CN109991359A - A kind of method of quality control of the Chinese medicine composition with cough-suppressing phlegm-dispelling functions - Google Patents
A kind of method of quality control of the Chinese medicine composition with cough-suppressing phlegm-dispelling functions Download PDFInfo
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Abstract
The present invention relates to a kind of method of quality control of the Chinese medicine composition of specific cough-relieving apophlegmatic, the Chinese medicine composition is had disclosed.Specifically, the present invention is to be related to the quality control of the discrimination method and content assaying method of the Chinese medicine composition of this cough-relieving apophlegmatic.The chemical component of volatile oil and assay has been carried out in present invention applicant's system research this product, so that it is determined that the quality control standard of volatile oil of the present invention, so that this product requisite quality method is specific and accurate, the model of Chinese medicine composition and its preparation quality standard of the research containing volatile oil is established.
Description
Technical field
The present invention relates to a kind of method of quality control of the Chinese medicine composition of specific cough-relieving apophlegmatic.
Background technique
Chinese medicine composition according to the present invention, by ardisia japonica, loguat leaf, Chinese ephedra, semen armeniacae amarae, peppermint, dried orange peel, caulis bambusae in taenian,
Cordate houttuynia, radix glycyrrhizae preparata, 9 taste Chinese medicinal compositions.With cough-suppressing phlegm-dispelling functions, for the Chinese medicine exterior syndrome of cough and asthma, real example, heat symptom-complex,
Syndrome of superficies cold and interior heat and set.Acute bronchitis, acute exacerbation of chronic bronchitis etc. can be treated.
The present composition is authorized, Patent No. in application on March 24th, 2009 Chinese invention patent:
ZL200910048132.0.Although needing to prepare this method invention described above provide the preparation method of the composition
Product carries out quality control, to guarantee the stability and controllability of product quality, simultaneously because the particularity of tcm product Quality Control,
The quality control method is specially required again with specificity.
Summary of the invention
Present invention aims at the method for quality control for disclosing a kind of Chinese medicine composition with cough-suppressing phlegm-dispelling functions, this hairs
It is bright to be achieved by the following technical solution:
A kind of method of quality control of the Chinese medicine composition with cough-suppressing phlegm-dispelling functions, including to discrimination method and assay side
The quality of method controls.
A kind of method of quality control of the Chinese medicine composition with cough-suppressing phlegm-dispelling functions, using Bergenin, loguat leaf, salt
Sour ephedrine, aurantiamarin, benzaldehyde, methylnonanone, menthol, limonene are reference substance, carry out the control of discrimination method quality.
A kind of method of quality control of the Chinese medicine composition with cough-suppressing phlegm-dispelling functions, using Bergenin, hydrochloric acid Chinese ephedra
Alkali and pseudoephedrine hydrochloride, benzaldehyde are reference substance, carry out the control of content assaying method quality.
The advantages of invention
At qualitative aspect, ardisia japonica, loguat leaf, Chinese ephedra, dried orange peel thin layer are identified, volatile oil in semen armeniacae amarae, peppermint and cordate houttuynia
Discrimination method, the discrimination method of benzaldehyde is included in quality control standard in semen armeniacae amarae；At quantitative aspect, to Chinese ephedra, ardisia japonica,
The composition measurement of volatile oil representativeness is included in quality control standard in semen armeniacae amarae, peppermint and cordate houttuynia.These combine the present invention
Object all has specificity and feasibility, can effectively ensure the quality of this composition.
Chinese medicine composition quality research is conventional not to carry out quality control to volatile oil, and present invention applicant's system research
In this product the chemical component of volatile oil and assay is carried out, so that it is determined that the quality control standard of volatile oil of the present invention,
So that this product requisite quality method is specific and accurate, Chinese medicine composition and its preparation quality standard of the research containing volatile oil are established
Model.
