CN110133172A - The thin layer for joining rhizoma atractylodis, nutmeg and red ginseng in times Guchang capsule identifies measuring method - Google Patents
The thin layer for joining rhizoma atractylodis, nutmeg and red ginseng in times Guchang capsule identifies measuring method Download PDFInfo
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- CN110133172A CN110133172A CN201910507806.2A CN201910507806A CN110133172A CN 110133172 A CN110133172 A CN 110133172A CN 201910507806 A CN201910507806 A CN 201910507806A CN 110133172 A CN110133172 A CN 110133172A
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- 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
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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- 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
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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Abstract
The present invention relates to effective ingredient technical fields, identify measuring method more particularly to the thin layer for being rhizoma atractylodis, nutmeg and red ginseng in a seed ginseng times Guchang capsule, including rhizoma atractylodis thin layer identifies measuring method, nutmeg thin layer identifies measuring method and red ginseng thin layer identifies measuring method.Pass through the characteristic for each drug ingedient in ginseng times Guchang capsule, the thin layer identification based on rhizoma atractylodis, nutmeg and red ginseng is specific again, adaptable extraction and preparation technique is provided, so as to the separation and Extraction ingredient to be determined from many active drug ingredients of ginseng times Guchang capsule.It solves existing thin layer and identifies that measuring method is more difficult to extract drug target to be determined from ginseng times Guchang capsule, while being influenced by drug target is volatile, the more difficult problem of final colour developing.
Description
Technical field
The present invention relates to effective ingredient technical fields, and in particular to be ginseng times Guchang capsule in rhizoma atractylodis, nutmeg and
The thin layer of red ginseng identifies measuring method.
Background technique
Ginseng times Guchang capsule is a kind of common Chinese patent drug, wherein including Chinese gall, nutmeg (stewing), terminalia flesh (stewing), crow
Plum, radix aucklandiae, rhizoma atractylodis, Poria cocos, cornu cerve degelatinatum, red ginseng have intestine-stabling and anti-diarrheal, the effect of invigorating the spleen warm kidney.Caused by because of the insufficiency of both the spleen and the kindey
Chronic diarrhea, abdominal pain, limbs burnout, spiritlessness and sparing of words, shape trembles with fear limb cold, deficiency of food, soreness and weakness of waist and knees；Irritable bowel syndrome (diarrhea-type)
See above-mentioned disease person.
It needs to identify measuring method by thin layer to wherein rhizoma atractylodis, nutmeg and red ginseng in effective ingredient analysis and carry out
Identification, but it is more due to joining each Ingredients Weight in times Guchang capsule, and rhizoma atractylodis, nutmeg etc. contain volatile oil, existing routine
Thin layer identify that measuring method is more difficult to extract drug to be determined from ginseng times Guchang capsule, while being influenced by volatile, colour developing is relatively tired
It is difficult.
Summary of the invention
The present invention extracts drug target to be determined from ginseng times Guchang capsule for conventional thin layer identification measuring method is more difficult,
It is influenced simultaneously by drug target is volatile, the more difficult problem of final colour developing provides rhizoma atractylodis, meat in a seed ginseng times Guchang capsule
The thin layer of cardamom and red ginseng identifies measuring method.
The present invention solves above-mentioned technical problem, the technical solution adopted is that, rhizoma atractylodis, nutmeg in a seed ginseng times Guchang capsule
Identify measuring method with the thin layer of red ginseng, including rhizoma atractylodis thin layer identifies measuring method, nutmeg thin layer identifies measuring method and red ginseng
Thin layer identifies measuring method.
Further, it includes the preparation of control group reagent, the preparation of measurement group reagent and thin layer that rhizoma atractylodis thin layer, which identifies measuring method,
Identify measurement, control group reagent preparation the following steps are included:
S1 takes rhizoma atractylodis, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and volatilizes to filtrate, and residue is made；
S3, reagent is extracted in addition in residue, so that residue dissolves, control group reagent is made；
Measure group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and volatilizes to filtrate, and residue is made；
S3, reagent is extracted in addition in residue, so that residue dissolves, measurement group reagent is made；
Thin layer identify measurement the following steps are included:
S1 takes control group reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and by solvent into
Row expansion；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, heating；
S3 after being heated to adaptive temperature, in control group reagent chromatography and the measurement corresponding position of group reagent chromatography, is obtained
Show the fluorescence spot of identical color.
Further, rhizoma atractylodis thin layer identifies in the control group reagent preparation step of measuring method, extracts reagent in S1 and S3
It is 60 DEG C~90 DEG C of boiling range specification of petroleum ether, measures in group reagent preparation step, it is boiling range that reagent is extracted in S1 and S3
The petroleum ether that 60 DEG C~90 DEG C of specification, thin layer identify in determination step, the petroleum that S1 solvent is 60 DEG C~90 DEG C of boiling range specification
Ether, S2 developing agents are anisaldehyde test solution.
Optionally, rhizoma atractylodis thin layer identifies in the control group reagent preparation step of measuring method, and S1 rhizoma atractylodis take 0.5g, and addition mentions
Taking reagent is 15mL, and it is 1mL that reagent is extracted in S2 ultrasonication 20min, S3 addition, is measured in group reagent preparation step, S1 is grey
Art takes 5g, and it is 15mL that reagent is extracted in addition, and it is 1mL that reagent is extracted in S2 ultrasonication 20min, S3 addition, and thin layer identifies measurement
In step, it is 105 DEG C that S1, which takes control 2 μ L of group reagent, measurement 10 μ L, S3 heating temperature of group reagent,.
Further, nutmeg thin layer identification measuring method includes that prepared by control group reagent, prepared by measurement group reagent and thin
Layer identify measurement, control group reagent preparation the following steps are included:
S1 takes nutmeg, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and collects filtrate and control group reagent is made；
Measure group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and collects filtrate and measurement group reagent is made；
Thin layer identify measurement the following steps are included:
S1 takes control group reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and by solvent into
Row expansion；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, heating；
S3 after being heated to adaptive temperature, in control group reagent chromatography and the measurement corresponding position of group reagent chromatography, is obtained
Show the fluorescence spot of identical color.
