical compound 1 high dose, chemical compound are 2 low, high dose all can obviously suppress by the mice auricle swelling due to the dimethylbenzene; The strong antiinflammatory action of chemical compound 1,2 tools.
Table three chemical compound 1 and 2 xylol cause the influence of mice auricle swelling
(3) chemical compound 1 and 2 pairs of influences that the phenol red secretion of mice trachea is discharged
Accurately take by weighing the phenol red solution that is formulated as variable concentrations, measure absorption value (OD) at the 546nm place with photometer, (μ g/mL) is abscissa with phenol red concentration, and the OD value is a vertical coordinate drawing standard curve.
Select 60 of 18～22g mices for use, male and female half and half are divided into 6 groups at random by sex and body weight, 10 every group.Each treated animal is pressed table four dosage gastric infusion respectively 1 time, pure water is held in blank group fillings etc., phenol red according to 0.1mL/10g body weight lumbar injection 0.5% respectively behind administration 30min, behind 30min, take off cervical vertebra again and put to death animal, peel off the trachea surrounding tissue, cut one section trachea down to the bronchus crotch from thyroid cartilage, put into the test tube that fills the 2mL normal saline, add 0.1mL sodium hydroxide (1mol/L) again, supersound process 5min, centrifugalize is drawn supernatant and is measured the OD value at wavelength 546nm place.Calculate the phenol red concentration of discharge in the mice tracheal secretion according to standard curve, result and statistical analysis see Table four.
The result shows, the phenol red excretion amount that ammonium chloride (positive drug), chemical compound 1 high dose, chemical compound are 2 low, high dose all can obviously increase the mice trachea; Chemical compound 1,2 has phlegm-dispelling functions.
The influence of table Four Modernizations compound 1 and the phenol red discharge of 2 pairs of mice tracheas
(4) chemical compound 1 and 2 Dichlorodiphenyl Acetates cause the influence of mouse writhing pain
Choose 60 of 18～22g mices, male and female half and half are divided into 6 groups at random by sex and body weight, 10 every group.Each treated animal is pressed table five dosage respectively and is irritated stomach 1 time, and pure water is held in blank group filling etc.After irritating stomach 45min, inject with the amount mouse peritoneal of 0.1mL/10g with 0.6% glacial acetic acid normal saline solution respectively, observe and the writhing response number of times of record test mice in 10min, calculate suppression ratio according to following formula, result and statistical analysis see Table five.
Suppression ratio=[(blank group is turned round body number of times-test group and turned round the body number of times)/blank group is turned round the body number of times] * 100%
The result shows, aspirin (positive drug), chemical compound are 1,2 low, high dose all can significantly suppress the acetic acid induced mice turns round body pain; Chemical compound 1,2 has analgesic activity.
Table five chemical compound 1 and 2 Dichlorodiphenyl Acetates cause the influence of mouse writhing pain
The present invention has overcome art methods only can detect alkaloids composition in Folium Alstoniae Scholaris and the preparation thereof, and do not detect the weak point of another kind of even more important active component flavonoid glycoside, a kind of qualitative identification and quantitative analysis method that can accurately detect in Folium Alstoniae Scholaris medical material and the preparation thereof two flavonoid glycoside effective ingredient chemical compounds 1 and 2 is provided, can be used for accurately estimating the Folium Alstoniae Scholaris quality of medicinal material, also can be used for detecting with the Folium Alstoniae Scholaris is various preparations (the Folium Alstoniae Scholaris granule of raw material production, tablet, capsule, oral liquid etc.) quality analysis can directly apply to the quality analysis of actual production process and product.
Description of drawings
Fig. 1 is the chemical structural formula of chemical compound 1 and 2.
Fig. 2 is a different places of production Folium Alstoniae Scholaris medical material thin-layer chromatographic analysis collection of illustrative plates.
Fig. 3 is the standard curve of spectrophotometry content of the present invention.