Specific embodiment
Embodiment 1[discrimination method]
This product 1ml is taken, adds methanol 20ml, shakes up, is filtered, filtrate is concentrated into about 2ml, as test solution.Separately take purple bergenia herb
Plain reference substance adds methanol that solution of every 1ml containing 0.5mg is made, as reference substance solution.It is tested according to thin-layered chromatography, in absorption
Each 5 μ l of two kinds of solution is stated, is put respectively on same silica gel g thin-layer plate, is with chloroform-acetate-methanol (5:4:2)
Solvent is unfolded, and takes out, dries, and sprays with the mixed solution of -1% potassium ferricyanide of 1% ferric trichloride (1:1).In sample chromatogram,
At the position corresponding to the chromatogram of the reference substance, the spot of same color is shown.
Embodiment 2[discrimination method]
This product 5ml is taken, water-saturated n-butanol shaking is added to extract 4 times, each 10ml, merges n-butanol liquid, ammonification test solution washing 2
Secondary, each 20ml merges n-butanol liquid, is evaporated, residue adds water 5ml to make to dissolve, and lets cool, and passes through D101 type large pore resin absorption column
(internal diameter 1.5cm, long 8cm) discards aqueous with water 50ml elution, then is eluted to Diluted Alcohol colourless, collects eluent, is evaporated,
Residue adds methanol 1ml to make to dissolve, as test solution.Loguat leaf control medicinal material 1g separately is taken, adds water 100ml, is decocted 1 hour,
Filtration, filtrate is with being made in the same way of control medicinal material solution.It is tested according to thin-layered chromatography, draws each 20 μ l of above two solution, respectively
Point with cyclohexane-ethyl acetate-glacial acetic acid (8:4:0.1) for solvent, is unfolded on same silica gel g thin-layer plate, takes out, dry in the air
It is dry, it sprays with 5% vanillin-sulfuric acid solution, it is clear to be heated to spot development at 105 DEG C.In sample chromatogram, with control medicinal material
On the corresponding position of chromatography, the spot of same color is shown.
Embodiment 3[discrimination method]
Take this product 10ml, few drops of enriching ammonia solution, then plus chloroform extraction 2 times, each 10ml, merge chloroform, be evaporated,
Residue adds methanol 1ml to make to dissolve, and filtration, filtrate is as test solution.Ephedrine hydrochloride reference substance separately is taken, methanol is added to be made
Solution of every 1ml containing 0.5mg, as reference substance solution.It is tested according to thin-layered chromatography, draws each 5 μ l of above two solution, point
Other point, with chloroform-methanol-strong ammonia solution (20:5:0.5) for solvent, is unfolded on same silica gel g thin-layer plate,
It takes out, dries, spray with ninhydrin solution, it is clear to be heated to spot development at 105 DEG C.In sample chromatogram, with reference substance color
It composes on corresponding position, shows identical punctation.
Embodiment 4[discrimination method]
This product 20ml is taken, sets and is steamed near dry in water-bath, diatomite 10g is added to grind well, adds ethyl alcohol 30ml, is ultrasonically treated 20 minutes, puts
Cold, filtration, filtrate is concentrated into about 5ml, as test solution；Aurantiamarin reference substance separately is taken, adds methanol that saturated solution is made, is made
For reference substance solution.It is tested according to thin-layered chromatography, draws each 10 μ l of above two solution, put respectively in same with 0.5% hydroxide
On the silica gel g thin-layer plate of sodium solution preparation, with acetate-methanol-water (100:17:13) for solvent, it is unfolded, takes out, dry in the air
Dry, spray is set and is inspected under ultraviolet lamp (365nm) with hot blast drying with 1% alchlor methanol solution.In sample chromatogram,
On position corresponding with reference substance chromatography, the fluorescence spot of same color is shown.
