CN109030681A - The method for identifying the subprostrate sophora true and false - Google Patents
The method for identifying the subprostrate sophora true and false Download PDFInfo
- Publication number
- CN109030681A CN109030681A CN201811102881.2A CN201811102881A CN109030681A CN 109030681 A CN109030681 A CN 109030681A CN 201811102881 A CN201811102881 A CN 201811102881A CN 109030681 A CN109030681 A CN 109030681A
- Authority
- CN
- China
- Prior art keywords
- subprostrate sophora
- medicinal material
- phenyl benzofurans
- material sample
- phenyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 241000219784 Sophora Species 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 34
- HXMZLDUBSSPQIB-UHFFFAOYSA-N 2-phenyl-1-benzofuran Chemical class O1C2=CC=CC=C2C=C1C1=CC=CC=C1 HXMZLDUBSSPQIB-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000000463 material Substances 0.000 claims abstract description 49
- 238000001514 detection method Methods 0.000 claims abstract description 20
- 238000005259 measurement Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 69
- 239000000523 sample Substances 0.000 claims description 57
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 33
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- 235000019441 ethanol Nutrition 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 23
- 239000012086 standard solution Substances 0.000 claims description 22
- 239000012488 sample solution Substances 0.000 claims description 20
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 18
- 238000010828 elution Methods 0.000 claims description 17
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 claims description 16
- 239000000284 extract Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 6
- 239000000287 crude extract Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000010812 external standard method Methods 0.000 claims description 4
- 238000004811 liquid chromatography Methods 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- -1 2- (2', 4'- dihydroxy phenyl) -5,6- dioxymethylene benzofuran Chemical class 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 2
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 1
- 238000010025 steaming Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 15
- 238000012360 testing method Methods 0.000 description 11
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 5
- 244000046052 Phaseolus vulgaris Species 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- XVPBINOPNYFXID-JARXUMMXSA-N 85u4c366qs Chemical compound C([C@@H]1CCC[N@+]2(CCC[C@H]3[C@@H]21)[O-])N1[C@@H]3CCCC1=O XVPBINOPNYFXID-JARXUMMXSA-N 0.000 description 4
- ZSBXGIUJOOQZMP-UHFFFAOYSA-N Isomatrine Natural products C1CCC2CN3C(=O)CCCC3C3C2N1CCC3 ZSBXGIUJOOQZMP-UHFFFAOYSA-N 0.000 description 4
- ZSBXGIUJOOQZMP-JLNYLFASSA-N Matrine Chemical compound C1CC[C@H]2CN3C(=O)CCC[C@@H]3[C@@H]3[C@H]2N1CCC3 ZSBXGIUJOOQZMP-JLNYLFASSA-N 0.000 description 4
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 4
- 229930014456 matrine Natural products 0.000 description 4
- 229930015582 oxymatrine Natural products 0.000 description 4
- 150000002240 furans Chemical class 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 230000003252 repetitive effect Effects 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- AQASRZOCERRGBL-UHFFFAOYSA-N Dauricine Natural products CN1CCC2=CC(OC)=C(OC)C=C2C1CC1=CC=C(O)C(OC2=CC=C(C=C2)CC2N(C)CCC=3C=C(C(=CC=32)OC)OC)=C1 AQASRZOCERRGBL-UHFFFAOYSA-N 0.000 description 1
- 206010068319 Oropharyngeal pain Diseases 0.000 description 1
- 201000007100 Pharyngitis Diseases 0.000 description 1
- AAGFPTSOPGCENQ-UHFFFAOYSA-N Sophocarpin I Natural products C1CCC2CN3C(=O)C=CCC3C3C2N1CCC3 AAGFPTSOPGCENQ-UHFFFAOYSA-N 0.000 description 1
- IGXQFUGORDJEST-UHFFFAOYSA-N Sophocarpine Natural products O=C1C=CCC2C3CCCC4CCCC(CN12)C34 IGXQFUGORDJEST-UHFFFAOYSA-N 0.000 description 1
