CN107621517A - A kind of detection method of Kechuanjing Syrup - Google Patents
A kind of detection method of Kechuanjing Syrup Download PDFInfo
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Abstract
The present invention relates to a kind of detection method of Kechuanjing Syrup of compound Chinese medicinal preparation made of Chinese medicine balloonflower root, aster, earthworm, the wind-weed, dandelion, radix scutellariae, Snakegourd Fruit, the tuber of dwarf lilyturf, semen armeniacae amarae, tussilago, the sweet tuber of stemona, radix glycyrrhizae, the radix paeoniae rubrathe and the red sage root, it is characterized in that carrying out assay to the compound Chinese medicinal preparation Chinese medicine radix scutellariae using high performance liquid chromatography, thin-layered chromatography and doing thin layer discriminating to scutelloside, Paeoniflorin, chinaroot greenbrier sapogenin, Sodium Danshensu and the Chinese medicine tuber of dwarf lilyturf.This method can effectively control the quality of Kechuanjing Syrup, can be as the medicine quality control and the method for investigating reliability of technology.
Description
Technical field
The present invention relates to one kind to treat the disease drugs such as chronic bronchitis, bronchial astehma, acpuei pharyngitis, infantile pneumonia
Detection method, belong to pharmaceutical field.
Background technology
Kechuanjing Syrup performs medicine ministry standard, has antitussive and antiasthmatic, eliminating the phlegm antiinflammation, for chronic bronchial
The diseases such as inflammation, bronchial astehma, acpuei pharyngitis, infantile pneumonia.The medicine is by Chinese medicine balloonflower root, aster, earthworm, the wind-weed, dandelion, Huang
A kind of reed mentioned in ancient books, Snakegourd Fruit, the tuber of dwarf lilyturf, semen armeniacae amarae, tussilago, the sweet tuber of stemona, radix glycyrrhizae, the radix paeoniae rubrathe and red sage root composition；Wherein radix scutellariae, tuber of dwarf lilyturf etc. have been masters
Want the medicinal material of therapeutic action.Existing Kechuanjing Syrup is performed in standard quality control method, is lacked and is played primary treatment work to these
With the method for quality control of medicinal material；Therefore, in terms of thoroughly evaluating Kechuanjing Syrup quality good or not there is limitation in prior art.
Overcome the deficiencies in the prior art of the present invention, the quality control standard of Kechuanjing Syrup is improved, add radix scutellariae (scutelloside) content
The method of quality control and scutelloside of measure, Paeoniflorin, chinaroot greenbrier sapogenin, Sodium Danshensu and Chinese medicine tuber of dwarf lilyturf thin-layer chromatography are determined
Property discrimination method, makes this compound preparation quality control standard further perfect.
The content of the invention
The present invention seeks to overcome prior art insufficient, improve and formulate the method for quality control of Kechuanjing Syrup, increase
The method of quality control and scutelloside of radix scutellariae (scutelloside) assay, Paeoniflorin, chinaroot greenbrier sapogenin, Sodium Danshensu and in
Medicinal material tuber of dwarf lilyturf thin-layer chromatography qualitative identification method, make this compound preparation quality control standard further perfect；Can effectively it control
The product quality of Kechuanjing Syrup.