Embodiment 5[discrimination method]
This product 5ml is taken, is set in 10ml measuring bottle, adds ethyl acetate ultrasound 15min, shakes up, stands, takes supernatant molten as test sample
Liquid.Benzaldehyde reference substance separately is taken, adds ethyl acetate that solution of every ml containing 1mg is made, as reference substance solution.It is accurate respectively to draw
Above-mentioned each 1 μ l of solution injects gas chromatograph, measures according to gas chromatography.Chromatographic condition: being solid with crosslinking bonding polyethylene glycol
Determine the chromatographic column (30m*320 μm, 0.25 μm) of phase；Injector temperature: 250 DEG C；Detector temperature: 270 DEG C；Split sampling, point
Flow ratio: 20:1；Carrier gas: nitrogen, flow velocity: 1ml/min；Temperature programming: with 50 DEG C of holding 10min, then with the rate liter of 5 DEG C/min
To 150 DEG C.Test solution is respectively with reference substance solution in identical retention time appearance.
Embodiment 6[discrimination method]
It takes semen armeniacae amarae, volatile oil 0.1ml in peppermint and cordate houttuynia, sets in 10ml measuring bottle, add ethyl acetate constant volume, shake up as confession
Test sample solution.Benzaldehyde, methylnonanone, menthol, limonene reference substance separately are taken, adds ethyl acetate that every ml is made containing above-mentioned right
According to the solution of each 1mg of product, as reference substance solution.It is accurate respectively to draw above-mentioned each 1 μ l of solution, gas chromatograph is injected, according to gas
Phase chromatography measurement.Chromatographic condition: using crosslinking bonding polyethylene glycol as the chromatographic column (30m*320 μm, 0.25 μm) of stationary phase；Into
Sample mouth temperature: 250 DEG C；Detector temperature: 270 DEG C；Split sampling, split ratio: 20:1；Carrier gas: nitrogen, flow velocity: 1ml/min；
Temperature programming: with 50 DEG C of holding 10min, then with the rate of 5 DEG C/min 150 DEG C are raised to.Test solution respectively with reference substance
Solution is in identical retention time appearance.
Embodiment 7[ardisia japonica assay]
Chromatographic condition and system suitability are using octadecylsilane chemically bonded silica as filler；With acetonitrile-water (12:88)
For mobile phase；Flow velocity 1.0ml/min；Detection wavelength is 275nm.Theoretical cam curve should be not less than by the calculating of Bergenin peak
3000。
The preparation of reference substance solution takes Bergenin reference substance appropriate, accurately weighed, adds methanol that every 1ml is made containing 25 μ g's
Solution to get.
The preparation precision of test solution measures this product 1ml, sets neutral alumina column (100 ~ 200 mesh, 1g, internal diameter 1cm)
On, eluted with methanol, collect eluent about 30ml, set in 50ml measuring bottle, with methanol dilution to scale, shake up, filtration to get.
Measuring method is accurate respectively to draw reference substance solution and 20 μ l of test solution, injects liquid chromatograph, measures, meter
It calculates, the every 1ml of this product is containing ardisia japonica with Bergenin (C14H16O9) meter, 1.1mg must not be less than.
Embodiment 8[Chinese ephedra assay]
Chromatographic condition and system suitability are using octadecylsilane chemically bonded silica as filler, with acetonitrile: 0.1% phosphoric acid
(4:96) is mobile phase, Detection wavelength 207nm.Number of theoretical plate should not be low by ephedrine hydrochloride and the calculating of pseudoephedrine hydrochloride peak
In 3000.
The preparation precision of reference substance solution weighs ephedrine hydrochloride reference substance 10mg, pseudoephedrine hydrochloride 15mg, respectively
It sets in 100ml measuring bottle, scale is dissolved and be diluted to methanol, is shaken up.The above-mentioned ephedrine hydrochloride solution 5ml of the accurate measurement of difference,
Pseudoephedrine hydrochloride solution 1ml is set in same 50ml measuring bottle, is diluted to scale with mobile phase, is shaken up to get (every 1ml is hydrochloric
Ephedrine 10 μ g and 3 μ g of pseudoephedrine hydrochloride).