- 240000003968 Sophora davidii Species 0.000 description 1
- 235000007245 Sophora davidii Nutrition 0.000 description 1
- 241000123725 Sophora tonkinensis Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940076810 beta sitosterol Drugs 0.000 description 1
- LGJMUZUPVCAVPU-UHFFFAOYSA-N beta-Sitostanol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CC)C(C)C)C1(C)CC2 LGJMUZUPVCAVPU-UHFFFAOYSA-N 0.000 description 1
- NJKOMDUNNDKEAI-UHFFFAOYSA-N beta-sitosterol Natural products CCC(CCC(C)C1CCC2(C)C3CC=C4CC(O)CCC4C3CCC12C)C(C)C NJKOMDUNNDKEAI-UHFFFAOYSA-N 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- AQASRZOCERRGBL-ROJLCIKYSA-N dauricine Chemical compound CN1CCC2=CC(OC)=C(OC)C=C2[C@H]1CC1=CC=C(O)C(OC2=CC=C(C=C2)C[C@H]2N(C)CCC=3C=C(C(=CC=32)OC)OC)=C1 AQASRZOCERRGBL-ROJLCIKYSA-N 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 229940045109 genistein Drugs 0.000 description 1
- TZBJGXHYKVUXJN-UHFFFAOYSA-N genistein Natural products C1=CC(O)=CC=C1C1=COC2=CC(O)=CC(O)=C2C1=O TZBJGXHYKVUXJN-UHFFFAOYSA-N 0.000 description 1
- 235000006539 genistein Nutrition 0.000 description 1
- ZCOLJUOHXJRHDI-CMWLGVBASA-N genistein 7-O-beta-D-glucoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC(O)=C2C(=O)C(C=3C=CC(O)=CC=3)=COC2=C1 ZCOLJUOHXJRHDI-CMWLGVBASA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002398 materia medica Substances 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 206010039083 rhinitis Diseases 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 1
- 229950005143 sitosterol Drugs 0.000 description 1
- AAGFPTSOPGCENQ-JLNYLFASSA-N sophocarpine Chemical compound C1CC[C@H]2CN3C(=O)C=CC[C@@H]3[C@@H]3[C@H]2N1CCC3 AAGFPTSOPGCENQ-JLNYLFASSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a kind of methods for identifying the subprostrate sophora true and false, and the true and false of the subprostrate sophora medicinal material sample is judged by the content of phenyl benzofurans in measurement subprostrate sophora medicinal material sample.Detection method provided by the invention is accurate and reliable, can effectively eliminate the interference of other impurities in sample, can get satisfied separation detection effect, and this method is easy to operate, easy, at low cost, practical, is very suitable to the detection of product quality.
Description
Technical field
The present invention relates to Materia Medica Identification method fields.It is more particularly related to a kind of identification subprostrate sophora true and false
Method.
Background technique
Subprostrate sophora is the drying root and rhizome of leguminous plant sophora tonkinensis Gapnep, has the effect of clearing heat and detoxicating, relieving sore-throat of reducing swelling, contains
Matrine, oxymatrine, sophocarpine, Dauricine, genistein, β-sitosterol, the ingredients such as flavones, existing " middle traditional Chinese medicines
Allusion quotation " it is fairly simple to subprostrate sophora method of quality control, only using matrine and oxymatrine concentration as evaluation of medical materials' quality
Index, but matrine and oxymatrine are generally existing in leguminous plant hardship beans, kuh-seng, Sophora viciifolia, sandliving sophora seed etc., without
It is subprostrate sophora endemic element, the assay of matrine and oxymatrine is difficult to react quality of medicinal material on the whole.
Phenyl benzofurans be it is isolated in subprostrate sophora for the first time, have prevent and treat very significantly rhinitis cancer at
Point, it is one of the main active of the anti-curing cancers of subprostrate sophora, establishes subprostrate sophora quality by index components of phenyl benzofurans
Control and true and false superiority and inferiority test stone, will preferably reflect subprostrate sophora quality of medicinal material.