Optionally, nutmeg thin layer identifies in the control group reagent preparation step of measuring method, and it is three that reagent is extracted in S1
Chloromethanes measures in group reagent preparation step, and it is chloroform that reagent is extracted in S1, and thin layer identifies in determination step, S1 expansion
Agent be 9:1 according to volume ratio 60 DEG C~90 DEG C petroleum ethers of boiling range specification and ethyl acetate mixed solvent, S2 developing agents be
10% ethanol solution of sulfuric acid.
Optionally, nutmeg thin layer identifies in the control group reagent preparation step of measuring method, and nutmeg takes 0.5g in S1,
It is 10mL, S2 ultrasonication 20min that reagent is extracted in addition, is measured in group reagent preparation step, joins a times Guchang capsule in S1 and takes
5g, addition extract reagent as 15mL, and S2 ultrasonication 20min, thin layer identifies in determination step, and S1 takes control 10 μ of group reagent
L, measurement 10 μ L, S3 heating temperature of group reagent is 105 DEG C.
Further, it includes the preparation of control group reagent, the preparation of measurement group reagent and thin layer that red ginseng thin layer, which identifies measuring method,
Identify measurement, control group reagent preparation the following steps are included:
S1 takes ginsenoside Rb1, ginsenoside Re, ginsenoside Rg1, extraction reagent is set in Soxhlet extractor and adds,
Heating extracts, and reference substance extracting solution is made, takes red ginseng to set in Soxhlet extractor and adds extraction reagent, and heating is mentioned
It takes, control medicinal material extracting solution is made；
S2 volatilizes the solution of reference substance extracting solution in S1, and adds reflux reagent, and after being heated to reflux, filtering, filtrate is steamed
It is dry, reference substance residue is made；The solution of control medicinal material extracting solution in S1 is volatilized, and adds reflux reagent, after being heated to reflux, mistake
Filter, filtrate are evaporated, and control medicinal material residue is made；
S3 adds solvent in reference substance residue, after to be dissolved, extracts, then alkali cleaning, extracts again after alkali cleaning, system
Reference substance reagent is obtained, solvent is added in control medicinal material residue, after to be dissolved, extracts, then alkali cleaning, is mentioned again after alkali cleaning
It takes, control medicinal material reagent is made；
Measure group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule, sets in Soxhlet extractor and add extraction reagent, heating extracts；
S2, solution volatilizes after S1 is extracted, and adds reflux reagent, and after being heated to reflux, filtering, filtrate is evaporated, and is made residual
Slag；
S3 adds solvent in residue, after to be dissolved, extracts, then alkali cleaning, extracts again after alkali cleaning, and measurement is made
Group reagent；
Thin layer identify measurement the following steps are included:
S1 takes reference substance reagent, control medicinal material reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and
It is unfolded by solvent；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, heating；
S3, after being heated to adaptive temperature, in reference substance reagent chromatography, control medicinal material reagent chromatography and measurement group reagent chromatography
On corresponding position, it is respectively placed under daylight and ultraviolet lamp and inspects, obtain the fluorescence spot for showing identical color.
Optionally, red ginseng thin layer identifies in the control group reagent preparation step of measuring method, and reference substance is used to prepare in S1
The extraction reagent of extracting solution is methanol, and the extraction reagent for being used to prepare control medicinal material extracting solution is ether, and reflux reagent is in S2
Methanol, solvent is the water of n-butanol saturation in S3, is measured in group reagent preparation step, and it is ether that reagent is extracted in S1, in S2
Reflux reagent is methanol, and solvent is the water of n-butanol saturation in S3, and thin layer identifies in determination step, and solvent is at 10 DEG C in S1
Environment temperature under be 65:35:10 according to volume ratio chloroform-methanol-water lower layer solution, developing agents are in S2
10% ethanol solution of sulfuric acid.
Optionally, red ginseng thin layer identifies in the control group reagent preparation step of measuring method, and ginsenoside Rb is taken in S11、
Ginsenoside Re, ginsenoside Rg1Each 1mg, it is 1mL that reagent is extracted in addition, heats 3h, and reflux reagent is 150mL, heating in S2
Return time is 3h, adds the water 30mL of n-butanol saturation to make to dissolve in reference substance residue in S3, is transferred in separatory funnel, uses
Water saturated n-butanol extracts 3 times, and each 40ml, combination system obtains n-butanol extracting liquid, is washed 2 times with 1% sodium hydroxide solution,
50mL is wherein used for the first time, and second uses 30mL, and the n-butanol 50ml that lye is saturated with water is extracted 1 time, discards lye, and above-mentioned
N-butanol extracting liquid merges, then is washed to neutrality with what n-butanol was saturated, discards water lotion, to doing, residue adds recycling n-butanol
Methanol 2ml makes to dissolve, and reference substance reagent is made；
Red ginseng 1g is taken in S1, it is 80mL that reagent is extracted in addition, heats 3h, reflux reagent is 150mL in S2, when being heated to reflux
Between be 3h, in S3 in control medicinal material residue plus the water 30mL of n-butanol saturation makes to dissolve, be transferred in separatory funnel, it is full with water
The n-butanol of sum extracts 3 times, and each 40ml, combination system obtains n-butanol extracting liquid, is washed 2 times with 1% sodium hydroxide solution, wherein
50mL is used for the first time, uses 30mL for the second time, and the n-butanol 50ml that lye is saturated with water is extracted 1 time, lye is discarded, with above-mentioned positive fourth
Alcohol extract merges, then is washed to neutrality with what n-butanol was saturated, discards water lotion, for recycling n-butanol to doing, residue adds methanol
2ml makes to dissolve, and control medicinal material reagent is made；
It measuring in group reagent preparation step, ginseng times Guchang capsule 12g is taken in S1, it is 80mL that reagent is extracted in addition, 3h is heated,
The reagent that flows back in S2 is 150mL, and being heated to reflux the time is 3h, adds the water 30mL of n-butanol saturation to make to dissolve in residue in S3,
It is transferred in separatory funnel, the n-butanol being saturated with water extracts 3 times, and each 40ml, combination system obtains n-butanol extracting liquid, with 1%
Sodium hydroxide solution washs 2 times, wherein using 50mL for the first time, uses 30mL, the n-butanol 50ml that lye is saturated with water to mention for the second time
It takes 1 time, discards lye, merge with above-mentioned n-butanol extracting liquid, then be washed to neutrality with what n-butanol was saturated, discard water lotion,
N-butanol is recycled to doing, residue adds methanol 2ml to make to dissolve, and measurement group reagent is made；
Thin layer identifies in determination step, and measurement 10 μ L of group reagent is taken in S1, takes reference substance reagent and control medicinal material reagent each 2
μ L, S3 heating temperature is 105 DEG C.
