CN109164200A - The method of quality control of the relieving cough and asthma particle of small infantile paralysis dragon - Google Patents
The method of quality control of the relieving cough and asthma particle of small infantile paralysis dragon Download PDFInfo
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- CN109164200A CN109164200A CN201810764757.6A CN201810764757A CN109164200A CN 109164200 A CN109164200 A CN 109164200A CN 201810764757 A CN201810764757 A CN 201810764757A CN 109164200 A CN109164200 A CN 109164200A
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- G—PHYSICS
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- 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
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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
- G01N30/02—Column chromatography
Abstract
The invention discloses a kind of method of quality control of the relieving cough and asthma particle of small infantile paralysis dragon, carry out Qualitive test to pheretima, loguat leaf, Radix Glycyrrhizae in the relieving cough and asthma particle of small infantile paralysis dragon using thin-layered chromatography；Quantitative control is carried out using the content of three amarogentin, ephedrine and forsythiaside A active constituents in the relieving cough and asthma particle of the small infantile paralysis dragon of high effective liquid chromatography for measuring.The method of the present invention is simple, separating degree is good, specificity is strong, favorable reproducibility, has effectively ensured the quality and curative effect of the relieving cough and asthma particle of small infantile paralysis dragon, has had very strong practicability.
Description
Technical field
The invention belongs to medicine quality detection technique fields, and in particular to the quality control of the relieving cough and asthma particle of small infantile paralysis dragon
Method.
Background technique
The medicine group of the relieving cough and asthma particle of small infantile paralysis dragon becomes: frying 1~3 part of semen armeniacae amarae, 1~3 part of stir-baked SEMEN PERSICAE, prepared RHIZOMA PINELLIZE without adju-vant 2
~4 parts, 1~2 part of Radix Glycyrrhizae, 4~9 parts of gypsum, 1~2 part of Chinese ephedra, 1~3 part of pheretima, 1~3 part of Fructus Forsythiae, 1~3 part of the root bark of white mulberry,
1~3 part of the sweet tuber of stemona, 1~3 part of the root of purple-flowered peucedanum, 2~4 parts of loguat leaf have the effect of clearing lung and eliminating phlegm, expelling wind and cold pathogens, sending down abnormally ascending cough-relieving.
Wherein, Chinese ephedra, two medicine of pheretima share, clearing heat and freeing lung, expelling wind and cold pathogens, and spasmolysis cough-relieving is altogether monarch drug in a prescription, semen armeniacae amarae, hundred
Portion, loguat leaf, gypsum, prepared RHIZOMA PINELLIZE without adju-vant are ministerial drug altogether, and Fructus Forsythiae, the root of purple-flowered peucedanum, the root bark of white mulberry are adjutant.
It is pheretima, the loguat leaf, licorice medicinal materials discrimination method of 2015 editions Chinese Pharmacopoeias one record below.
Pheretima medicinal material identifies: taking this product powder lg, adds chloroform 20ml, be ultrasonically treated 20 minutes, filtration, filtrate is steamed
Dry, residue adds chloroform lm l to make to dissolve, as test solution；Pheretima control medicinal material lg separately is taken, is made in the same way of comparison medicine
Material solution.It is tested according to thin-layered chromatography, draws each 5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with first
Benzene-acetone (9:1) is solvent, is unfolded, and takes out, dries, set and inspect under ultraviolet lamp.In sample chromatogram, comparison medicine wood color
It composes on corresponding position, shows the fluorescence spot of same color.
Loguat leaf identifies: taking this product powder lg, adds methanol 20ml, be ultrasonically treated 20 minutes, filtration, filtrate is evaporated, residue
Methanol 5ml is added to make to dissolve, as test solution.Loguat leaf control medicinal material lg separately is taken, is made in the same way of control medicinal material solution；It takes again
Ursolic acid reference substance adds methanol that the solution of every lm l g containing lm is made, as reference substance solution；It tests, inhales according to thin-layered chromatography
Above-mentioned each 1 μ l of three kinds of solution is taken, is put respectively on same silica gel g thin-layer plate, with toluene-acetone (5:1) for solvent, is unfolded,
It takes out, dries, spray with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot development at 105 DEG C.In sample chromatogram, with it is right
According in medicinal material chromatography and the corresponding position of reference substance chromatography, the spot of same color is shown.
Radix Glycyrrhizae identifies: taking this product powder 1g, add diethyl ether 40ml, is heated to reflux 1 hour, filters, discards ether liquid, the dregs of a decoction add first
Alcohol 30ml is heated to reflux 1 hour, and filtration, filtrate is evaporated, and residue adds water 40ml to make to dissolve, and extracts 3 times with n-butanol, every time
20ml merges n-butanol liquid, is washed with water 3 times, discards aqueous, and positive fourth zymotic fluid is evaporated, and residue adds methanol 5ml to make to dissolve, as
Test solution；Another extracting liquorice control medicinal material 1g, is made in the same way of control medicinal material solution；Extracting liquorice acid mono-ammonium reference substance again, adds
Every solution of the lm l containing 2mg is made in methanol, as reference substance solution.It is tested according to thin-layered chromatography, draws above-mentioned three kinds of solution each 1
~2 μ l, put respectively in it is same with 1% sodium hydroxide solution prepare silica gel g thin-layer plate on, with acetic ether-methanoic acid-ice vinegar
Acid-water (15:1:1:2) is solvent, is unfolded, and takes out, dries, and sprays with 10% ethanol solution of sulfuric acid, is heated to spot at 105 DEG C
Colour developing is clear, sets and inspects under ultraviolet lamp.In sample chromatogram, on position corresponding with reference medicine chromatography, identical face is shown
The fluorescence spot of color；At the position corresponding to the chromatogram of the reference substance, identical orange-yellow fluorescence spot is shown.