Summary of the invention
It is an object of the invention to solve at least the above problems, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide a kind of identification subprostrate sophoras that can more preferably reflect subprostrate sophora medicinal material sample quality
The method of the true and false.
In order to realize these purposes and other advantages according to the present invention, a kind of side for identifying the subprostrate sophora true and false is provided
Method judges the true and false of the subprostrate sophora medicinal material sample by the content of phenyl benzofurans in measurement subprostrate sophora medicinal material sample.
Preferably, when the phenyl benzofurans mass fraction in subprostrate sophora medicinal material sample is not less than 0.04%, mountain beans
Root herb sample is genuine piece；When the phenyl benzofurans mass fraction in subprostrate sophora medicinal material sample is lower than 0.04%, subprostrate sophora
Medicinal material sample is fake and poor products.
Preferably, first the phenyl benzofurans in subprostrate sophora medicinal material sample are extracted and is dissolved, obtain phenyl benzene
And furans sample solution, then measure the content of phenyl benzofurans in subprostrate sophora medicinal material sample.
Preferably, phenyl benzofurans sample solution is measured using liquid chromatography and external standard method, obtains mountain
The content of phenyl benzofurans in beans root herb sample.
Preferably, specific mistake phenyl benzofurans sample solution being measured using liquid chromatography and external standard method
Journey the following steps are included:
Step 1: preparing phenyl benzofurans standard solution；
Step 2: carrying out liquid chromatogram inspection to phenyl benzofurans sample solution and phenyl benzofurans standard solution
It surveys, measures in phenyl benzofurans sample solution benzene in the peak area of phenyl benzofurans and phenyl benzofurans standard solution
The peak area of base benzofuran；
Step 3: the mass fraction X% of phenyl benzofurans in subprostrate sophora medicinal material sample is calculated according to following formula:
Wherein, V is phenyl benzofurans sample solution volume；AsFor phenyl benzo furan in phenyl benzofurans sample solution
The peak area muttered；AsdFor the peak area of phenyl benzofurans in phenyl benzofurans standard solution；C is phenyl benzofurans mark
The concentration of quasi- product solution；M is the quality of subprostrate sophora medicinal material sample.
Preferably, the process phenyl benzofurans in subprostrate sophora medicinal material sample extracted and dissolved are as follows: weigh mountain beans
Root herb sample powder, is added the extractant of 5~20 times of weight of subprostrate sophora medicinal material sample powder, and refluxing extraction 1~2 time, every time 1
~2h, vacuum rotary steam recycle extractant to crude extract is evaporated to obtain, are dissolved in water, cross macroreticular resin, washed with 10~40% ethyl alcohol
60~95% ethanol elutions are used after de- again, collect 60~95% ethanol elution parts, vacuum rotary steam recycling ethyl alcohol is to being evaporated smart
Extract, essence extract add methanol to dissolve constant volume.
Preferably, extractant be mass fraction be 45~100% methanol solution, mass fraction be 45~99.8%
Ethanol solution (when concentration of alcohol is 99.8%, ethanol solution is analytically pure dehydrated alcohol) or mass fraction be 45~
100% acetone soln.
Preferably, extractant is the ethanol solution that mass fraction is 80%.
Preferably, the phenyl benzofurans are 2- (2', 4'- dihydroxy phenyl) -5,6- dioxymethylene benzo furan
It mutters, structural formula is
Preferably, the process phenyl benzofurans in subprostrate sophora medicinal material sample extracted and dissolved are as follows: weigh mountain beans
The extractant of 5~20 times of weight is added in root herb sample powder, and refluxing extraction 1~2 time, 1~2h, vacuum rotary steam recycle every time
Extractant is dissolved in water to crude extract is evaporated to obtain, and crosses macroreticular resin, with after 39% ethanol elution again with 95% ethanol elution,
95% ethanol elution part is collected, vacuum rotary steam recycles ethyl alcohol and adds methanol to dissolve constant volume to essence extract, essence extract is evaporated to obtain.