Beneficial effects of the present invention include at least following one；
1, by the characteristic for each drug ingedient in ginseng times Guchang capsule, then based on the thin of rhizoma atractylodis, nutmeg and red ginseng
Layer identification feature, adaptable extraction and preparation technique and required preparation are provided, so as to from ginseng times Guchang capsule it is many
Separation and Extraction ingredient to be determined in active drug ingredient.
2, it solves existing thin layer and identifies that measuring method is more difficult to extract drug target to be determined from ginseng times Guchang capsule, together
When influenced by drug target is volatile, the more difficult problem of final colour developing.
Detailed description of the invention
Fig. 1 is that measurement chart is unfolded in rhizoma atractylodis specificity；
Measurement chart is unfolded from making sheet for rhizoma atractylodis durability silica G in Fig. 2；
Fig. 3 is that measurement chart is unfolded in rhizoma atractylodis durability silica G prefabricated board；
Fig. 4 is that measurement chart is unfolded in nutmeg specificity；
Measurement chart is unfolded from making sheet for nutmeg durability silica G in Fig. 5；
Fig. 6 is that measurement chart is unfolded in nutmeg durability silica G prefabricated board；
Fig. 7 is to inspect expansion measurement chart under red ginseng specificity daylight；
Fig. 8 is to inspect expansion measurement chart under red ginseng specificity ultraviolet lamp (365nm)；
Measurement chart is unfolded from making sheet for silica G under red ginseng durability daylight in Fig. 9；
Measurement chart is unfolded from making sheet for silica G under red ginseng durability ultraviolet lamp (365nm) in Figure 10；
Figure 11 is that measurement chart is unfolded in silica G prefabricated board under red ginseng durability daylight；
Figure 12 is that measurement chart is unfolded in silica G prefabricated board under red ginseng durability ultraviolet lamp (365nm)；
Specific embodiment
It is clear in order to enable the objectives, technical solutions, and advantages of the present invention to be more clear, with reference to embodiments to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting present invention protection content.
Embodiment 1
The thin layer for joining rhizoma atractylodis, nutmeg and red ginseng in times Guchang capsule identifies measuring method, including rhizoma atractylodis thin layer identifies measurement
Method, nutmeg thin layer identify measuring method and red ginseng thin layer identifies measuring method, and wherein rhizoma atractylodis thin layer identifies measuring method packet
Include control group reagent preparation, measurement group reagent preparation and thin layer identify measurement, control group reagent preparation the following steps are included:
S1 takes rhizoma atractylodis, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and volatilizes to filtrate, and residue is made；
S3, reagent is extracted in addition in residue, so that residue dissolves, control group reagent is made；
Measure group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and volatilizes to filtrate, and residue is made；
S3, reagent is extracted in addition in residue, so that residue dissolves, measurement group reagent is made；
Thin layer identify measurement the following steps are included:
S1 takes control group reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and by solvent into
Row expansion；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, heating；
S3 after being heated to adaptive temperature, in control group reagent chromatography and the measurement corresponding position of group reagent chromatography, is obtained
Show the fluorescence spot of identical color.
It includes that the preparation of control group reagent, the preparation of measurement group reagent and thin layer identify that wherein nutmeg thin layer, which identifies measuring method,
Measurement, control group reagent preparation the following steps are included:
S1 takes nutmeg, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and collects filtrate and control group reagent is made；
Measure group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and collects filtrate and measurement group reagent is made；
Thin layer identify measurement the following steps are included:
S1 takes control group reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and by solvent into
Row expansion；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, heating；
S3 after being heated to adaptive temperature, in control group reagent chromatography and the measurement corresponding position of group reagent chromatography, is obtained
Show the fluorescence spot of identical color.
It includes compareing group reagent preparation, the preparation of measurement group reagent and thin layer to identify survey that wherein red ginseng thin layer, which identifies measuring method,
It is fixed, the preparation of control group reagent the following steps are included:
S1 takes ginsenoside Rb1, ginsenoside Re, ginsenoside Rg1, extraction reagent is set in Soxhlet extractor and adds,
Heating extracts, and reference substance extracting solution is made, takes red ginseng to set in Soxhlet extractor and adds extraction reagent, and heating is mentioned
It takes, control medicinal material extracting solution is made；
S2 volatilizes the solution of reference substance extracting solution in S1, and adds reflux reagent, and after being heated to reflux, filtering, filtrate is steamed
It is dry, reference substance residue is made；The solution of control medicinal material extracting solution in S1 is volatilized, and adds reflux reagent, after being heated to reflux, mistake
Filter, filtrate are evaporated, and control medicinal material residue is made；
S3 adds solvent in reference substance residue, after to be dissolved, extracts, then alkali cleaning, extracts again after alkali cleaning, system
Reference substance reagent is obtained, solvent is added in control medicinal material residue, after to be dissolved, extracts, then alkali cleaning, is mentioned again after alkali cleaning
It takes, control medicinal material reagent is made；
Measure group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule, sets in Soxhlet extractor and add extraction reagent, heating extracts；
S2, solution volatilizes after S1 is extracted, and adds reflux reagent, and after being heated to reflux, filtering, filtrate is evaporated, and is made residual
Slag；
S3 adds solvent in residue, after to be dissolved, extracts, then alkali cleaning, extracts again after alkali cleaning, and measurement is made
Group reagent；
Thin layer identify measurement the following steps are included:
S1 takes reference substance reagent, control medicinal material reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and
It is unfolded by solvent；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, heating；
S3, after being heated to adaptive temperature, in reference substance reagent chromatography, control medicinal material reagent chromatography and measurement group reagent chromatography
On corresponding position, it is respectively placed under daylight and ultraviolet lamp and inspects, obtain the fluorescence spot for showing identical color.