Pheretima, loguat leaf and Radix Glycyrrhizae are identified with reference to pharmacopeia discrimination method, feminine gender has an interference, unstable result, because
This, the present invention improves above-mentioned discrimination method, can be with exclusive PCR, the result made is accurate.
Summary of the invention
The present invention provides one kind simply, specificity is strong and the quality control of the reproducible relieving cough and asthma particle of small infantile paralysis dragon
Method processed, the quality for the relieving cough and asthma particle of small infantile paralysis dragon provide guarantee.
A kind of method of quality control of the relieving cough and asthma particle of small infantile paralysis dragon, includes the following steps:
(1) qualitative mirror is carried out to pheretima, loguat leaf and Radix Glycyrrhizae in the relieving cough and asthma particle of small infantile paralysis dragon using thin-layered chromatography
Not；
(2) using high performance liquid chromatography to the active constituent amarogentin in the relieving cough and asthma particle of small infantile paralysis dragon, Chinese ephedra
Alkali and forsythiaside A carry out quantitative identification；
In step (1), the chromatographic condition of the pheretima identification are as follows: using pheretima as control medicinal material, with volume ratio for 3~7:
0.5~1.5: 1 n-butanol-glacial acetic acid-water is that solvent develops the color using ninhydrin solution as color developing agent at 105 DEG C；
The chromatographic condition that the loguat leaf identifies are as follows: using loguat leaf as control medicinal material, with volume ratio be 3~6: 4~8: 2~
5 chloroform-methanol-water lower layer's solution is solvent, using 10% phosphomolybdic acid ethanol solution as color developing agent, at 105 DEG C
Colour developing；
The chromatographic condition that the Radix Glycyrrhizae identifies are as follows: using Radix Glycyrrhizae as control medicinal material, with volume ratio for 15~22: 4~8: 2~4:
0.2~0.6: 0.15 chloroform-methanol-ethyl acetate-formic acid-water is solvent, is aobvious with 10% ethanol solution of sulfuric acid
Toner develops the color at 105 DEG C.
In step (2), the ephedrine is specially ephedrine hydrochloride and pseudoephedrine hydrochloride.
The present invention has first carried out careful research to prescription Chinese medicinal materials, has investigated a variety of methods and has extracted, using a variety of expansion
System expansion, the sweet tuber of stemona have a preferable characteristic spots, but test of many times find its method be disturbed more factor, stability,
Poor repeatability；The root bark of white mulberry also has preferable characteristic spots, but can not rule out interference；Gypsum and its characteristic spots of prepared RHIZOMA PINELLIZE without adju-vant are equal
It is unobvious；Therefore it is not satisfactory for the sweet tuber of stemona, the root bark of white mulberry, prepared RHIZOMA PINELLIZE without adju-vant and gypsum experimental study, thin layer identifies poor repeatability
Or it can not rule out interference.And pheretima, loguat leaf, Radix Glycyrrhizae indentification by TLC clear spot, favorable reproducibility is negative noiseless.
Therefore, in order to effectively control drug quality, the method for quality control of science is established, to Chinese ephedra, fries semen armeniacae amarae, stir-fry peach
Benevolence, Fructus Forsythiae four traditional Chinese medicine material carry out quantitative control, remaining 8 taste medicinal material establishes 3 thin layers identification items by experimental study, be respectively with
The Qualitive test that Radix Glycyrrhizae, pheretima, loguat leaf are carried out as control medicinal material.
Pheretima is the monarch drug in a prescription in the relieving cough and asthma particle of fiber crops dragon, and pheretima main component is proteins and peptides, amino acid, nucleosides
Succinic acid, hypoxanthine, xanthine, adenine of acids etc. can not establish quantitative Con trolling index through research, therefore carry out thin layer
Identify research.Identified with reference to this product pharmacopeia discrimination method, feminine gender has interference；Through many experiments investigate benzene-ethyl acetate and
N-butanol-glacial acetic acid-water development system, as a result with n-butanol-glacial acetic acid-water (3~7: 0.5~1.5: 1) be solvent, spray with
Ninhydrin solution, 105 DEG C of colour developings, available more satisfied result.
Ursolic acid and oleanolic acid are mainly contained in loguat leaf, the method in pharmacopeia is to identify ursolic acid, this test application
Official method identifies, but feminine gender has interference.Through experimental study instead sodium hydroxide solution alkali is used to control medicinal material and test solution
Change is extracted with ethyl acetate again, can exclusive PCR；Through investigating, with the lower layer of chloroform-methanol-water (3~6: 4~8: 2~5)
Solution is solvent, and spray is with 10% phosphomolybdic acid ethanol solution, 105 DEG C of colour developings, the result being more satisfied with.
Radix Glycyrrhizae is first identified using the method for pharmacopeia, finds there is corresponding spot with reference medicine chromatography in sample chromatogram,
But speckled background is deeper, it appears that has interference, therefore does not use.The present invention is with chloroform-methanol-ethyl acetate-formic acid-water
(15~22: 4~8: 2~4: 0.2~0.6: 0.15) be solvent, spray 10% ethanol solution of sulfuric acid, 105 DEG C colour developing, as a result compared with
For satisfied and repeatability, have good stability.