The specific embodiment
Following specific embodiment can further specify the present invention and application thereof, but does not constitute the restriction of the scope that claim of the present invention is protected.Its operation principle and process are:
1. thin layer chromatography qualitative detection: the chemical compound of same structure, on same chromatographic sheet, launch with same mobile phase solvent, should show consistent chromatographic behavior; Directly on chromatographic sheet, launch the back contrast with reference substance and detected sample,, can determine whether there be the chemical constituent consistent in the sample with reference substance according to whether identical speckle occurring in the position identical with reference substance.
The key technology main points of thin layer chromatography are at different products, different compositions, by systematic research and comparison, screen, determine to have the developing solvent system of optimal separation effect.
2. spectrophotometric detection by quantitative: the flavone compound that contains in the Folium Alstoniae Scholaris, in the presence of sodium nitrite, produce complex reaction with aluminum nitrate reagent, there is absorption maximum the colour developing back at 510nm in diluted sodium hydroxide solution, its absorption value and content are linear, can relatively determine its content with the absorption value of standard solution under identical color condition according to its absorption value.
Embodiment 1: the analyzing and testing of Folium Alstoniae Scholaris medical material-1
1, chemical compound 1 with 2 separate and structure is identified
(1) extraction separation
Cornus controversa medical material 50kg pulverizes the back and uses 95% alcohol reflux, and decompression and solvent recovery gets extractum.Alcohol-extracted extract adds water and stirs and use ethyl acetate, n-butanol extraction successively after loosing, and reclaims n-butyl alcohol and partly obtains the flavonoid glycoside mixture.The flavonoid glycoside mixture is eluant enrichment flavonoid glycoside through the decolouring of MCI post with methanol.The flavonoid glycoside of enrichment separates repeatedly through the sephadex lh-20 chromatograph again, is eluant with methanol, in conjunction with conventional purification process such as recrystallization, obtains chemical compound 1 and 2.
(2) structure is identified
Chemical compound 1: yellow powder, be soluble in methanol, water, be insoluble to chloroform, ethyl acetate etc., but dissolve in dilute alkaline soln.214～217 ℃ of fusing points.Determine that by physics and chemistry and spectrum test the structure of chemical compound 1 is kaempferol-3-O-β-D-galactose-(2--1)-O-β-D-xyloside.
Chemical compound 2: yellow powder, be soluble in methanol, water, be insoluble to chloroform, ethyl acetate etc., but dissolve in dilute alkaline soln.215～219 ℃ of fusing points.Determine that by physics and chemistry and spectrum test the structure of chemical compound 2 is Quercetin-3-O-β-D-galactose-(2--1)-O-β-D-xyloside.
2, chemical compound 1 and 2 thin layer chromatography qualitative detection
(1) preparation of reference substance and sample solution
The flavonoid glycoside compound 1 and 2 that takes by weighing extraction separation from Folium Alstoniae Scholaris respectively is an amount of, makes the solution of about 1mg/mL with dissolve with ethanol, is reference substance solution.The drying in the sun Folium Alstoniae Scholaris was pulverized 40 eye mesh screens, got powder 2g and added the 20mL alcohol solvent, soaked supersound process 30min extraction after 1 hour, filtered, and filtrate is reclaimed solvent and got ethanol extract.Ethanol extract filters with the weak ammonia 20mL dissolving of pH=8.5; Filtrate again with 20mL n-butanol extraction flavonoid glycoside, is reclaimed butanol solution with the dilute hydrochloric acid pH=4 that neutralizes, and residue 1mL dissolve with methanol is the sample solution of confession thin-layer chromatographic analysis.
(2) thin-layer chromatographic analysis of Folium Alstoniae Scholaris sample and judgement
With the silica gel G plate is adsorbent, presses 5: 3: 1 with ethyl acetate-butanone-formic acid-water: 1 volume ratio preparation developing solvent; Analyze 17 parts of Folium Alstoniae Scholaris medical material samples that compare from 15 places of production, thin-layer chromatogram is seen accompanying drawing 2.Different place of production Folium Alstoniae Scholaris medical materials (sample 1-10,12-13,15-16) all can detect chemical compound 1 and 2; 2 parts of Folium Alstoniae Scholaris medical materials that go mouldy fully (sample 11,14) fail to detect chemical compound 1 and 2; 1 part of Folium Alstoniae Scholaris medical material (sample 17) that part is gone mouldy detects a spot of chemical compound 1 and 2.