Pass through the characteristic for each drug ingedient in ginseng times Guchang capsule, then the thin layer based on rhizoma atractylodis, nutmeg and red ginseng
It identifies specific, adaptable extraction and preparation technique is provided, so as to from many active drug ingredients of ginseng times Guchang capsule
Separation and Extraction ingredient to be determined.It solves existing thin layer and identifies that measuring method is more difficult to extract mesh to be determined from ginseng times Guchang capsule
Drug is marked, while being influenced by drug target is volatile, the more difficult problem of final colour developing.
Embodiment 2
The thin layer for joining rhizoma atractylodis, nutmeg and red ginseng in times Guchang capsule identifies measuring method, including rhizoma atractylodis thin layer identifies measurement
Method, nutmeg thin layer identify measuring method and red ginseng thin layer identifies measuring method, and wherein rhizoma atractylodis thin layer identifies measuring method packet
Include control group reagent preparation, measurement group reagent preparation and thin layer identify measurement, control group reagent preparation the following steps are included:
S1 takes rhizoma atractylodis 0.5g, its is finely ground, sets in stuffed conical flask and add 60 DEG C~90 DEG C of 15mL boiling range specification of stone
Oily ether, extracts；
S2, solution carries out ultrasonication 20min after S1 is extracted, and filters, and volatilizes to filtrate, and residue is made；
S3 adds 60 DEG C~90 DEG C of 1mL boiling range specification of petroleum ether in residue, so that residue dissolves, control group is made
Reagent；
Measure group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule 5g, its is finely ground, sets in stuffed conical flask and adds 15mL boiling range specification 60 DEG C~90
DEG C petroleum ether, extract；
S2, solution carries out ultrasonication 20min after S1 is extracted, and filters, and volatilizes to filtrate, and residue is made；
S3 adds 60 DEG C~90 DEG C of 1mL boiling range specification of petroleum ether in residue, so that residue dissolves, measurement group is made
Reagent；
Thin layer identify measurement the following steps are included:
S1 takes control 2 μ L of group reagent and measurement 10 μ L of group reagent, is put respectively on same silica gel g thin-layer plate, and pass through boiling
The petroleum ether that 60 DEG C~90 DEG C of journey specification is unfolded；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with anisaldehyde, heating；
S3 after being heated to 105 DEG C, in control group reagent chromatography and the measurement corresponding position of group reagent chromatography, is shown
Show the fluorescence spot of identical color.
It includes that the preparation of control group reagent, the preparation of measurement group reagent and thin layer identify that wherein nutmeg thin layer, which identifies measuring method,
Measurement, control group reagent preparation the following steps are included:
S1 takes nutmeg 0.5g, its is finely ground, sets in stuffed conical flask and adds 10mL chloroform, extract；
S2, solution carries out ultrasonication 20min after S1 is extracted, and filters, and collects filtrate and control group reagent is made；
Measure group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule 5g, its is finely ground, sets in stuffed conical flask and adds 10mL chloroform, mentioned
It takes；
S2, solution carries out ultrasonication 20min after S1 is extracted, and filters, and collects filtrate and measurement group reagent is made；
Thin layer identify measurement the following steps are included:
S1 takes control group reagent and measurement each 10 μ L of group reagent, is put respectively on same silica gel g thin-layer plate, and by pressing
It is unfolded according to 60 DEG C~90 DEG C petroleum ethers of boiling range specification and ethyl acetate mixed solvent that volume ratio is 9:1；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with 10% ethanol solution of sulfuric acid, heating；
S3 after being heated to 105 DEG C, in control group reagent chromatography and the measurement corresponding position of group reagent chromatography, is shown
Show the fluorescence spot of identical color.