According to the selected requirement of new Chinese medicine quality standard research assay, selection and this product major function and indication
Assay index components of the relevant principle active component as this product, ephedrine have antiallergy, and it is flat to alleviate bronchus
Sliding muscle spasmus effect, amarogentin have anti-inflammatory, anti-allergic effects with significant antitussive and antiasthmatic effect, forsythiaside A.Therefore quasi-
It is main in main component amarogentin and left medicine Fructus Forsythiae in selected monarch drug in a prescription Chinese ephedra main component ephedrine hydrochloride, ministerial drug semen armeniacae amarae
Ingredient forsythiaside A is the assay index that the quality of this product controls.
Contain semen armeniacae amarae and peach kernel medicinal material in the relieving cough and asthma particle of small infantile paralysis dragon, amarogentin is the main of this two tastes medicinal material
Effective component, amarogentin can be decomposed slowly in vivo, gradually generate micro hydrogen cyanide, can play slight inhibition respiratory center,
So that respiratory system is tended to be quiet and the effect of in significant antitussive and antiasthmatic.Therefore select amarogentin as this product quality control index
Ingredient establishes the content of HPLC method measurement amarogentin, has carried out methodological study.
Chinese ephedra is the monarch drug in a prescription in the relieving cough and asthma particle prescription of small infantile paralysis dragon, ephedrine be Herba Ephedrae it is main effectively at
Point, there is antiasthmatic-antitussive effect, therefore select ephedrine as this product quality control index ingredient, establishes HPLC method while surveying
Determine the method for Content of Ephedrine With, carries out methodological study.
Fructus Forsythiae is that the relieving cough and asthma particle of fiber crops dragon forms one of flavour of a drug, and forsythiaside A is the principle active component of the medicinal material, existing
Show that forsythiaside A has anti-inflammatory, anti-allergic effects for pharmacological research, has document report forsythiaside A stability poor, therefore select
Forsythiaside A is selected as one of multiple quantitatively control index components of this product, establishes the side of HPLC method measurement forsythiaside A content
Method has carried out methodological study.
In step (1), the discrimination method of the pheretima are as follows: take this product 6g to be dissolved in water, add at chloroform ultrasound
Reason 20~60 minutes divides and filtrate is taken to be evaporated, and residue adds 1ml methanol to dissolve, as test solution；Separately pheretima control medicinal material is taken to add
Enter 20~60ml methanol, is ultrasonically treated 20~60 minutes, filtrate is evaporated, and residue adds methanol to dissolve, as control medicinal material solution；According to
2015 editions four general rules 0502 tests of thin-layered chromatography Chinese Pharmacopoeia, draw test solution, each 10 μ l of control medicinal material solution, point
Other point takes out after being unfolded in solvent and dries on same silica gel g thin-layer plate, spray color developing agent, and 105 DEG C to be dried to spot development clear
It is clear, in sample chromatogram, on reference medicine chromatography corresponding position, show the spot of same color.
In step (1), the discrimination method of the loguat leaf are as follows: take this product 6g to be dissolved in water, with 1% sodium hydroxide solution tune
PH value is saved to 8~11, is extracted 2 times, is evaporated with 15~30ml ethyl acetate respectively, residue adds 0.5ml methanol to dissolve, as examination
Product solution；Loguat leaf control medicinal material is taken, adds water refluxing extraction 30~60 minutes, filtrate adjusts pH value with 1% sodium hydroxide solution
To 8~11, is extracted 2 times, be evaporated, residue adds methanol to dissolve, as control medicinal material solution with 15~30ml ethyl acetate respectively；According to
2015 editions four general rules 0502 tests of thin-layered chromatography Chinese Pharmacopoeia, draw test solution, each 10 μ l of control medicinal material solution, point
Other point takes out after being unfolded in solvent and dries on same silica gel g thin-layer plate, spray color developing agent, and 105 DEG C to be dried to spot development clear
It is clear, in sample chromatogram, on reference medicine chromatography corresponding position, show the spot of same color.
In step (1), the discrimination method of the Radix Glycyrrhizae are as follows: take this product 3g, add methanol 30ml, be ultrasonically treated 20~60 points
Clock, filtrate are evaporated, and residue is dissolved in water, and are extracted 3 times with the petroleum ether of 10~40ml respectively, combining water layer, respectively with 20~
50ml ethyl acetate extracts 2 times, and acetic acid ethyl acetate extract is evaporated, and residue adds methanol 2ml to make to dissolve, as test solution；Claim
Extracting liquorice control medicinal material adds methanol to be ultrasonically treated 20~60 minutes, and filtrate is evaporated, and residue is dissolved in water, respectively with 10~30ml
Ethyl acetate extracts 2 times, and combined ethyl acetate liquid is evaporated, and residue adds methanol to make to dissolve, as control medicinal material solution；According to thin layer
2015 editions four general rules 0502 tests of chromatography Chinese Pharmacopoeia, draw test solution, each 10 μ l of control medicinal material solution, respectively point
In on same silica gel g thin-layer plate, taking out and dry after being unfolded in solvent, spray color developing agent, 105 DEG C to be dried to spot development clear,
In sample chromatogram, on reference medicine chromatography corresponding position, the spot of same color is shown.