Preferably, chromatographic column used in liquid chromatographic detection does filler, column temperature with octadecylsilane chemically bonded silica
It is 25~30 DEG C；Detector used in liquid chromatographic detection is ultraviolet detector, the use of wavelength is 205~280nm；Liquid phase color
Sample volume when spectrum detection is 10~20 μ l, flow velocity 1.0ml/min；Liquid chromatographic detection takes gradient elution, wherein acetonitrile
For A phase, water is B phase, and the ratio of acetonitrile changes are as follows: in 0~5min, acetonitrile proportion is 25%；In 5~55min, acetonitrile institute
Accounting example gradually rises up to 50% from 25%；In 55~80min, acetonitrile proportion gradually rises up to 95% from 50%.
The present invention is include at least the following beneficial effects: the present invention is by extracting the main active phenyl benzene in subprostrate sophora
And furans, and the index evaluated using its content as subprostrate sophora quality standard, can precise Identification subprostrate sophora medicinal material the true and false, have
Detection sensitivity and accuracy is higher, repeatable high, simple and easy to do advantage, realizes subprostrate sophora medicinal material and its quality of the pharmaceutical preparations
Stability contorting, for Guangxi subprostrate sophora application and drive the development of ethnic drug to provide theoretical to support with method.This hair
It is bright by linear relationship test, precision test, stability test, repetitive test, sample recovery rate test to this method into
Row verifying, the results showed that detection method provided by the invention is accurate and reliable, can effectively eliminate the interference of other magazines in sample,
It can get satisfied detection effect；And this method is easy to operate, easy, at low cost, practical, is very suitable to product quality
Detection.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Detailed description of the invention
Fig. 1 is the liquid chromatogram of phenyl benzofurans sample solution described in a wherein embodiment of the invention；
Fig. 2 is the liquid chromatogram of phenyl benzofurans standard solution described in a wherein embodiment of the invention；
Fig. 3 is the linear relationship of the present invention test phenyl benzofurans canonical plotting.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples, to enable those skilled in the art's reference
Specification word can be implemented accordingly.
It should be noted that experimental method described in following embodiments is unless otherwise specified conventional method, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained.
<embodiment>
The subprostrate sophora medicinal material sample place of production: Medicinal Plants of Guangxi garden.
The method for identifying the above-mentioned subprostrate sophora true and false, comprising the following steps:
Step 1: weighing subprostrate sophora medicinal material sample powder 2g, the extraction of 20 times of weight of subprostrate sophora medicinal material sample powder is added
Agent refluxing extraction 1 time, extracts duration 2h, and vacuum rotary steam recycles extractant to crude extract is evaporated to obtain, adds 20ml water to dissolve, mistake
Macroreticular resin, with 95% ethanol elution part again with 95% ethanol elution, is collected after 39% ethanol elution, vacuum rotary steam recycles second
Alcohol adds methanol dissolution to be settled to 10ml volumetric flask, obtains phenyl benzofurans sample solution to essence extract, essence extract is evaporated to obtain,
Wherein extractant is the ethanol solution that mass fraction is 80%；
Step 2: weighing phenyl benzofurans monomer, adding methanol dissolution to be configured to concentration is 1.41mg/ml phenyl benzo furan
It mutters standard solution；
Step 3: carrying out liquid chromatogram inspection to phenyl benzofurans sample solution and phenyl benzofurans standard solution
It surveys, wherein the condition of liquid chromatographic detection are as follows:
Chromatographic column: Waters Sunfire-C18 (4.6mm × 250mm, 5 μm)；
Column temperature: 30 DEG C；
Detector: ultraviolet detector uses wavelength 280nm；
Sample volume: 20 μ l；
Flow velocity: 1.0ml/min；
Mobile phase: acetonitrile is mobile phase A, and water is Mobile phase B, carries out gradient elution by table 1:
Table 1
The liquid chromatogram of phenyl benzofurans sample solution as shown in Figure 1, phenyl benzofurans standard solution liquid
Phase chromatogram is as shown in Figure 2.