It includes compareing group reagent preparation, the preparation of measurement group reagent and thin layer to identify survey that wherein red ginseng thin layer, which identifies measuring method,
It is fixed, the preparation of control group reagent the following steps are included:
S1 takes ginsenoside Rb1, ginsenoside Re, ginsenoside Rg1Each 1mg sets in Soxhlet extractor and adds 1mL first
Alcohol, heating extract for 3 hours, and reference substance extracting solution is made, takes red ginseng 1g to set in Soxhlet extractor and adds 80mL ether, add
Heat extracts for 3 hours, and control medicinal material extracting solution is made；
S2 volatilizes the solution of reference substance extracting solution in S1, and adds 150mL methanol, after being heated to reflux 3 hours, filtering,
Filtrate is evaporated, and reference substance residue is made；The solution of control medicinal material extracting solution in S1 is volatilized, and adds 150mL methanol, is heated back
After 3 hours, filtering, filtrate is evaporated stream, and control medicinal material residue is made；
S3, in reference substance residue plus the water 30mL of n-butanol saturation makes to dissolve, and is transferred in separatory funnel, is saturated with water
N-butanol extract 3 times, each 40ml, combination system obtains n-butanol extracting liquid, is washed 2 times with 1% sodium hydroxide solution, wherein the
50mL is once used, uses 30mL for the second time, the n-butanol 50ml that lye is saturated with water is extracted 1 time, lye is discarded, with above-mentioned n-butanol
Extracting solution merges, then is washed to neutrality with what n-butanol was saturated, discards water lotion, for recycling n-butanol to doing, residue adds methanol 2ml
Make to dissolve, reference substance reagent is made, in control medicinal material residue plus the water 30mL of n-butanol saturation makes to dissolve, and is transferred to liquid separation leakage
In bucket, the n-butanol being saturated with water is extracted 3 times, and each 40ml, combination system obtains n-butanol extracting liquid, with 1% sodium hydroxide solution
Washing 2 times uses 30mL wherein using 50mL for the first time for the second time, and the n-butanol 50ml that lye is saturated with water is extracted 1 time, discards alkali
Liquid merges with above-mentioned n-butanol extracting liquid, then is washed to neutrality with what n-butanol was saturated, discards water lotion, recycling n-butanol is extremely
Dry, residue adds methanol 2ml to make to dissolve, and control medicinal material reagent is made；
Measure group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule 12g, sets in Soxhlet extractor and add 80mL ether, and heating extracts for 3 hours；
S2, solution volatilizes ether after S1 is extracted, and adds 150mL methanol, and after being heated to reflux 3 hours, filtering, filtrate is steamed
It is dry, residue is made；
S3, in residue plus the water 30mL of n-butanol saturation makes to dissolve, and is transferred in separatory funnel, the positive fourth being saturated with water
Alcohol extracting 3 times, each 40ml, combination system obtains n-butanol extracting liquid, is washed 2 times with 1% sodium hydroxide solution, wherein using for the first time
50mL uses 30mL for the second time, and the n-butanol 50ml that lye is saturated with water is extracted 1 time, lye is discarded, with above-mentioned n-butanol extracting liquid
Merge, then be washed to neutrality with what n-butanol was saturated, discards water lotion, for recycling n-butanol to doing, it is molten that residue adds methanol 2ml to make
Measurement group reagent is made in solution；
Thin layer identify measurement the following steps are included:
S1 takes 2 μ L of reference substance reagent, 2 μ L of control medicinal material reagent and measurement 10 μ L of group reagent, is put respectively in same silica G
On lamellae, and by molten according to chloroform-methanol-water lower layer that volume ratio is 65:35:10 under 10 DEG C of environment temperature
Liquid is unfolded；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with 10% sulfuric acid ethyl alcohol, heating；
S3, after being heated to 105 DEG C, in reference substance reagent chromatography, control medicinal material reagent chromatography and measurement group reagent chromatography phase
On the position answered, it is respectively placed under daylight and ultraviolet lamp (365nm) and inspects, obtain the fluorescence spot for showing identical color.
Embodiment 3
In order to ensure effect of the invention, applicant carries out the discrimination method of rhizoma atractylodis, nutmeg and red ginseng in preparation
Corresponding experimental study and demonstration, specific as follows:
Rhizoma atractylodis thin layer identifies measuring method
(1) reagent and reagent
A ginseng times Guchang capsule is provided by Liansheng Pharmaceutical Co., Ltd., Guizhou；Rhizoma atractylodis control medicinal material (120932-201006) by
Nat'l Pharmaceutical & Biological Products Control Institute provides；Silica gel g thin-layer plate: subsidiary factory, Haiyang Chemical Plant, Qingdao production silica gel g thin-layer plate and
Make silica gel g thin-layer plate by oneself；Reagent: (60 DEG C~90 DEG C) of petroleum ether pure to analyze.
Ten batches of sample assay results
(2) specificity
It takes ginseng times Guchang capsule, lack rhizoma atractylodis negative sample, measurement group reagent and control group examination is made with 2 method of embodiment
Agent, then group reagent (being free of ingredient agent to be detected) is measured by prior art preparation feminine gender, measurement group reagent, feminine gender are taken respectively
Group reagent, control group reagent point sample, expansion, colour developing are measured, inspects under daylight, in measurement group reagent chromatography, is tried with control group
Identical principal spot is shown on the corresponding position of agent chromatography, spot separation is preferable, and negative noiseless.
(3) durability
It takes that measurement group reagent, negative measurement group reagent is made and compares group reagent by above-mentioned 10 batches of samples and puts respectively in silicon
Glue G prefabricated board and silica G are from after making sheet, expansion, colour developing, and as a result spot separator well, noiseless.
The following contents is obtained after measuring according to the technical solution provided in embodiment 2:
Carrier is silica G plate in Fig. 1, and the petroleum ether that solvent is 60 DEG C~90 DEG C of boiling range specification develops the color to spray with fennel
Aldehyde test solution, 105 DEG C to be heated to spot development clear, inspects under daylight.
Wherein corresponding 1511010 sample lots of label 1 measure group reagent, 2 corresponding 1512010 sample lots measurement groups examinations
Agent, 3 corresponding 1512020 sample lots measure group reagent, 4 corresponding negative samples, and 5 corresponding rhizoma atractylodis compare group reagent.
In Fig. 2 and Fig. 3, only carrier is had differences, and Fig. 2 carrier is silica G from making sheet, and Fig. 3 carrier silica gel G prefabricated board is opened up
The petroleum ether that agent is 60 DEG C~90 DEG C of boiling range specification is opened, is developed the color to spray with anisaldehyde test solution, 105 DEG C to be heated to spot development clear
It is clear, it is inspected under daylight.
Wherein corresponding 1511010 sample lots of label 1 measure group reagent, 2 corresponding 1512010 sample lots measurement groups
Reagent, 3 corresponding 1512020 sample lots measure group reagent, and 4 correspond to negative sample, and 5 correspond to rhizoma atractylodis control group reagent.
Nutmeg thin layer identifies measuring method
(1) reagent and reagent
A ginseng times Guchang capsule is provided by Liansheng Pharmaceutical Co., Ltd., Guizhou；Nutmeg control medicinal material (120926-201307)
It is provided by Nat'l Pharmaceutical & Biological Products Control Institute；Silica gel g thin-layer plate: the silica gel g thin-layer plate of subsidiary factory, Haiyang Chemical Plant, Qingdao production
And self-control silica gel g thin-layer plate；Reagent: petroleum ether (60 DEG C~90 DEG C), chloroform and ethyl acetate are that analysis is pure.