In step (2), the high-efficient liquid phase chromatogram condition of the amarogentin are as follows: use with octadecylsilane chemically bonded silica
For the chromatographic column of filler, using volume ratio be 15~25: 75~85-0.05% phosphate aqueous solution of methanol as mobile phase, detection
Wavelength is 210nm, and number of theoretical plate is calculated by amarogentin peak is not less than 6000；
The high-efficient liquid phase chromatogram condition of the ephedrine are as follows: using octadecylsilane chemically bonded silica as filler, with volume
It is mobile phase than -0.1% phosphate aqueous solution of acetonitrile for 2~8: 92~98, Detection wavelength 210nm, number of theoretical plate is by hydrochloric acid
Ephedrine peak, which calculates, is not less than 6000；
The high performance liquid chromatography condition of the Fructus Forsythiae are as follows: it uses using octadecylsilane chemically bonded silica as filler, with
- 0.05% phosphate aqueous solution of methanol that volume ratio is 30~38: 62~70 is mobile phase, Detection wavelength 330nm, number of theoretical plate
It is calculated by forsythiaside A peak and is not less than 5000.
In step (2), the high performance liquid chromatography discrimination method of the amarogentin are as follows: weigh amarogentin reference substance, essence
It is close weighed, add 50% methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；This product 0.2g is taken to be added 50~80%
Methanol 25ml is ultrasonically treated 10~30 minutes, the weight of less loss is supplied with 50~80% methanol, is shaken up, and takes filtrate to get for examination
Product solution；Amarogentin reference substance solution, each 10 μ l of test solution are drawn, injection liquid chromatograph is measured；It is described small
In the imperial relieving cough and asthma particle of infantile paralysis containing semen armeniacae amarae and peach kernel in terms of amarogentin, content must not be less than 3.9mg/g.
In step (2), the high performance liquid chromatography discrimination method of the ephedrine are as follows: weigh ephedrine hydrochloride reference substance and salt
Sour pseudoephedrine control product, it is accurately weighed, add the dissolution of 50% methanol that every 1ml ephedrine hydrochloride containing 0.04mg and 0.01mg salt is made
The mixed solution of sour pseudoephedrine is to get reference substance solution；Weigh this product, precision be added containing 1.0~2.0% phosphoric acid 50~
80% methanol 25ml is ultrasonically treated 10~40 minutes, and the weight of less loss is supplied with 50~80% methanol containing 1.0~2.0% phosphoric acid
Amount, takes subsequent filtrate to get test solution；Precision draws reference substance solution, each 10 μ l of test solution, injects liquid chromatogram
Instrument is measured；It is total in the relieving cough and asthma particle of the small infantile paralysis dragon containing Chinese ephedra in terms of ephedrine hydrochloride and pseudoephedrine hydrochloride
Must not measure less than 0.5mg/g.
In step (2), the high performance liquid chromatography discrimination method of the forsythiaside A are as follows: forsythiaside A reference substance is weighed,
It is accurately weighed, add the dissolution of 50% methanol that forsythiaside A solution of every 1ml containing 0.05mg is made to get reference substance solution；Weigh this
50~80% methanol 25ml are added in product, are ultrasonically treated 10~40 minutes, the weight of less loss is supplied with 50~80% methanol, is shaken up,
Take subsequent filtrate to get test solution；Precision draw forsythiaside A reference substance, each 10 μ l of test sample, injection liquid chromatograph into
Row measurement；In the relieving cough and asthma particle of the small infantile paralysis dragon containing Fructus Forsythiae in terms of Forsythoside, content must not be less than 0.07mg/g.
Compared with the prior art, the present invention has the following beneficial effects:
(1) present invention is using the thin-layered chromatography improved to pheretima in the relieving cough and asthma particle of small infantile paralysis dragon, loguat leaf, sweet
Grass carries out Qualitive test, and obtained indentification by TLC clear spot is negative noiseless, as a result more satisfied and repeated, steady
It is qualitative good；
(2) present invention utilizes ephedrine hydrochloride, bitter apricot in the relieving cough and asthma particle of the small infantile paralysis dragon of high effective liquid chromatography for measuring
The content of benevolence glycosides and forsythiaside A, this method have many advantages, such as good separating effect, sensitive, accurate, ensure that the quality of this product is steady
Determine homogeneity and curative effect；
(3) method of quality control of the invention is simple, specificity is strong, favorable reproducibility, has effectively ensured that small infantile paralysis dragon is stopped
Cloperastine breathes heavily the quality and curative effect of particle, has very strong practicability.
Detailed description of the invention
Fig. 1 is the thin-layer chromatogram of pheretima in embodiment 1, wherein 1 be negative controls, 2 be reference substance, 3-5 is for trying
Product；
Fig. 2 is the thin-layer chromatogram of loguat leaf in embodiment 2, wherein 1 be reference substance, 2 be negative controls, 3-5 is confession
Test product；
Fig. 3 is the thin-layer chromatogram of Radix Glycyrrhizae in embodiment 3, wherein 1 be reference substance, 2 be negative controls, 3-5 is for trying
Product；
Fig. 4 is the high-efficient liquid phase chromatogram of amarogentin reference substance in embodiment 4；
Fig. 5 is the high-efficient liquid phase chromatogram of amarogentin test sample in embodiment 4；
Fig. 6 is the high-efficient liquid phase chromatogram of amarogentin feminine gender test sample in embodiment 4；
Fig. 7 is the high-efficient liquid phase chromatogram of ephedrine hydrochloride and pseudoephedrine hydrochloride reference substance in embodiment 5；
Fig. 8 is the high-efficient liquid phase chromatogram of 5 Ephedrine test sample of embodiment；
Fig. 9 is the high-efficient liquid phase chromatogram of 5 Ephedrine feminine gender test sample of embodiment；
Figure 10 is the high-efficient liquid phase chromatogram of forsythiaside A reference substance in embodiment 6；
Figure 11 is the high-efficient liquid phase chromatogram of forsythiaside A test sample in embodiment 6；
Figure 12 is the high-efficient liquid phase chromatogram of forsythiaside A feminine gender test sample in embodiment 6.