Step 4: the mass fraction X% of phenyl benzofurans in subprostrate sophora medicinal material sample is calculated according to following formula:
Wherein, V is phenyl benzofurans sample solution volume, unit ml；AsFor in phenyl benzofurans sample solution
The peak area of phenyl benzofurans；AsdFor the peak area of phenyl benzofurans in phenyl benzofurans standard solution；C is phenyl
The concentration of benzofuran standard solution, unit mg/ml；M is the quality of subprostrate sophora medicinal material sample, unit g.The present embodiment
Subprostrate sophora medicinal material sample in phenyl benzofurans mass fraction be 0.082%.
Step 5: when the phenyl benzofurans mass fraction in subprostrate sophora medicinal material sample is not less than 0.04%, subprostrate sophora
Medicinal material sample is genuine piece；When the phenyl benzofurans mass fraction in subprostrate sophora medicinal material sample is lower than 0.04%, subprostrate sophora medicine
Material sample is fake and poor products.According to the above discrimination standard, the subprostrate sophora medicinal material sample of the present embodiment is genuine piece.
Wherein, phenyl benzofurans described in the present embodiment are 2- (2', 4'- dihydroxy phenyl) -5,6- dioxymethylene benzene
And furans.
<linear relationship test>
It is appropriate to weigh phenyl benzofurans monomer, add methanol be configured to solubility be respectively 0.24mg/ml, 0.28mg/ml,
The standard solution of 0.72mg/ml, 0.96mg/ml, 1.2mg/ml, 1.41mg/ml, and according to the liquid chromatogram of above-described embodiment
Testing conditions carry out liquid chromatographic detection to the standard solution of these various concentrations, obtain canonical plotting as shown in figure 3, mark
Ordinate in directrix curve figure is chromatographic peak area, and abscissa is sample volume, and unit is μ g, and standard curve linear equation is y=4
×106X-130105, R2=0.9999.The result shows that phenyl benzofurans standard solution sample volume is in 0.24 μ of μ g~1.44 g
Between when, have good linear relationship between sample volume and peak area.
<precision test>
The phenyl benzofurans standard solution for drawing same concentrations, using liquid chromatographic detection item identical with embodiment
Part repeats sample introduction 6 times, records the liquid chromatogram obtained every time, analyzes the peak area of more each liquid chromatogram, calculates respectively
The relative standard deviation of the peak area of liquid chromatogram is 1.19%, shows that method precision provided by the invention is good.
<stability test>
Draw the phenyl benzofurans standard solution of 6 parts of same concentrations, every part of 1ml, 6 parts of phenyl benzofurans standard items
Solution places 0,1,2,4,8,12h respectively, is measured using liquid chromatographic detection condition identical with embodiment, records 6 parts respectively
The liquid chromatogram of phenyl benzofurans standard solution analyzes the peak area of more each chromatogram, it is inclined to obtain relative standard
Difference is 1.86%, shows that phenyl benzofurans standard solution is stablized in 12h.
<repetitive test>
It weighs with a collection of 6 parts of sample powder, every part of about 1g of subprostrate sophora medicinal material, is detected using method identical with embodiment every
The content of phenyl benzofurans in part sample, and analysis comparison is carried out, obtaining relative standard deviation values is 1.28%, shows that the present invention mentions
The method repeatability of confession is good.
<sample recovery rate test>
6 parts of subprostrate sophora medicinal material samples are weighed, the phenyl benzofurans standard solution that concentration is 1.44mg/ml is separately added into
0.5ml, after being measured using method identical with embodiment, calculating the rate of recovery and obtaining average recovery rate is 99.41%, relatively
Standard deviation is 1.92%, shows that method sample recovery rate provided by the invention is preferable.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (10)
1. the method for identifying the subprostrate sophora true and false, which is characterized in that pass through phenyl benzofurans in measurement subprostrate sophora medicinal material sample
Content judges the true and false of the subprostrate sophora medicinal material sample.