Ten batches of sample assay results
(2) specificity
Ginseng times Guchang capsule, misrun cardamom negative sample are taken, measurement group reagent and control group examination is made with 2 method of embodiment
Agent, then group reagent (being free of ingredient agent to be detected) is measured by prior art preparation feminine gender, measurement group reagent, feminine gender are taken respectively
Group reagent, control group reagent point sample, expansion, colour developing are measured, inspects under daylight, in measurement group reagent chromatography, is tried with control group
Identical principal spot is shown on the corresponding position of agent chromatography, spot separation is preferable, and negative noiseless.
(3) durability
It takes that measurement group reagent, negative measurement group reagent is made and compares group reagent by above-mentioned 10 batches of samples and puts respectively in silicon
Glue G prefabricated board and silica G are from after making sheet, expansion, colour developing, and as a result spot separator well, noiseless.
The following contents is obtained after measuring according to the technical solution provided in embodiment 2:
Carrier is silica G plate in Fig. 4, and solvent is 60 DEG C~90 DEG C petroleum of boiling range specification for being 9:1 according to volume ratio
Ether and ethyl acetate mixed solvent develop the color to spray with 10% ethanol solution of sulfuric acid, 105 DEG C of clear, daylight that are heated to spot development
Under inspect.
Wherein corresponding 1511010 sample lots of label 1 measure group reagent, 2 corresponding 1512010 sample lots measurement groups examinations
Agent, 3 corresponding 1512020 sample lots measure group reagent, 4 corresponding negative samples, and 5 corresponding nutmegs compare group reagent.
In Fig. 5 and Fig. 6, only carrier is had differences, and Fig. 5 carrier is silica G from making sheet, and Fig. 6 carrier silica gel G prefabricated board is opened up
Opening agent is 60 DEG C~90 DEG C petroleum ethers of boiling range specification and ethyl acetate mixed solvent for being 9:1 according to volume ratio, is developed the color for spray
With 10% ethanol solution of sulfuric acid, 105 DEG C to be heated to spot development clear, inspects under daylight.
Wherein corresponding 1511010 sample lots of label 1 measure group reagent, 2 corresponding 1512010 sample lots measurement groups
Reagent, 3 corresponding 1512020 sample lots measure group reagent, and 4 correspond to negative sample, and 5 correspond to the examination of nutmeg control group
Agent.
Red ginseng thin layer identifies measuring method
(1) reagent and reagent
A ginseng times Guchang capsule is provided by Liansheng Pharmaceutical Co., Ltd., Guizhou；Red ginseng control medicinal material (121045-201105), people
Ginseng saponin(e Re (110754-201324), ginsenoside Rb1 (110704-201223) are mentioned by Nat'l Pharmaceutical & Biological Products Control Institute
For；Silica gel g thin-layer plate: the silica gel g thin-layer plate and self-control silica gel g thin-layer plate of subsidiary factory, Haiyang Chemical Plant, Qingdao production；Reagent: positive fourth
Alcohol, chloroform, ether, methanol are that analysis is pure.
Ten batches of sample assay results
(2) specificity
It takes ginseng times Guchang capsule, lack red ginseng negative sample, measurement group reagent, control medicinal material examination is made with 2 method of embodiment
Agent and reference substance reagent, then group reagent (being free of ingredient agent to be detected) is measured by prior art preparation feminine gender, survey is taken respectively
Determine group reagent, negative measurement group reagent, control medicinal material reagent and reference substance reagent point sample, expansion, colour developing, is inspected under daylight,
It measures in group reagent chromatography, identical principal spot is shown on position corresponding with control group reagent chromatography, spot separation is preferable, and yin
Property is noiseless.
(3) durability
It takes and measurement group reagent, negative measurement group reagent, control medicinal material reagent and reference substance is made by above-mentioned 10 batches of samples
Reagent is put respectively in silica G prefabricated board and silica G from after making sheet, expansion, colour developing, and as a result spot separator well, noiseless.
The following contents is obtained after measuring according to the technical solution provided in embodiment 2:
In Fig. 7 carrier be silica G plate, solvent be under 10 DEG C of environment temperature according to volume ratio be 65:35:10
Chloroform-methanol-water lower layer solution develops the color to spray with 10% ethanol solution of sulfuric acid, and 105 DEG C to be heated to spot development clear
It is clear, it is inspected under daylight.
In Fig. 8 carrier be silica G plate, solvent be under 10 DEG C of environment temperature according to volume ratio be 65:35:10
Chloroform-methanol-water lower layer solution develops the color to spray with 10% ethanol solution of sulfuric acid, and 105 DEG C to be heated to spot development clear
It is clear, it is inspected under ultraviolet lamp (365nm).
Wherein corresponding 1511010 sample lots of label 1 measure group reagent, 2 corresponding 1512010 sample lots measurement groups examinations
Agent, 3 corresponding 1512020 sample lots measure group reagent, and 4 corresponding negative samples, 5 corresponding red ginseng control medicinal material reagents, 6 correspondences are red
Joining reference substance reagent (is from top to bottom ginsenoside Rb1, ginsenoside Re, ginsenoside Rg1)。
In Fig. 9 and Figure 11, only carrier is had differences, and Fig. 9 carrier is silica G from making sheet, Figure 11 carrier silica gel G prefabricated board,
Solvent is the chloroform-methanol-water lower layer solution for being 65:35:10 according to volume ratio under 10 DEG C of environment temperature,
Colour developing is spray with 10% ethanol solution of sulfuric acid, and 105 DEG C to be heated to spot development clear, is inspected under daylight.