Specific embodiment
Agilent1100 high performance liquid chromatograph, including G1310A modular pump, G1313A autosampler, G1314A
VWD detector, CO-201 column oven, Agilent chromatographic work station；AB204-N type electronic analytical balance (METTLER
TOLEDO)。
Methanol used is chromatographically pure, other reagents are that analysis is pure, and solution uses 0.45 μm of filter membrane filtration；Control medicinal material
Dragon, loguat leaf and Radix Glycyrrhizae are purchased from National Institute for Food and Drugs Control.
Embodiment 1
(1) 0.5g pheretima control medicinal material is weighed, 20ml methanol is added, is ultrasonically treated 40 minutes, lets cool, is filtered, filtrate is steamed
Dry, residue adds methanol 2ml to dissolve to obtain control medicinal material solution；
(2) weigh 6g it is finely ground after the relieving cough and asthma particle of small infantile paralysis dragon, add 20ml water to dissolve, with chloroform 30ml, surpass
It sonication 50 minutes, lets cool, divides and take chloroform soln, be evaporated, residue adds methanol 1ml to dissolve, as test solution；
(3) weigh 3g it is finely ground after pheretima negative sample, according to step (2) the method operate, it is molten as negative control
Liquid；
(4) according to thin-layered chromatography (2015 editions four general rules 0502 of Chinese Pharmacopoeia), take test solution, control medicinal material molten
Liquid and negative each 10 μ l of test solution, put respectively on same silica gel g thin-layer plate, with n-butanol-glacial acetic acid-water (5: 1.5:
1) it is solvent, is unfolded, take out, dry, sprays with ninhydrin solution, 105 DEG C to be dried to spot development clear.
Identification result on reference medicine chromatography corresponding position, shows phase as shown in Figure 1, in sample chromatogram
With the spot of color；In negative control chromatography and on reference medicine chromatography corresponding position, the spot of no same color.
Embodiment 2
(1) 1g loguat leaf control medicinal material is weighed, adds 20ml water, refluxing extraction 60 minutes, lets cool, is filtered, 1% hydrogen of filtrate
Sodium hydroxide solution tune PH=11 is extracted 2 times with ethyl acetate, and each 30ml, ethyl acetate extracting solution is evaporated, and residue adds methanol
0.5ml dissolution, as control medicinal material solution；
(2) weigh 6g it is finely ground after the relieving cough and asthma particle of small infantile paralysis dragon, add water 20ml to dissolve, with 1% sodium hydroxide solution
PH=11 is adjusted, is extracted 2 times with ethyl acetate, each 30ml, ethyl acetate extracting solution is evaporated, and residue adds methanol 0.5ml to dissolve, and is made
For test solution；
(3) it is finely ground to weigh 2.5g loguat leaf negative sample, is operated according to step (2) the method, it is molten as negative control
Liquid；
(4) it is tested according to thin-layered chromatography (2015 editions four general rules 0502 of Chinese Pharmacopoeia), draws test solution, control
Medicinal material solution and negative each 10 μ l of test solution are put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (5
: 4: 4) lower layer's solution is solvent, is unfolded, and takes out, dries, and sprays 10% phosphomolybdic acid ethanol solution, 105 DEG C are dried to spot development
Clearly.
Identification result shows the spot of same color as shown in Fig. 2, in sample chromatogram and on reference medicine chromatography corresponding position
Point；In negative control chromatography and on reference medicine chromatography corresponding position, the spot of no same color.
Embodiment 3
(1) 0.5g Radix Glycyrrhizae control medicinal material is weighed, methanol 30ml is added, is ultrasonically treated 50 minutes, lets cool, is filtered, filtrate is evaporated,
Residue adds water 20ml to dissolve, and is extracted with ethyl acetate 2 times, each 30ml, combined ethyl acetate liquid is evaporated, and residue adds methanol 2ml
Make to dissolve, as control medicinal material solution；
(2) weigh 3g it is finely ground after the relieving cough and asthma particle of small infantile paralysis dragon, add methanol 30ml, be ultrasonically treated 50 minutes, let cool,
Filtration, filtrate are evaporated, and residue adds water 20ml to dissolve, and are extracted 3 times, each 40ml with (60-90 DEG C) of petroleum ether, and it is standby to merge aqueous layer
With, be extracted with ethyl acetate 2 times, each 40ml, combined ethyl acetate extracting solution is evaporated, and residue adds methanol 2ml to make to dissolve, make
For test solution；
(3) weigh 1.5g it is finely ground after Radix Glycyrrhizae negative sample, according to step (2) the method operate, as negative control
Solution；
(4) according to 2015 editions four general rules 0502 of thin-layered chromatography Chinese Pharmacopoeia) test, draw test solution, control
Medicinal material solution and each 10 μ l of negative control solution are put respectively on same silica gel g thin-layer plate, with chloroform-methanol-acetic acid second
Ester-formic acid-water (16: 5: 4: 0.3: 0.15) is solvent, is unfolded, and takes out, dries, and sprays 10% ethanol solution of sulfuric acid, 105 DEG C of bakings
It is clear to spot development.