2. the method for the identification subprostrate sophora true and false as described in claim 1, which is characterized in that the benzene in subprostrate sophora medicinal material sample
When base benzofuran mass fraction is not less than 0.04%, subprostrate sophora medicinal material sample is genuine piece；Benzene in subprostrate sophora medicinal material sample
When base benzofuran mass fraction is lower than 0.04%, subprostrate sophora medicinal material sample is fake and poor products.
3. the method for the identification subprostrate sophora true and false as described in claim 1, which is characterized in that first in subprostrate sophora medicinal material sample
Phenyl benzofurans are extracted and are dissolved, and obtain phenyl benzofurans sample solution, then measure benzene in subprostrate sophora medicinal material sample
The content of base benzofuran.
4. the method for the identification subprostrate sophora true and false as claimed in claim 3, which is characterized in that use liquid chromatography and external standard method
Phenyl benzofurans sample solution is measured, the content of phenyl benzofurans in subprostrate sophora medicinal material sample is obtained.
5. the method for the identification subprostrate sophora true and false as claimed in claim 4, which is characterized in that use liquid chromatography and external standard method
The detailed process that be measured to phenyl benzofurans sample solution the following steps are included:
Step 1: preparing phenyl benzofurans standard solution；
Step 2: liquid chromatographic detection is carried out to phenyl benzofurans sample solution and phenyl benzofurans standard solution,
Measure in phenyl benzofurans sample solution phenyl in the peak area of phenyl benzofurans and phenyl benzofurans standard solution
The peak area of benzofuran；
Step 3: the mass fraction X% of phenyl benzofurans in subprostrate sophora medicinal material sample is calculated according to following formula:
Wherein, V is phenyl benzofurans sample solution volume；AsFor phenyl benzofurans in phenyl benzofurans sample solution
Peak area；AsdFor the peak area of phenyl benzofurans in phenyl benzofurans standard solution；C is phenyl benzofurans standard items
The concentration of solution；M is the quality of subprostrate sophora medicinal material sample.
6. the method for the identification subprostrate sophora true and false as claimed in claim 3, which is characterized in that the benzene in subprostrate sophora medicinal material sample
The process that base benzofuran is extracted and dissolved are as follows: weigh subprostrate sophora medicinal material sample powder, be added subprostrate sophora medicinal material sample powder 5~
The extractant of 20 times of weight, refluxing extraction 1~2 time, every time 1~2h, vacuum rotary steam recycles extractant to being evaporated to obtain crude extract,
Be dissolved in water, cross macroreticular resin, with after 10~40% ethanol elutions again use 60~95% ethanol elutions, collection 60~95% ethyl alcohol
Elution fraction, vacuum rotary steam recycle ethyl alcohol and add methanol to dissolve constant volume to essence extract, essence extract is evaporated to obtain.
7. as claimed in claim 6 identification the subprostrate sophora true and false method, which is characterized in that extractant be mass fraction be 45~
The acetone that the ethanol solution or mass fraction that 100% methanol solution, mass fraction are 45~99.8% are 45~100% is molten
Liquid.
8. the method for the identification subprostrate sophora true and false as described in claim 1, which is characterized in that the phenyl benzofurans are 2-
(2', 4'- dihydroxy phenyl) -5,6- dioxymethylene benzofuran.
9. the method for the identification subprostrate sophora true and false as claimed in claim 6, which is characterized in that the benzene in subprostrate sophora medicinal material sample
The process that base benzofuran is extracted and dissolved are as follows: subprostrate sophora medicinal material sample powder is weighed, the extractant of 5~20 times of weight is added,
Refluxing extraction 1~2 time, 1~2h, vacuum rotary steam recycle extractant to crude extract is evaporated to obtain, are dissolved in water every time, cross macropore tree
Rouge, with again with 95% ethanol elution, collecting 95% ethanol elution part after 39% ethanol elution, vacuum rotary steam recycles ethyl alcohol to steaming
It is dry that essence extract, essence extract add methanol to dissolve constant volume.