The present invention is achieved by following technical proposals:
Scutelloside contained by 1 Kechuanjing Syrup Chinese medicine radix scutellariae carries out assay with high performance liquid chromatography:
A. chromatographic condition and system suitability:Using octadecylsilane chemically bonded silica as filler, with methanol-water-phosphoric acid
（47：53：0.2）For mobile phase；Detection wavelength is 280nm, and number of theoretical plate is calculated by scutelloside peak should be not less than 3000；
B. the preparation of reference substance solution:Take scutelloside reference substance appropriate, it is accurately weighed, add Diluted Alcohol alcohol that every 1ml is made and contain radix scutellariae
The μ g-35 μ g of glycosides 25 solution, as reference substance solution；
C. the preparation of need testing solution:Precision measures Kechuanjing Syrup 8ml-12ml, puts in 100ml measuring bottles, is dissolved with water and dilute
Release to scale, shake up, precision measures 5ml, puts in 50ml measuring bottles, is dissolved with Diluted Alcohol and is diluted to scale, shaken up, and filtration, takes
Subsequent filtrate, as need testing solution；
D. determination method:It is accurate respectively to draw reference substance solution and each 8-12 μ l of need testing solution, inject liquid chromatograph, measure；
Kechuanjing Syrup contains radix scutellariae per 1ml in terms of scutelloside, must not be less than 1.5mg；
Scutelloside is differentiated with thin-layered chromatography in 2 Kechuanjing Syrups:
A. the preparation of reference substance solution:Scutelloside reference substance is taken, adds methanol that solution of every 1ml containing 1mg is made, as reference substance
Solution；
B. the preparation of need testing solution:Kechuanjing Syrup 8ml-12ml is taken, adds water 10ml, shakes up, puts D101 type macroporous absorption trees
Fat post（Internal diameter is 1.5cm, a height of 12cm）On, eluted with water 80ml, discard water lotion, then eluted with 40% ethanol 60ml, collect
Eluent, it is evaporated, residue adds methanol 3ml, and low-grade fever is stirred to dissolve, and centrifugation, supernatant is taken, as need testing solution；
C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 3-8 μ l of need testing solution are drawn, is put respectively in same silica G
On lamellae, with ethyl acetate-butanone-formic acid-water（5:3:1:1）For solvent, deploy, take out, dry, spray with 1% tri-chlorination
Iron ethanol solution, in test sample chromatogram, on position corresponding with reference substance chromatogram, show the spot of same color；
Paeoniflorin is differentiated with thin-layered chromatography in 3 Kechuanjing Syrups:
A. the preparation of control medicinal material solution:Take Paeoniflorin to compare medicine, add methanol that solution of every 1ml containing 1mg is made, as right
According to product solution；
B. the preparation of need testing solution:Kechuanjing Syrup 8ml-12ml is taken, adds water 10ml, shakes up, puts D101 type macroporous absorption trees
Fat post（Internal diameter is 1.5cm, a height of 12cm）On, eluted with water 80ml, discard water lotion, then eluted with 40% ethanol 60ml, collect
Eluent, it is evaporated, residue adds methanol 3ml, and low-grade fever is stirred to dissolve, and centrifugation, supernatant is taken, as need testing solution；
C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 3-8 μ l of need testing solution are drawn, is put respectively in same silica G
On lamellae, with chloroform-methanol-water（9:3:0.3）For solvent, deploy, take out, dry, spray with 5% vanillin-sulfuric acid
Solution, it is clear to be heated to spot development at 105 DEG C, in test sample chromatogram, on position corresponding with reference substance chromatogram, shows identical
The spot of color；
Chinaroot greenbrier sapogenin is differentiated with thin-layered chromatography in 4 Kechuanjing Syrups:
A. the preparation of reference substance solution:Chinaroot greenbrier sapogenin reference substance is taken, adds methanol that solution of every 1ml containing 1mg is made, as right
According to product solution；
B. the preparation of need testing solution:Kechuanjing Syrup 8ml-12ml is taken, adds water 10ml, shakes up, puts D101 type macroporous absorption trees
Fat post（Internal diameter is 1.5cm, a height of 12cm）On, eluted with water 80ml, discard water lotion, then eluted with 40% ethanol 60ml, collect
Eluent, it is evaporated, residue adds methanol 3ml, and low-grade fever is stirred to dissolve, and centrifugation, takes supernatant, puts D101 type large pore resin absorption columns
Continue to be eluted with 70% ethanol 60ml, collect eluent, add hydrochloric acid 1-3ml, be heated to reflux 1 hour, be concentrated into about 1-3ml, add water
15-25ml makes dissolving, with ethyl acetate shaking extraction 2 times, each 20-40ml, combined ethyl acetate liquid, is evaporated, residue adds first
Alcohol 1-3ml makes dissolving, as need testing solution；
C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 5-10 μ l of need testing solution are drawn, is put respectively in same silica gel
On G lamellaes, with toluene-acetone（9:1）For solvent, deploy, take out, dry, spray with 5% vanillin-sulfuric acid solution,
105 DEG C to be heated to spot development clear, in test sample chromatogram, on position corresponding with reference substance chromatogram, shows same color
Spot；
Sodium Danshensu is differentiated with thin-layered chromatography in 5 Kechuanjing Syrups:
A. the preparation of reference substance solution:Sodium Danshensu reference substance is taken, adds 75% methanol that solution of every 1ml containing 1mg is made, as right
According to product solution；
B. the preparation of need testing solution:Take Kechuanjing Syrup 10-20ml, add water 10-20ml, shake up, with watery hydrochloric acid adjust pH to
2, with ethyl acetate shaking extraction 2 times, each 20-40ml, combined ethyl acetate liquid, it is evaporated, it is molten that residue adds methanol 1-3ml to make
Solution, as need testing solution；
C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 2-5 μ l of need testing solution are drawn, is put respectively in same silica G
On lamellae, with toluene-ethyl acetate-formic acid（5:5:1）For solvent, deploy, take out, dry, put after being smoked in ammonia steam, put
Ultraviolet lamp（365nm）Under inspect, in test sample chromatogram, on position corresponding with reference substance chromatogram, show same color spot
Point；
The 6 Kechuanjing Syrup Chinese medicine tubers of dwarf lilyturf were differentiated with thin-layered chromatography:
A. the preparation of control medicinal material solution:Tuber of dwarf lilyturf control medicinal material 1g is taken, adds water 25-35ml, decocts 30 minutes, lets cool, is filtered,
Filtrate is taken, as control medicinal material solution；
B. the preparation of need testing solution:Kechuanjing Syrup 5-15ml is taken, adds water 15-25ml, shakes up, adds hydrochloric acid 1-3ml, is heated
Backflow 1 hour, lets cool, and is shaken and extracted with ether 20-40ml, and ether solution volatilizes, and residue adds chloroform 1-3ml to make dissolving, makees
For need testing solution；
C. thin-layered chromatography is tested:Above-mentioned each 2-5 μ l of control medicinal material solution and need testing solution are drawn, are put respectively in same silica gel
On G lamellaes, with chloroform-acetone（4:1）For solvent, deploy, take out, dry, spray with 10% ethanol solution of sulfuric acid,
Heated 5 minutes at 105 DEG C, in test sample chromatogram, on position corresponding with control medicinal material chromatogram, show the spot of same color.
The invention provides the method for quality control of radix scutellariae (scutelloside) assay and scutelloside, Paeoniflorin, chinaroot greenbrier
Sapogenin, Sodium Danshensu and Chinese medicine tuber of dwarf lilyturf thin-layer chromatography qualitative identification method, method is simple, can be used as Kechuanjing Syrup
Quality control index.
Embodiment
Embodiment:
Take balloonflower root 100g in prescription, aster 100g, earthworm 120g, wind-weed 150g, dandelion 150g, radix scutellariae 150g, Snakegourd Fruit 200g,
Tuber of dwarf lilyturf 100g, semen armeniacae amarae 100g, tussilago 100g, sweet tuber of stemona 100g, radix glycyrrhizae 100g, radix paeoniae rubrathe 120g and red sage root 120g, add decocting
Boil 2 times, 2 hours for the first time, second 1 hour, collecting decoction, filtration, filtrate is concentrated into 2000ml, stands 24 hours, incline and take
Supernatant, it is concentrated into right amount, adds sucrose 660g, stirring evenly makes dissolving, adds sodium benzoate 3g and water to 1200ml, it is small to stand 48
When, take supernatant addition essence appropriate, stir evenly, produce.
The method of quality control of Kechuanjing Syrup comprises the following steps:
Scutelloside contained by 1 Kechuanjing Syrup Chinese medicine radix scutellariae carries out assay with high performance liquid chromatography:
A. chromatographic condition and system suitability:Using octadecylsilane chemically bonded silica as filler, with methanol-water-phosphoric acid
（47：53：0.2）For mobile phase；Detection wavelength is 280nm, and number of theoretical plate is calculated by scutelloside peak should be not less than 3000；
B. the preparation of reference substance solution:Take scutelloside reference substance appropriate, it is accurately weighed, add Diluted Alcohol alcohol that every 1ml is made and contain radix scutellariae
The μ g of glycosides 30 solution, as reference substance solution；
C. the preparation of need testing solution:Precision measures Kechuanjing Syrup 10ml, puts in 100ml measuring bottles, is dissolved and be diluted to water
Scale, shake up, precision measures 5ml, puts in 50ml measuring bottles, is dissolved with Diluted Alcohol and is diluted to scale, shaken up, and filtration, takes continuous filter
Liquid, as need testing solution；
D. determination method:It is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, inject liquid chromatograph, measure；Cough
Breathe heavily quiet syrup and contain radix scutellariae per 1ml in terms of scutelloside, 1.5mg must not be less than；
Scutelloside is differentiated with thin-layered chromatography in 2 Kechuanjing Syrups:
A. the preparation of reference substance solution:Scutelloside reference substance is taken, adds methanol that solution of every 1ml containing 1mg is made, as reference substance
Solution；
B. the preparation of need testing solution:Kechuanjing Syrup 10ml is taken, adds water 10ml, shakes up, puts D101 type large pore resin absorption columns
（Internal diameter is 1.5cm, a height of 12cm）On, eluted with water 80ml, discard water lotion, then eluted with 40% ethanol 60ml, collect elution
Liquid, it is evaporated, residue adds methanol 3ml, and low-grade fever is stirred to dissolve, and centrifugation, supernatant is taken, as need testing solution；