Identification result, on reference medicine chromatography corresponding position, shows same color as shown in figure 3, in sample chromatogram
Spot；In negative control chromatography and on reference medicine chromatography corresponding position, the spot of no same color.
Embodiment 4
(1) amarogentin reference substance (purity is in terms of 85.8%) 12.49mg is weighed, the dissolution of 50% methanol is added concentration is made to be
The amarogentin reference substance stock solution of 0.50mg/ml；Amarogentin reference substance stock solution 2.0ml is drawn again, sets 10ml amount
In bottle, with 50% methanol dilution to scale, shake up to get reference substance solution；
(2) this product under content uniformity item is taken, it is finely ground, 0.2g is taken, it is accurately weighed, it sets in stuffed conical flask, is added 60%
Methanol 25ml, close plug, weighed weight are ultrasonically treated 30 minutes, let cool, then weighed weight, the weight of less loss is supplied with 60% methanol
Amount, shakes up, and 0.45 μm of miillpore filter filtration takes subsequent filtrate to get test solution；
(3) this product prescription preparation method is pressed, the negative granules of scarce bitter almond and peach kernel are made, by step (2) the method system
It is standby to obtain negative test solution；
(4) amarogentin reference substance solution, test solution, each 10 μ l of negative test solution are drawn, liquid is injected separately into
Chromatography is measured, wherein the condition of high performance liquid chromatography are as follows: with Dikma Diamonsil-C18 (4.6mm × 250mm,
5 μm) it is chromatographic column, with -0.05% phosphate aqueous solution of methanol (15: 85) is mobile phase, Detection wavelength 210nm, volume flow
30 DEG C of 1.0ml/min, column temperature.
Obtained reference substance solution, test solution, negative test solution chromatogram are respectively such as Fig. 4~6, as a result table
Bright: under the chromatographic condition, the chromatographic peak peak shape of amarogentin is good in reference substance solution；Amarogentin is corresponding in test solution
Chromatographic peak peak shape at retention time is good, and the separating degree of amarogentin chromatographic peak and impurity peaks is greater than 1.5；Negative test sample is molten
Occur at the corresponding retention time of amarogentin chromatographic peak without chromatographic peak in liquid, the chromatographic condition specificity is good.
Embodiment 5
(1) ephedrine hydrochloride reference substance 10.12mg is weighed, adds methanol dissolution that the salt that concentration is 0.405mg/ml is made tingle
Yellow alkali reference substance stock solution weighs pseudoephedrine hydrochloride reference substance 6.25mg, and adding methanol dissolution that concentration is made is 0.250mg/
The pseudoephedrine hydrochloride reference substance stock solution of ml；Precision draws ephedrine hydrochloride reference substance stock solution 1.0ml and hydrochloric acid is pseudo-
Ephedrine reference substance stock solution 0.5ml, sets in 10ml measuring bottle, with 50% methanol dilution to scale, shakes up molten to get reference substance
Liquid；
(2) this product under content uniformity item is weighed, it is finely ground, 1.0g is taken, it is accurately weighed, it sets in stuffed conical flask, precision adds
Enter to contain 60% methanol 25ml of 2.0% phosphoric acid, close plug, weighed weight is ultrasonically treated 20 minutes, lets cool, then weighed weight, with containing
60% methanol of 2.0% phosphoric acid supplies the weight of less loss, shakes up, and 0.45 μm of miillpore filter filtration takes subsequent filtrate to get test sample
Solution；
(3) this product prescription preparation method is pressed, the negative granules of scarce taste Chinese ephedra are made, yin is prepared by step (2) the method
Property test solution；
(4) accurate to draw reference substance solution, test solution and each 10 μ l of negative test solution, inject liquid chromatograph
It is measured, wherein chromatographic condition uses Dikma Diamonsil-C18 (4.6mm × 250mm, 5 μm) chromatographic column, with acetonitrile-
0.1% phosphate aqueous solution (triethylamine 0.2ml is added in every 100ml) (8: 92) is mobile phase, Detection wavelength 210nm, volume
Flow 1.0ml/min, 30 DEG C of column temperature.
Obtained reference substance solution, test solution and negative test solution chromatogram are respectively such as Fig. 7~9, as a result
Show: under the chromatographic condition, the chromatographic peak peak shape of ephedrine hydrochloride and pseudoephedrine hydrochloride is good in reference substance solution；Test sample
Chromatographic peak peak shape in solution at ephedrine hydrochloride and the corresponding retention time of pseudoephedrine hydrochloride is good, ephedrine hydrochloride and hydrochloric acid
The separating degree of pseudoephedrine chromatographic peak and impurity peaks is greater than 1.5；In ephedrine hydrochloride and the pseudo- fiber crops of hydrochloric acid in negative test solution
Occur at the corresponding retention time of yellow alkaline color spectral peak without chromatographic peak, the chromatographic condition specificity is good.