Result according to the thin layer chromatography qualitative detection judges: Folium Alstoniae Scholaris medical material sample 1-10,12-13,15-16 are qualified medical materials, and sample 11,14,17 (go mouldy or partly go mouldy) is a medical material inferior.
2, chemical compound 1 and 2 assay
(1) preparation of reference substance and sample solution
Accurately take by weighing chemical compound 1 and 2 each 12.5mg, place the 50mL measuring bottle, add dissolve with methanol and be settled to scale, promptly get the reference substance solution that concentration is 0.5mg/mL, standby.
The Folium Alstoniae Scholaris pulverizing medicinal materials is crossed 60 eye mesh screens, and precision takes by weighing 1g, puts in the 100mL round-bottomed flask, accurately adds ethanol 50mL, claims decide weight, soaks after 1 hour, and reflux, extract, 1 hour is put coldly, supplies the weight that subtracts mistake with ethanol, filtration, and it is standby to get subsequent filtrate.The accurate extracting solution 10mL decompression recycling ethanol of drawing, residue adds the weak ammonia 20mL dissolving of pH=8.5, filters, and subsequent filtrate is standby.
(2) standard curve
Accurately draw 0.5mg/mL reference substance solution 0,1,2,3,4,5,6,7mL respectively, put in the 25mL measuring bottle, replenish an amount of purified water respectively to 10mL.The sodium nitrite solution 1mL that each adds 5% shakes up; Place after 6 minutes, add 10% aluminum nitrate 1mL, shake up; Place after 6 minutes, add 4% sodium hydroxide 10mL again, after shaking up, be settled to scale with purified water; Placing after 15 minutes, is reference with the blank solution, measures its absorbance A, data such as table six at the 510nm place.The data regression treatment gets regression equation: A=6.3036 * C+0.0182, and r=0.9999, standard curve see accompanying drawing 3.
The linear relationship of table six spectrophotometry content
| Sample volume mL | 0.5 | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Solution concentration mg/mL | 0.01 | 0.02 | 0.04 | 0.06 | 0.08 | 0.10 | 0.12 | 0.14 |
| Absorbance A | 0.083 | 0.144 | 0.268 | 0.394 | 0.526 | 0.650 | 0.774 | 0.900 |
(3) sample determination
Accurately draw each sample solution 2mL of Folium Alstoniae Scholaris, put in the 25mL measuring bottle, add the 8mL purified water, add 5% sodium nitrite solution 1mL, shake up; Place after 6 minutes, add 10% aluminum nitrate 1mL, shake up; Place after 6 minutes, add 4% sodium hydroxide 10mL again, after shaking up, be settled to scale with purified water; Placing after 15 minutes, is reference with the blank solution, measures its absorbance A at the 510nm place.
The sample absorbance A of measuring, establishing criteria curve calculation flavonoid glycoside chemical compound 1 and 2 total content.The determination data of the Folium Alstoniae Scholaris medical material in the different places of production sees Table seven.
The content of flavonoid glycoside compound in the Folium Alstoniae Scholaris medical material of the different place of production of table seven
| Sample number into spectrum | Content % | Sample number into spectrum | Content % | Sample number into | Content % | |
| 1 # | 3.458 | 7 # | 2.485 | 13 # | 4.616 | |
| 2 # | 2.750 | 8 # | 4.604 | 14 # | 0.440 | |
| 3 # | 5.268 | 9 # | 2.666 | 15 # | 2.811 | |
| 4 # | 2.656 | 10 # | 2.785 | 16 # | 5.247 | |
| 5 # | 2.378 | 11 # | 0.436 | 17 # | 0.737 | |
| 6 # | 5.118 | 12 # | 2.096 |
Testing result shows, the effective component content of different Folium Alstoniae Scholaris medical materials is differentiated, the flavonoid glycoside compound content of Folium Alstoniae Scholaris medical material sample 1-10,12-13,15-16 is between 2.096%～5.118%, and is best in quality with the sample 3,6,8,13,16 that content is higher.And go mouldy or the content of the sample 11,14,17 that goes mouldy of part only between 0.436%～0.7378%, belong to medical material inferior.The The qualitative analysis that the quantitative analysis results of assay and thin layer chromatography detect has concordance.The content of flavonoid glycoside has been represented the quality of Folium Alstoniae Scholaris quality of medicinal material, can be directly used in objective evaluation Folium Alstoniae Scholaris quality of medicinal material.