In Figure 10 and Figure 11, only carrier is had differences, and Fig. 9 carrier is silica G from making sheet, Figure 11 carrier silica gel G prefabricated board,
Solvent is the chloroform-methanol-water lower layer solution for being 65:35:10 according to volume ratio under 10 DEG C of environment temperature,
Colour developing is spray with 10% ethanol solution of sulfuric acid, and 105 DEG C to be heated to spot development clear, is inspected under ultraviolet lamp (365nm).
Wherein corresponding 1511010 sample lots of label 1 measure group reagent, 2 corresponding 1512010 sample lots measurement groups examinations
Agent, 3 corresponding 1512020 sample lots measure group reagent, and 4 corresponding negative samples, 5 corresponding red ginseng control medicinal material reagents, 6 correspondences are red
Joining reference substance reagent (is from top to bottom ginsenoside Rb1, ginsenoside Re, ginsenoside Rg1)。
Claims (10)
1. the thin layer for joining rhizoma atractylodis, nutmeg and red ginseng in times Guchang capsule identifies measuring method, it is characterised in that: including rhizoma atractylodis thin layer
Identify measuring method, nutmeg thin layer identifies measuring method and red ginseng thin layer identifies measuring method.
2. the thin layer of rhizoma atractylodis, nutmeg and red ginseng identifies measuring method in ginseng times Guchang capsule according to claim 1, special
Sign is: it includes compareing group reagent preparation, the preparation of measurement group reagent and thin layer to identify survey that the rhizoma atractylodis thin layer, which identifies measuring method,
It is fixed, the control group reagent prepare the following steps are included:
S1 takes rhizoma atractylodis, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and volatilizes to filtrate, and residue is made；
S3, reagent is extracted in addition in residue, so that residue dissolves, control group reagent is made；
Measurement group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and volatilizes to filtrate, and residue is made；
S3, reagent is extracted in addition in residue, so that residue dissolves, measurement group reagent is made；
The thin layer identify measurement the following steps are included:
S1 takes control group reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and opened up by solvent
It opens；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, heating；
S3 after being heated to adaptive temperature, in control group reagent chromatography and the measurement corresponding position of group reagent chromatography, is shown
The fluorescence spot of identical color.
3. the thin layer of rhizoma atractylodis, nutmeg and red ginseng identifies measuring method in ginseng times Guchang capsule according to claim 2, special
Sign is: in control group reagent preparation step, extracting the petroleum ether that reagent is 60 DEG C~90 DEG C of boiling range specification in S1 and S3；
It measures in group reagent preparation step, extracts the petroleum ether that reagent is 60 DEG C~90 DEG C of boiling range specification in S1 and S3；
Thin layer identifies in determination step, the petroleum ether that S1 solvent is 60 DEG C~90 DEG C of boiling range specification, and S2 developing agents are fennel
Aldehyde test solution.
4. the thin layer of rhizoma atractylodis, nutmeg and red ginseng identifies measuring method in ginseng times Guchang capsule according to claim 3, special
Sign is: in control group reagent preparation step, S1 rhizoma atractylodis take 0.5g, and it is 15mL, S2 ultrasonication that reagent is extracted in addition
It is 1mL that reagent is extracted in 20min, S3 addition；
It measures in group reagent preparation step, S1 rhizoma atractylodis take 5g, and it is 15mL that reagent is extracted in addition, S2 ultrasonication 20min, and S3 adds
Add and extracts reagent as 1mL；
Thin layer identifies in determination step, and it is 105 DEG C that S1, which takes control 2 μ L of group reagent, measurement 10 μ L, S3 heating temperature of group reagent,.
5. the thin layer of rhizoma atractylodis, nutmeg and red ginseng identifies measuring method in ginseng times Guchang capsule according to claim 1, special
Sign is: it includes that the preparation of control group reagent, the preparation of measurement group reagent and thin layer identify that the nutmeg thin layer, which identifies measuring method,
Measurement, the control group reagent prepare the following steps are included:
S1 takes nutmeg, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and collects filtrate and control group reagent is made；
Measurement group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule, its is finely ground, sets in stuffed conical flask and adds extraction reagent, extract；
S2, solution carries out ultrasonication after S1 is extracted, and filters, and collects filtrate and measurement group reagent is made；
The thin layer identify measurement the following steps are included:
S1 takes control group reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and opened up by solvent
It opens；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, heating；
S3 after being heated to adaptive temperature, in control group reagent chromatography and the measurement corresponding position of group reagent chromatography, is shown
The fluorescence spot of identical color.
6. the thin layer of rhizoma atractylodis, nutmeg and red ginseng identifies measuring method in ginseng times Guchang capsule according to claim 5, special
Sign is: it is chloroform that reagent is extracted in control group reagent preparation step, in S1；
It measures in group reagent preparation step, it is chloroform that reagent is extracted in S1；
Thin layer identify determination step in, S1 solvent be according to volume ratio be 9:1 60 DEG C~90 DEG C petroleum ethers of boiling range specification and
Ethyl acetate mixed solvent, S2 developing agents are 10% ethanol solution of sulfuric acid.
7. the thin layer of rhizoma atractylodis, nutmeg and red ginseng identifies measuring method in ginseng times Guchang capsule according to claim 6, special
Sign is: in control group reagent preparation step, nutmeg takes 0.5g in S1, and it is 10mL, S2 ultrasonication that reagent is extracted in addition
20min；
It measures in group reagent preparation step, joins a times Guchang capsule in S1 and take 5g, it is 15mL, S2 ultrasonication that reagent is extracted in addition
20min；
Thin layer identifies in determination step, and it is 105 DEG C that S1, which takes control 10 μ L of group reagent, measurement 10 μ L, S3 heating temperature of group reagent,.