Embodiment 6
(1) precision weighs forsythiaside A reference substance 12.42mg (purity is in terms of 94.1%), adds methanol dissolution that concentration is made
For the forsythiaside A reference substance stock solution of 0.497mg/ml.Precision draws forsythiaside A reference substance stock solution 1.0ml, sets
In 10ml measuring bottle, with 50% methanol dilution to scale, shake up to get reference substance solution；
(2) this product under content uniformity item is taken, it is finely ground, about 0.7g is taken, it is accurately weighed, it sets in stuffed conical flask, precision adds
Enter 80% methanol 25ml, close plug, weighed weight is ultrasonically treated 30 minutes, lets cool, then weighed weight, supplied and subtracted with 70% methanol
The weight of mistake, shakes up, and 0.45 μm of miillpore filter filtration takes subsequent filtrate to get test solution；
(3) this product prescription preparation method is pressed, the negative granules of scarce taste Fructus Forsythiae medicinal material are made, are prepared by step (2) the method
To negative test solution；
(4) accurate to draw forsythiaside A reference substance, test sample and each 10 μ l of negative control solution, inject liquid chromatograph
It is measured, high-efficient liquid phase chromatogram condition uses Dikma Diamonsil-C18 (4.6mm × 250mm, 5 μm) chromatographic column, Yi Jia
- 0.05% phosphate aqueous solution of alcohol (38: 62) is mobile phase, Detection wavelength 330nm, volume flow 1.0ml/min, column temperature 30
℃。
Obtained reference substance solution, test solution and negative control solution chromatogram respectively as shown in Figure 10~12,
The result shows that: under the chromatographic condition, the chromatographic peak peak shape of forsythiaside A is good in reference substance solution；Fructus Forsythiae in test solution
Chromatographic peak peak shape at the corresponding retention time of ester glycosides A is good, and the separating degree of forsythiaside A chromatographic peak and impurity peaks is greater than 1.5；Yin
Property test solution in occur at the corresponding retention time of forsythiaside A chromatographic peak without chromatographic peak, the chromatographic condition specificity is good
It is good.
Claims (10)
1. a kind of method of quality control of the relieving cough and asthma particle of small infantile paralysis dragon, includes the following steps:
(1) Qualitive test is carried out to pheretima, loguat leaf and Radix Glycyrrhizae in the relieving cough and asthma particle of small infantile paralysis dragon using thin-layered chromatography；
(2) using high performance liquid chromatography in the relieving cough and asthma particle of small infantile paralysis dragon active constituent amarogentin, ephedrine and
Forsythiaside A carries out quantitative identification；
In step (1), chromatographic condition that the pheretima identifies are as follows: using pheretima as control medicinal material, with volume ratio be 3~7: 0.5~
1.5: 1 n-butanol-glacial acetic acid-water is that solvent develops the color using ninhydrin solution as color developing agent at 105 DEG C；
The chromatographic condition that the loguat leaf identifies are as follows: be 3~6: 4~8: 2~5 with volume ratio using loguat leaf as control medicinal material
Chloroform-methanol-water lower layer's solution is solvent, using 10% phosphomolybdic acid ethanol solution as color developing agent, is shown at 105 DEG C
Color；
The chromatographic condition that the Radix Glycyrrhizae identifies are as follows: using Radix Glycyrrhizae as control medicinal material, with volume ratio for 15~22: 4~8: 2~4: 0.2
~0.6: 0.15 chloroform-methanol-ethyl acetate-formic acid-water is solvent, is colour developing with 10% ethanol solution of sulfuric acid
Agent develops the color at 105 DEG C.
2. the method for quality control of the relieving cough and asthma particle of small infantile paralysis dragon according to claim 1, which is characterized in that step
(1) in, the discrimination method of the pheretima are as follows: it takes this product 6g to be dissolved in water, adds chloroform and be ultrasonically treated 20~60 minutes,
Dividing takes filtrate to be evaporated, and residue adds 1ml methanol to dissolve, as test solution；Separately take pheretima control medicinal material that 20~60ml first is added
Alcohol is ultrasonically treated 20~60 minutes, and filtrate is evaporated, and residue adds methanol to dissolve, as control medicinal material solution；According in thin-layered chromatography
2015 editions four general rules 0502 tests of state's pharmacopeia, draw test solution, each 10 μ l of control medicinal material solution, are put respectively in same silicon
On glue G lamellae, takes out and dry after being unfolded in solvent, spray color developing agent, 105 DEG C to be dried to spot development clear, in test sample
In chromatography, on reference medicine chromatography corresponding position, the spot of same color is shown.
3. the method for quality control of the relieving cough and asthma particle of small infantile paralysis dragon according to claim 1, which is characterized in that step
(1) in, the discrimination method of the loguat leaf are as follows: take this product 6g to be dissolved in water, with 1% sodium hydroxide solution adjust pH value to 8~
11, it is extracted 2 times, is evaporated with 15~30ml ethyl acetate respectively, residue adds 0.5ml methanol to dissolve, as test solution；Take Pi
Rake leaf control medicinal material, adds water refluxing extraction 30~60 minutes, filtrate 1% sodium hydroxide solution adjusting pH value to 8~11, respectively
It is extracted 2 times, is evaporated, residue adds methanol to dissolve, as control medicinal material solution with 15~30ml ethyl acetate；According in thin-layered chromatography
2015 editions four general rules 0502 tests of state's pharmacopeia, draw test solution, each 10 μ l of control medicinal material solution, are put respectively in same silicon
On glue G lamellae, takes out and dry after being unfolded in solvent, spray color developing agent, 105 DEG C to be dried to spot development clear, in test sample
In chromatography, on reference medicine chromatography corresponding position, the spot of same color is shown.