Embodiment 2: the analyzing and testing of Folium Alstoniae Scholaris medical material-2
Method is with embodiment 1, but the expansion solvent of thin-layer chromatographic analysis is changed into: ethyl acetate-butanone-formic acid-water=5: 5: 1: 1.Testing result: judge consistent with embodiment 1.
Embodiment 3: the analyzing and testing of Folium Alstoniae Scholaris medical material-3
Method is with embodiment 1, but the expansion solvent of thin-layer chromatographic analysis is changed into: ethyl acetate-butanone-formic acid-water=5: 3: 0.5: 1.Testing result: judge consistent with embodiment 1.
Embodiment 4: the analyzing and testing of Folium Alstoniae Scholaris medical material-4
Method is with embodiment 1, but the expansion solvent of thin-layer chromatographic analysis is changed into: ethyl acetate-butanone-formic acid-water=5: 3: 1: 0.5.Testing result: judge consistent with embodiment 1.
Embodiment 5: the analyzing and testing of Folium Alstoniae Scholaris medical material-5
Method is with embodiment 1, but the expansion solvent of thin-layer chromatographic analysis is changed into: butyl formate-acetone-acetic acid-water=5: 3: 1: 1.Testing result: judge consistent with embodiment 1.
Embodiment 6: the analyzing and testing of Folium Alstoniae Scholaris medical material-6
Method is with embodiment 1, but the expansion solvent of thin-layer chromatographic analysis is changed into: methyl butyl-pentanone-formic acid-water=5: 4: 1: 1.Testing result: judge consistent with embodiment 1.
Embodiment 7: the analyzing and testing of Folium Alstoniae Scholaris medical material-7
Method is with embodiment 1, but the expansion solvent of thin-layer chromatographic analysis is changed into: methyl butyl-pentanone-butanoic acid-water=5: 5: 1: 1.Testing result: judge consistent with embodiment 1.
Embodiment 8: the analyzing and testing of Folium Alstoniae Scholaris medical material-8
Method is with embodiment 1, but the expansion solvent of thin-layer chromatographic analysis is changed into: ethyl acetate-butanone-n-caproic acid-water=5: 4: 1: 1.Testing result: judge consistent with embodiment 1.
Embodiment 9: the particulate detection of Folium Alstoniae Scholaris
Folium Alstoniae Scholaris granule 2g adds 20mL hot water and dissolves, and neutralizes behind the pH=4 again with 20mL n-butanol extraction flavonoid glycoside with dilute hydrochloric acid, reclaims butanol solution, and residue 1mL dissolve with methanol is sample solution.Reference substance solution preparation, point sample, expansion, judgement are equal to embodiment 1, and the expansion solvent is ethyl acetate-butanone-formic acid-water=5: 3: 1: 1.The result is: can detect flavonoid glycoside compound 1 and 2 in the Folium Alstoniae Scholaris granule.
Precision takes by weighing 1g Folium Alstoniae Scholaris granule, and the accurate weak ammonia 20mL that adds pH=8.5 dissolves, and filters, and accurately draws subsequent filtrate 2mL, puts in the 25mL measuring bottle, and following moisturizing, colour developing, mensuration are equal to embodiment 1.The total amount that contains flavonoid glycoside chemical compound 1 and 2 in the Folium Alstoniae Scholaris granule is 2.17%.