C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 3-8 μ l of need testing solution are drawn, is put respectively in same silica G
On lamellae, with ethyl acetate-butanone-formic acid-water（5:3:1:1）For solvent, deploy, take out, dry, spray with 1% tri-chlorination
Iron ethanol solution, in test sample chromatogram, on position corresponding with reference substance chromatogram, show the spot of same color；
Paeoniflorin is differentiated with thin-layered chromatography in 3 Kechuanjing Syrups:
A. the preparation of control medicinal material solution:Take Paeoniflorin to compare medicine, add methanol that solution of every 1ml containing 1mg is made, as right
According to product solution；
B. the preparation of need testing solution:Kechuanjing Syrup 10ml is taken, adds water 10ml, shakes up, puts D101 type large pore resin absorption columns
（Internal diameter is 1.5cm, a height of 12cm）On, eluted with water 80ml, discard water lotion, then eluted with 40% ethanol 60ml, collect elution
Liquid, it is evaporated, residue adds methanol 3ml, and low-grade fever is stirred to dissolve, and centrifugation, supernatant is taken, as need testing solution；
C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 3-8 μ l of need testing solution are drawn, is put respectively in same silica G
On lamellae, with chloroform-methanol-water（9:3:0.3）For solvent, deploy, take out, dry, spray with 5% vanillin-sulfuric acid
Solution, it is clear to be heated to spot development at 105 DEG C, in test sample chromatogram, on position corresponding with reference substance chromatogram, shows identical
The spot of color；
Chinaroot greenbrier sapogenin is differentiated with thin-layered chromatography in 4 Kechuanjing Syrups:
A. the preparation of reference substance solution:Chinaroot greenbrier sapogenin reference substance is taken, adds methanol that solution of every 1ml containing 1mg is made, as right
According to product solution；
B. the preparation of need testing solution:Kechuanjing Syrup 10ml is taken, adds water 10ml, shakes up, puts D101 type large pore resin absorption columns
（Internal diameter is 1.5cm, a height of 12cm）On, eluted with water 80ml, discard water lotion, then eluted with 40% ethanol 60ml, collect elution
Liquid, it is evaporated, residue adds methanol 3ml, and low-grade fever is stirred to dissolve, and centrifugation, takes supernatant, puts the continuation of D101 types large pore resin absorption column
Eluted with 70% ethanol 60ml, collect eluent, add hydrochloric acid 2ml, be heated to reflux 1 hour, be concentrated into about 2ml, add water 20ml to make molten
Solution, with ethyl acetate shaking extraction 2 times, each 30ml, combined ethyl acetate liquid, it is evaporated, residue adds methanol 2ml to make dissolving, makees
For need testing solution；
C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 5-10 μ l of need testing solution are drawn, is put respectively in same silica gel
On G lamellaes, with toluene-acetone（9:1）For solvent, deploy, take out, dry, spray with 5% vanillin-sulfuric acid solution,
105 DEG C to be heated to spot development clear, in test sample chromatogram, on position corresponding with reference substance chromatogram, shows same color
Spot；
Sodium Danshensu is differentiated with thin-layered chromatography in 5 Kechuanjing Syrups:
A. the preparation of reference substance solution:Sodium Danshensu reference substance is taken, adds 75% methanol that solution of every 1ml containing 1mg is made, as right
According to product solution；
B. the preparation of need testing solution:Kechuanjing Syrup 15ml is taken, adds water 15ml, shakes up, pH to 2 is adjusted with watery hydrochloric acid, uses second
Acetoacetic ester shaking extraction 2 times, each 30ml, combined ethyl acetate liquid, is evaporated, residue adds methanol 2ml to make dissolving, as test sample
Solution；
C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 2-5 μ l of need testing solution are drawn, is put respectively in same silica G
On lamellae, with toluene-ethyl acetate-formic acid（5:5:1）For solvent, deploy, take out, dry, put after being smoked in ammonia steam, put
Ultraviolet lamp（365nm）Under inspect, in test sample chromatogram, on position corresponding with reference substance chromatogram, show same color spot
Point；
The 6 Kechuanjing Syrup Chinese medicine tubers of dwarf lilyturf were differentiated with thin-layered chromatography:
A. the preparation of control medicinal material solution:Tuber of dwarf lilyturf control medicinal material 1g is taken, adds water 30ml, decocts 30 minutes, lets cool, filters, takes filter
Liquid, as control medicinal material solution；
B. the preparation of need testing solution:Kechuanjing Syrup 10ml is taken, adds water 20ml, shakes up, adds hydrochloric acid 2ml, it is small to be heated to reflux 1
When, let cool, shaken and extracted with ether 30ml, ether solution volatilizes, and residue adds chloroform 2ml to make dissolving, as need testing solution；
C. thin-layered chromatography is tested:Above-mentioned each 2-5 μ l of control medicinal material solution and need testing solution are drawn, are put respectively in same silica gel
On G lamellaes, with chloroform-acetone（4:1）For solvent, deploy, take out, dry, spray with 10% ethanol solution of sulfuric acid,
Heated 5 minutes at 105 DEG C, in test sample chromatogram, on position corresponding with control medicinal material chromatogram, show the spot of same color.