8. the thin layer of rhizoma atractylodis, nutmeg and red ginseng identifies measuring method in ginseng times Guchang capsule according to claim 1, special
Sign is: it includes compareing group reagent preparation, the preparation of measurement group reagent and thin layer to identify survey that the red ginseng thin layer, which identifies measuring method,
It is fixed, the control group reagent prepare the following steps are included:
S1 takes ginsenoside Rb1, ginsenoside Re, ginsenoside Rg1, extraction reagent is set in Soxhlet extractor and is added, is heated
It extracts, reference substance extracting solution is made, takes red ginseng to set in Soxhlet extractor and adds extraction reagent, heating extracts, system
Obtain control medicinal material extracting solution；
S2 volatilizes the solution of reference substance extracting solution in S1, and adds reflux reagent, and after being heated to reflux, filtering, filtrate is evaporated,
Reference substance residue is made；The solution of control medicinal material extracting solution in S1 is volatilized, and adds reflux reagent, after being heated to reflux, filtering,
Filtrate is evaporated, and control medicinal material residue is made；
S3 adds solvent in reference substance residue, after to be dissolved, extracts, then alkali cleaning, extracts again after alkali cleaning, and obtained pair
According to product reagent, solvent is added in control medicinal material residue, after to be dissolved, extracts, then alkali cleaning, extracts again after alkali cleaning, is made
Obtain control medicinal material reagent；
Measurement group reagent preparation the following steps are included:
S1 takes ginseng times Guchang capsule, sets in Soxhlet extractor and add extraction reagent, heating extracts；
S2, solution volatilizes after S1 is extracted, and adds reflux reagent, and after being heated to reflux, filtering, filtrate is evaporated, and residue is made；
S3 adds solvent in residue, after to be dissolved, extracts, then alkali cleaning, extracts again after alkali cleaning, and the examination of measurement group is made
Agent；
The thin layer identify measurement the following steps are included:
S1 takes reference substance reagent, control medicinal material reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and pass through
Solvent is unfolded；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, heating；
S3, it is corresponding with measurement group reagent chromatography in reference substance reagent chromatography, control medicinal material reagent chromatography after being heated to adaptive temperature
Position on, be respectively placed under daylight and ultraviolet lamp and inspect, obtain the fluorescence spot for showing identical color.
9. the thin layer of rhizoma atractylodis, nutmeg and red ginseng identifies measuring method in ginseng times Guchang capsule according to claim 8, special
Sign is: in control group reagent preparation step, the extraction reagent that reference substance extracting solution is used to prepare in S1 is methanol, is used to prepare
The extraction reagent of control medicinal material extracting solution is ether, and reflux reagent is methanol in S2, and solvent is the water of n-butanol saturation in S3；
It measures in group reagent preparation step, it is ether that reagent is extracted in S1, and reflux reagent is methanol in S2, and solvent is positive in S3
The water of butanol saturation；
Thin layer identifies in determination step, and solvent is under 10 DEG C of environment temperature according to three that volume ratio is 65:35:10 in S1
Chloromethanes-methanol-water lower layer solution, developing agents are 10% ethanol solution of sulfuric acid in S2.
10. the thin layer of rhizoma atractylodis, nutmeg and red ginseng identifies measuring method in ginseng times Guchang capsule according to claim 9,
It is characterized in that: in control group reagent preparation step, ginsenoside Rb is taken in S11, ginsenoside Re, ginsenoside Rg1Each 1mg, adds
Adding extraction reagent is 1mL, heats 3h, and reflux reagent is 150mL in S2, is heated to reflux the time for 3h, in reference substance residue in S3
In plus the water 30mL of n-butanol saturation make to dissolve, be transferred in separatory funnel, the n-butanol that is saturated with water extracts 3 times, every time
40ml, combination system obtain n-butanol extracting liquid, are washed 2 times with 1% sodium hydroxide solution, wherein 50mL is used for the first time, second of use
30mL, n-butanol 50ml that lye is saturated with water are extracted 1 time, are discarded lye, are merged with above-mentioned n-butanol extracting liquid, then with positive fourth
Alcohol saturation is washed to neutrality, discards water lotion, and for recycling n-butanol to doing, residue adds methanol 2ml to make to dissolve, and reference substance examination is made
Agent；
Take red ginseng 1g in S1, it is 80mL that reagent is extracted in addition, heats 3h, and reflux reagent is 150mL in S2, is heated to reflux the time and is
Add the water 30mL of n-butanol saturation to make to dissolve in control medicinal material residue in 3h, S3, is transferred in separatory funnel, is saturated with water
N-butanol extracts 3 times, and each 40ml, combination system obtains n-butanol extracting liquid, is washed 2 times with 1% sodium hydroxide solution, wherein first
It is secondary to use 50mL, 30mL is used for the second time, and the n-butanol 50ml that lye is saturated with water is extracted 1 time, is discarded lye, is mentioned with above-mentioned n-butanol
It takes liquid to merge, then is washed to neutrality with what n-butanol was saturated, discard water lotion, for recycling n-butanol to doing, residue adds methanol 2ml to make
Control medicinal material reagent is made in dissolution；
In measurement group reagent preparation step, ginseng times Guchang capsule 12g is taken in S1, addition extracts reagent for 80mL, in heating 3h, S2
Reflux reagent is 150mL, and being heated to reflux the time is 3h, adds the water 30mL of n-butanol saturation to make to dissolve in residue in S3, shifts
Into separatory funnel, the n-butanol being saturated with water is extracted 3 times, and each 40ml, combination system obtains n-butanol extracting liquid, with 1% hydrogen-oxygen
Change sodium solution to wash 2 times, wherein using 50mL for the first time, uses 30mL for the second time, the n-butanol 50ml that lye is saturated with water extracts 1
It is secondary, lye is discarded, is merged with above-mentioned n-butanol extracting liquid, then is washed to neutrality with what n-butanol was saturated, water lotion is discarded, recycles
For n-butanol to doing, residue adds methanol 2ml to make to dissolve, and measurement group reagent is made；
Thin layer identifies in determination step, and measurement 10 μ L of group reagent is taken in S1, takes reference substance reagent and each 2 μ L of control medicinal material reagent,
S3 heating temperature is 105 DEG C.
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