10. the method for the identification subprostrate sophora true and false as described in claim 4 or 5, which is characterized in that used in liquid chromatographic detection
Chromatographic column does filler with octadecylsilane chemically bonded silica, and column temperature is 25~30 DEG C；Detector used in liquid chromatographic detection
It the use of wavelength is 205~280nm for ultraviolet detector；Sample volume when liquid chromatographic detection is 10~20 μ l, and flow velocity is
1.0ml/min；Liquid chromatographic detection takes gradient elution, wherein acetonitrile is A phase, and water is B phase, and the ratio of acetonitrile changes are as follows:
0~5min, acetonitrile proportion are 25%；In 5~55min, acetonitrile proportion gradually rises up to 50% from 25%；55~
80min, acetonitrile proportion gradually rise up to 95% from 50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811102881.2A CN109030681B (en) | 2018-09-20 | 2018-09-20 | Method for identifying authenticity of subprostrate sophora |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811102881.2A CN109030681B (en) | 2018-09-20 | 2018-09-20 | Method for identifying authenticity of subprostrate sophora |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109030681A true CN109030681A (en) | 2018-12-18 |
| CN109030681B CN109030681B (en) | 2021-10-01 |
Family
ID=64617674
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811102881.2A Active CN109030681B (en) | 2018-09-20 | 2018-09-20 | Method for identifying authenticity of subprostrate sophora |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109030681B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111317741A (en) * | 2020-04-23 | 2020-06-23 | 广西壮族自治区药用植物园 | Traditional Chinese medicine oral preparation for treating nasopharyngeal carcinoma and identification method and application thereof |
| CN112858497A (en) * | 2020-12-31 | 2021-05-28 | 四川新绿色药业科技发展有限公司 | Method for constructing characteristic spectrum of rhizoma Menispermi standard decoction and detecting quality of rhizoma Menispermi standard decoction |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4992204A (en) * | 1989-08-22 | 1991-02-12 | Miliken Research Corporation | Irradiation detection and identification method and compositions useful therein |
| US6184535B1 (en) * | 1997-09-19 | 2001-02-06 | Olympus Optical Co., Ltd. | Method of microscopic observation |
| CN1606551A (en) * | 2001-12-18 | 2005-04-13 | 惠氏公司 | Substituted 2-phenyl benzofurans as estrogenic agents |
| CN103690595A (en) * | 2013-01-07 | 2014-04-02 | 中国医学科学院药用植物研究所 | Ethyl acetate extract of radix sophorae tonkinensis, as well as preparation method, detection method and application thereof |
| CN103724306A (en) * | 2014-01-24 | 2014-04-16 | 温州大学 | Preparation method of benzofuran derivative |
-
2018
- 2018-09-20 CN CN201811102881.2A patent/CN109030681B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4992204A (en) * | 1989-08-22 | 1991-02-12 | Miliken Research Corporation | Irradiation detection and identification method and compositions useful therein |
| US6184535B1 (en) * | 1997-09-19 | 2001-02-06 | Olympus Optical Co., Ltd. | Method of microscopic observation |
| CN1606551A (en) * | 2001-12-18 | 2005-04-13 | 惠氏公司 | Substituted 2-phenyl benzofurans as estrogenic agents |
| CN103690595A (en) * | 2013-01-07 | 2014-04-02 | 中国医学科学院药用植物研究所 | Ethyl acetate extract of radix sophorae tonkinensis, as well as preparation method, detection method and application thereof |
| CN103724306A (en) * | 2014-01-24 | 2014-04-16 | 温州大学 | Preparation method of benzofuran derivative |
Non-Patent Citations (2)
| Title |
|---|
| LUO,GUOYONG 等: "Novel 2-arylbenzofuran dimers and polyisoprenylated flavanones from Sophora tonkinensis", 《FITOTERAPIA》 * |
| 刘吉成 等: "广西多叶越南槐HPLC指纹图谱的建立及与山豆根HPLC指纹图谱一致性比较研究", 《中国实验方剂学杂志》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111317741A (en) * | 2020-04-23 | 2020-06-23 | 广西壮族自治区药用植物园 | Traditional Chinese medicine oral preparation for treating nasopharyngeal carcinoma and identification method and application thereof |