Claims (1)
- A kind of 1. detection method of Kechuanjing Syrup, wherein the medicine is by Chinese medicine balloonflower root 100g, aster 100g, earthworm 120g, wind-weed 150g, dandelion 150g, radix scutellariae 150g, Snakegourd Fruit 200g, tuber of dwarf lilyturf 100g, semen armeniacae amarae 100g, tussilago 100g, honey Tuber of stemona 100g, radix glycyrrhizae 100g, radix paeoniae rubrathe 120g and red sage root 120g are made, it is characterised in that this method comprises the following steps:(1) scutelloside carries out assay with high performance liquid chromatography contained by Kechuanjing Syrup Chinese medicine radix scutellariae:A. chromatographic condition and system suitability:Using octadecylsilane chemically bonded silica as filler, with methanol-water-phosphoric acid （47：53：0.2）For mobile phase；Detection wavelength is 280nm, and number of theoretical plate is calculated by scutelloside peak should be not less than 3000；B. the preparation of reference substance solution:Take scutelloside reference substance appropriate, it is accurately weighed, add Diluted Alcohol alcohol that every 1ml is made and contain radix scutellariae The μ g-35 μ g of glycosides 25 solution, as reference substance solution；C. the preparation of need testing solution:Precision measures Kechuanjing Syrup 8ml-12ml, puts in 100ml measuring bottles, is dissolved with water and dilute Release to scale, shake up, precision measures 5ml, puts in 50ml measuring bottles, is dissolved with Diluted Alcohol and is diluted to scale, shaken up, and filtration, takes Subsequent filtrate, as need testing solution；D. determination method:It is accurate respectively to draw reference substance solution and each 8-12 μ l of need testing solution, inject liquid chromatograph, measure； Kechuanjing Syrup contains radix scutellariae per 1ml in terms of scutelloside, must not be less than 1.5mg；(2) scutelloside is differentiated with thin-layered chromatography in Kechuanjing Syrup:A. the preparation of reference substance solution:Scutelloside reference substance is taken, adds methanol that solution of every 1ml containing 1mg is made, as reference substance Solution；B. the preparation of need testing solution:Kechuanjing Syrup 8ml-12ml is taken, adds water 10ml, shakes up, puts D101 type macroporous absorption trees Fat post（Internal diameter is 1.5cm, a height of 12cm）On, eluted with water 80ml, discard water lotion, then eluted with 40% ethanol 60ml, collect Eluent, it is evaporated, residue adds methanol 3ml, and low-grade fever is stirred to dissolve, and centrifugation, supernatant is taken, as need testing solution；C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 3-8 μ l of need testing solution are drawn, is put respectively in same silica G On lamellae, with ethyl acetate-butanone-formic acid-water（5:3:1:1）For solvent, deploy, take out, dry, spray with 1% tri-chlorination Iron ethanol solution, in test sample chromatogram, on position corresponding with reference substance chromatogram, show the spot of same color；(3) Paeoniflorin is differentiated with thin-layered chromatography in Kechuanjing Syrup:A. the preparation of control medicinal material solution:Take Paeoniflorin to compare medicine, add methanol that solution of every 1ml containing 1mg is made, as right According to product solution；B. the preparation of need testing solution:Kechuanjing Syrup 8ml-12ml is taken, adds water 10ml, shakes up, puts D101 type macroporous absorption trees Fat post（Internal diameter is 1.5cm, a height of 12cm）On, eluted with water 80ml, discard water lotion, then eluted with 40% ethanol 60ml, collect Eluent, it is evaporated, residue adds methanol 3ml, and low-grade fever is stirred to dissolve, and centrifugation, supernatant is taken, as need testing solution；C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 3-8 μ l of need testing solution are drawn, is put respectively in same silica G On lamellae, with chloroform-methanol-water（9:3:0.3）For solvent, deploy, take out, dry, spray with 5% vanillin-sulfuric acid Solution, it is clear to be heated to spot development at 105 DEG C, in test sample chromatogram, on position corresponding with