4. the method for quality control of the relieving cough and asthma particle of small infantile paralysis dragon according to claim 1, which is characterized in that step
(1) in, the discrimination method of the Radix Glycyrrhizae are as follows: take this product 3g, add methanol 30ml, be ultrasonically treated 20~60 minutes, filtrate is evaporated, residual
Slag is dissolved in water, and is extracted 3 times with the petroleum ether of 10~40ml respectively, combining water layer, extracts 2 with 20~50ml ethyl acetate respectively
Secondary, acetic acid ethyl acetate extract is evaporated, and residue adds methanol 2ml to make to dissolve, as test solution；Radix Glycyrrhizae control medicinal material is weighed, is added
Methanol is ultrasonically treated 20~60 minutes, and filtrate is evaporated, and residue is dissolved in water, and is extracted 2 times with 10~30ml ethyl acetate respectively, is closed
And acetic acid ethyl fluid, it is evaporated, residue adds methanol to make to dissolve, as control medicinal material solution；According to thin-layered chromatography Chinese Pharmacopoeia 2015
Four general rules 0502 of version are tested, and are drawn test solution, each 10 μ l of control medicinal material solution, are put respectively in same silica gel g thin-layer plate
On, taking out and dry after being unfolded in solvent, spray color developing agent, 105 DEG C to be dried to spot development clear, in sample chromatogram, with
On reference medicine chromatography corresponding position, the spot of same color is shown.
5. the method for quality control of the relieving cough and asthma particle of small infantile paralysis dragon according to claim 1, which is characterized in that step
(2) in, the high-efficient liquid phase chromatogram condition of the amarogentin are as follows: use the color using octadecylsilane chemically bonded silica as filler
Compose column, using volume ratio be 15~25: 75~85-0.05% phosphate aqueous solution of methanol as mobile phase, Detection wavelength 210nm,
Number of theoretical plate is calculated by amarogentin peak is not less than 6000.
6. the method for quality control of the relieving cough and asthma particle of small infantile paralysis dragon according to claim 1, which is characterized in that step
(2) in, the high-efficient liquid phase chromatogram condition of the ephedrine are as follows: using octadecylsilane chemically bonded silica as filler, with volume ratio
- 0.1% phosphate aqueous solution of acetonitrile for 2~8: 92~98 is mobile phase, and Detection wavelength 210nm, it is tingle that number of theoretical plate presses salt
Yellow alkali peak, which calculates, is not less than 6000.
7. the method for quality control of the relieving cough and asthma particle of small infantile paralysis dragon according to claim 1, which is characterized in that step
(2) in, the high performance liquid chromatography condition of the Fructus Forsythiae are as follows: use using octadecylsilane chemically bonded silica as filler, with body
Product is mobile phase than -0.05% phosphate aqueous solution of methanol for being 30~38: 62~70, and Detection wavelength 330nm, number of theoretical plate is pressed
Forsythiaside A peak, which calculates, is not less than 5000.
8. the method for quality control of the relieving cough and asthma particle of small infantile paralysis dragon according to claim 5, which is characterized in that step
(2) in, the high performance liquid chromatography discrimination method of the amarogentin are as follows: amarogentin reference substance is weighed, it is accurately weighed, add 50%
Solution of every 1ml containing 0.1mg is made to get reference substance solution in methanol；Take this product 0.2g that 50~80% methanol 25ml, ultrasound is added
Processing 10~30 minutes, the weight of less loss is supplied with 50~80% methanol, is shaken up, takes filtrate to get test solution；It draws bitter
Each 10 μ l of almond glycosides reference substance solution, test solution, injection liquid chromatograph are measured；The small infantile paralysis dragon is relieving cough and asthma
In particle containing semen armeniacae amarae and peach kernel in terms of amarogentin, content must not be less than 3.9mg/g.
9. the method for quality control of the relieving cough and asthma particle of small infantile paralysis dragon according to claim 6, which is characterized in that step
(2) in, the high performance liquid chromatography discrimination method of the ephedrine are as follows: weigh ephedrine hydrochloride reference substance and pseudoephedrine hydrochloride pair
It is accurately weighed according to product, add the dissolution of 50% methanol that every 1ml ephedrine hydrochloride containing 0.04mg and 0.01mg pseudoephedrine hydrochloride is made
Mixed solution is to get reference substance solution；This product is weighed, 50~80% methanol 25ml for containing 1.0~2.0% phosphoric acid are added in precision,
Ultrasonic treatment 10~40 minutes supplies the weight of less loss with 50~80% methanol containing 1.0~2.0% phosphoric acid, takes subsequent filtrate, i.e.,
Obtain test solution；Precision draws reference substance solution, each 10 μ l of test solution, injects liquid chromatograph, is measured；It is described
In the relieving cough and asthma particle of small infantile paralysis dragon containing Chinese ephedra in terms of ephedrine hydrochloride and pseudoephedrine hydrochloride, total amount must not be less than 0.5mg/
g。
10. the method for quality control of the relieving cough and asthma particle of small infantile paralysis dragon according to claim 7, which is characterized in that step
(2) in, the high performance liquid chromatography discrimination method of the forsythiaside A are as follows: forsythiaside A reference substance is weighed, it is accurately weighed, add
Forsythiaside A solution of every 1ml containing 0.05mg is made to get reference substance solution in the dissolution of 50% methanol；Weigh this product, it is added 50~
80% methanol 25ml is ultrasonically treated 10~40 minutes, the weight of less loss is supplied with 50~80% methanol, is shaken up, takes subsequent filtrate, i.e.,
Obtain test solution；Precision draws forsythiaside A reference substance, each 10 μ l of test sample, and injection liquid chromatograph is measured；It is described
In the relieving cough and asthma particle of small infantile paralysis dragon containing Fructus Forsythiae in terms of forsythiaside A, content must not be less than 0.07mg/g.
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