Embodiment 10: the capsular detection of Folium Alstoniae Scholaris
Method is got the Folium Alstoniae Scholaris capsule 's content and is detected with embodiment 9, and the result is: can detect flavonoid glycoside compound 1 and 2 in the Folium Alstoniae Scholaris capsule; The total amount that contains flavonoid glycoside chemical compound 1 and 2 in the Folium Alstoniae Scholaris capsule is 1.75%.
Embodiment 11: the detection of Folium Alstoniae Scholaris oral liquid
Method is got the Folium Alstoniae Scholaris oral liquid and is detected with embodiment 9, and the result is: can detect flavonoid glycoside compound 1 and 2 in the Folium Alstoniae Scholaris oral liquid; The total amount that contains flavonoid glycoside chemical compound 1 and 2 in the Folium Alstoniae Scholaris oral liquid is 1.58%.
Embodiment 12: the detection of lamp-stand blade
Method is with embodiment 9, detects after getting lamp-stand blade levigation, and the result is: can detect flavonoid glycoside compound 1 and 2 in the lamp-stand blade; The total amount that contains flavonoid glycoside chemical compound 1 and 2 in the lamp-stand blade is 2.32%.
Claims (6)
1, the drug detection method of a kind of Folium Alstoniae Scholaris medical material and preparation thereof, it is characterized in that:, realize quality analysis and control Folium Alstoniae Scholaris medical material and preparation thereof with its content of spectrophotometry with the effective ingredient kaempferol-3-O-β-D-galactose of thin layer chromatography qualitative detection Folium Alstoniae Scholaris medical material and preparation thereof-(2--1)-O-β-D-xyloside, Quercetin-3-O-β-D-galactose-(2--1)-O-β-D-xyloside.
2, according to the drug detection method of described Folium Alstoniae Scholaris medical material of claim 1 and preparation thereof, it is characterized in that: thin-layered chromatography detection method is to be adsorbent with the silica gel G, is developing solvent with the mixed solution of ethyl acetate-butanone-formic acid-water; The volume ratio of the contained four kinds of solvents of developing solvent is an ethyl acetate: butanone: formic acid: water=5: 3～5: 0.5～1: 0.5～1.
3, according to the drug detection method of described Folium Alstoniae Scholaris medical material of claim 2 and preparation thereof, it is characterized in that: the volume ratio of the contained four kinds of solvents of developing solvent is an ethyl acetate: butanone: formic acid: water=5: 3: 1: 1.
4, according to the detection method of described Folium Alstoniae Scholaris medical material of claim 2 and preparation thereof, it is characterized in that: the ethyl acetate C in the developing solvent
1-C
4Fatty acid and C
1-C
4The ester that forms of aliphatic alcohol substitute butanone C
3-C
6Lower aliphatic ketone substitute formic acid C
2-C
6Lower fatty acid substitute.
5, according to the drug detection method of described Folium Alstoniae Scholaris medical material of claim 1 and preparation thereof, the spectrophotometric method that it is characterized in that described assay is: be developer with the aluminum nitrate in the presence of sodium nitrite, absorption value is measured in 510nm in colour developing back in diluted sodium hydroxide solution, and its content with the absorption value of sample solution and kaempferol-3-O-β-D-galactose-(2--1)-O-β-D-xyloside, Quercetin-3-O-β-D-galactose-(the 2--1)-absorption value of O-β-blended standard solution of D-xyloside under identical color condition relatively and determine.
6,, it is characterized in that described preparation is is the various preparations of raw material production with the Folium Alstoniae Scholaris, comprises Folium Alstoniae Scholaris granule, tablet, capsule, oral liquid according to the drug detection method of described Folium Alstoniae Scholaris medical material of claim 1 and preparation thereof.
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| CN100356172C (en) * | 2006-03-16 | 2007-12-19 | 朱光荣 | Use of picrinine in quality control of Dengtaiye medicine and its preparation |
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| RU2641093C1 (en) * | 2016-12-01 | 2018-01-15 | федеральное государственное автономное образовательное учреждение высшего образования "Российский университет дружбы народов" (РУДН) | Method for wild camomile flowers identification |
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