reference substance chromatogram, shows identical The spot of color；(4) chinaroot greenbrier sapogenin is differentiated with thin-layered chromatography in Kechuanjing Syrup:A. the preparation of reference substance solution:Chinaroot greenbrier sapogenin reference substance is taken, adds methanol that solution of every 1ml containing 1mg is made, as right According to product solution；B. the preparation of need testing solution:Kechuanjing Syrup 8ml-12ml is taken, adds water 10ml, shakes up, puts D101 type macroporous absorption trees Fat post（Internal diameter is 1.5cm, a height of 12cm）On, eluted with water 80ml, discard water lotion, then eluted with 40% ethanol 60ml, collect Eluent, it is evaporated, residue adds methanol 3ml, and low-grade fever is stirred to dissolve, and centrifugation, takes supernatant, puts D101 type large pore resin absorption columns Continue to be eluted with 70% ethanol 60ml, collect eluent, add hydrochloric acid 1-3ml, be heated to reflux 1 hour, be concentrated into about 1-3ml, add water 15-25ml makes dissolving, with ethyl acetate shaking extraction 2 times, each 20-40ml, combined ethyl acetate liquid, is evaporated, residue adds first Alcohol 1-3ml makes dissolving, as need testing solution；C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 5-10 μ l of need testing solution are drawn, is put respectively in same silica gel On G lamellaes, with toluene-acetone（9:1）For solvent, deploy, take out, dry, spray with 5% vanillin-sulfuric acid solution, 105 DEG C to be heated to spot development clear, in test sample chromatogram, on position corresponding with reference substance chromatogram, shows same color Spot；(5) Sodium Danshensu is differentiated with thin-layered chromatography in Kechuanjing Syrup:A. the preparation of reference substance solution:Sodium Danshensu reference substance is taken, adds 75% methanol that solution of every 1ml containing 1mg is made, as right According to product solution；B. the preparation of need testing solution:Take Kechuanjing Syrup 10-20ml, add water 10-20ml, shake up, with watery hydrochloric acid adjust pH to 2, with ethyl acetate shaking extraction 2 times, each 20-40ml, combined ethyl acetate liquid, it is evaporated, it is molten that residue adds methanol 1-3ml to make Solution, as need testing solution；C. thin-layered chromatography is tested:Above-mentioned reference substance solution and each 2-5 μ l of need testing solution are drawn, is put respectively in same silica G On lamellae, with toluene-ethyl acetate-formic acid（5:5:1）For solvent, deploy, take out, dry, put after being smoked in ammonia steam, put Ultraviolet lamp（365nm）Under inspect, in test sample chromatogram, on position corresponding with reference substance chromatogram, show same color spot Point；(6) the Kechuanjing Syrup Chinese medicine tuber of dwarf lilyturf is differentiated with thin-layered chromatography:A. the preparation of control medicinal material solution:Tuber of dwarf lilyturf control medicinal material 1g is taken, adds water 25-35ml, decocts 30 minutes, lets cool, is filtered, Filtrate is taken, as control medicinal material solution；B. the preparation of need testing solution:Kechuanjing Syrup 5-15ml is taken, adds water 15-25ml, shakes up, adds hydrochloric acid 1-3ml, is heated Backflow 1 hour, lets cool, and is shaken and extracted with ether 20-40ml, and ether solution volatilizes, and residue adds chloroform 1-3ml to make dissolving, makees For need testing solution；C. thin-layered chromatography is tested:Above-mentioned each 2-5 μ l of control medicinal material solution and need testing solution are drawn, are put respectively in same silica gel On G lamellaes, with chloroform-acetone（4:1）For solvent, deploy, take out, dry, spray with 10% ethanol solution of sulfuric acid, Heated 5 minutes at 105 DEG C, in test sample chromatogram, on position corresponding with control medicinal material chromatogram, show the spot of same color.
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| CN111351892A (en) * | 2018-12-21 | 2020-06-30 | 河北万邦复临药业有限公司 | Radix ophiopogonis detection method |
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