| CN112858497A (en) * | 2020-12-31 | 2021-05-28 | 四川新绿色药业科技发展有限公司 | Method for constructing characteristic spectrum of rhizoma Menispermi standard decoction and detecting quality of rhizoma Menispermi standard decoction |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109030681B (en) | 2021-10-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108717095A (en) | The detection method and discriminating, content assaying method of the drug of a kind of loguat leaf or the leaf raw material containing loquat | |
| CN103487516B (en) | A kind of assay method of Chinese medicinal composition preparation finger-print | |
| CN105842373A (en) | Method for establishing fingerprint of flos lonicerae medicinal preparation | |
| CN101419200B (en) | HPLC fingerprint identification method for origin ginseng protection | |
| CN106093262A (en) | A kind of method of the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae | |
| CN109030681A (en) | The method for identifying the subprostrate sophora true and false | |
| CN103197026A (en) | Quality control method of granules capable of strengthening and consolidating body resistance | |
| CN102335402A (en) | Detection method of Chinese preparation mixture for invigorating the spleen and replenishing qi | |
| CN100437112C (en) | Method for inspecting Chinese medicinal preparation quality in treatment of old man eyes dieases | |
| CN106753798A (en) | Cortex Cinnamomi volatile oil extraction by steam distillation technique | |
| CN104330482B (en) | A kind of HPLC of utilization measures the method for 17 kinds of characteristic components in Folium Camelliae sinensis simultaneously | |
| CN102435689A (en) | Determination method of UPLC-MS (ultrahigh performance liquid chromatography-mass spectrometry) fingerprint of Radix Scutellariae medicinal material | |
| CN102139039B (en) | Quality control method of coptis tablet for clearing away stomach heat | |
| CN109030694A (en) | The method of the finger-print identification subprostrate sophora true and false | |
| CN103822888B (en) | Catch up with the quality determining method of yellow grass | |
| CN103472148A (en) | Fingerprint spectrum detection method of Chinese medicine composition preparation | |
| CN104013673B (en) | A kind of Salvia root P.E and preparation method thereof | |
| CN103575821A (en) | Detection method of 14 chemical components in Tangminling preparation | |
| CN104678004A (en) | Quality control method for kudzuvine root and hawthorn lipid-lowering particles | |
| CN101703583B (en) | Quality detection method of Xinning capsules | |
| CN109115927B (en) | Quality detection and identification method for scalded rhizoma drynariae and rhizoma drynariae preparation | |
| CN103713067B (en) | Ultra-high performance liquid chromatography method for determining content of rheum lhasaense | |
| CN103293261A (en) | Content determination method of rhizoma bletillae | |
| CN113759057B (en) | Characteristic spectrum of allium macrostemon white water extract and preparation thereof and construction method thereof | |
| CN101816753A (en) | Method for detecting quality of compound preparation for treating cold |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Miao Jianhua Inventor after: Song Zhijun Inventor after: Yao Caiyun Inventor after: Yan Bingxiong Inventor after: Li Qiuping Inventor after: Ou Chunli Inventor before: Miao Jianhua Inventor before: Song Zhijun Inventor before: Yan Bingxiong Inventor before: Li Qiuping Inventor before: Ou Chunli |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20181218 Assignee: Pubei County Hongwei Nut Planting Co.,Ltd. Assignor: GUANGXI BOTANICAL GARDEN OF MEDICINAL PLANTS Contract record no.: X2023980046052 Denomination of invention: Method for identifying the authenticity of Shandou root Granted publication date: 20211001 License type: Common License Record date: 20231108 |