The preparation precision of test solution measures this product 1ml, sets in separatory funnel, and ammonium hydroxide 5ml is added, shakes up, then plus second
Ether extracts 5 times, each 10ml, merges ether solution, and 5% methanol hydrochloride solution 5ml is added, shakes up, 40 DEG C of water-bath recycling designs are residual
Slag adds mobile phase to make to dissolve, and is quantitatively transferred in 25ml measuring bottle, adds mobile phase to be diluted to scale, shakes up, filtration to get.
Measuring method is accurate respectively to draw reference substance solution and 20 μ l of test solution, injects liquid chromatograph, measures, meter
It calculates, the every 1ml of this product is containing Chinese ephedra with ephedrine hydrochloride (C10H15NOHCl) with pseudoephedrine hydrochloride (C10H15NOHCl it) counts, no
It obtains and is less than 0.30mg.
Embodiment 9[volatile oil content testing]
Chromatographic condition: using crosslinking bonding polyethylene glycol as the chromatographic column (30m*320 μm, 0.25 μm) of stationary phase；Injector temperature:
250℃；Detector temperature: 270 DEG C；Split sampling, split ratio: 20:1；Carrier gas: nitrogen, flow velocity: 1ml/min；Temperature programming:
With 50 DEG C of holding 10min, then with the rate of 5 DEG C/min it is raised to 150 DEG C.
The preparation of reference substance solution takes benzaldehyde reference substance 10mg is accurately weighed to set in 10ml measuring bottle, adds ethyl acetate molten
Solution constant volume, shakes up, to obtain the final product.
The preparation precision of test solution measures semen armeniacae amarae, volatile oil 0.5ml in peppermint and cordate houttuynia, sets 50ml measuring bottle
In, add ethyl acetate dissolution, constant volume, shake up to get.
Measuring method difference is accurate to draw reference substance solution and each 1 μ l of test solution, injects gas chromatograph, measures, this
The every 1ml of product (C containing benzaldehyde7H6O 90mg must not) be less than.
Claims (12)
1. a kind of method of quality control of the Chinese medicine composition with cough-suppressing phlegm-dispelling functions, it is characterized in that discrimination method and content
The quality of measuring method controls.
2. a kind of method of quality control of Chinese medicine composition with cough-suppressing phlegm-dispelling functions according to claim 1, special
Sign be use Bergenin, loguat leaf, ephedrine hydrochloride, aurantiamarin, benzaldehyde, methylnonanone, menthol, limonene for pair
According to product, the control of discrimination method quality is carried out.
3. a kind of method of quality control of Chinese medicine composition with cough-suppressing phlegm-dispelling functions according to claim 2, special
Sign is to use Bergenin for reference substance, method are as follows:
This product 1ml is taken, adds methanol 20ml, shakes up, is filtered, filtrate is concentrated into about 2ml, as test solution；Separately take purple bergenia herb
Plain reference substance adds methanol that solution of every 1ml containing 0.5mg is made, as reference substance solution；It is tested according to thin-layered chromatography, in absorption
Each 5 μ l of two kinds of solution is stated, is put respectively on same silica gel g thin-layer plate, is with chloroform-acetate-methanol (5:4:2)
Solvent is unfolded, and takes out, dries, and sprays with the mixed solution of -1% potassium ferricyanide of 1% ferric trichloride (1:1)；
In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown.
4. a kind of method of quality control of Chinese medicine composition with cough-suppressing phlegm-dispelling functions according to claim 2, special
Sign is to use loguat leaf for reference substance, method are as follows:
This product 5ml is taken, water-saturated n-butanol shaking is added to extract 4 times, each 10ml, merges n-butanol liquid, ammonification test solution washing 2
Secondary, each 20ml merges n-butanol liquid, is evaporated, residue adds water 5ml to make to dissolve, and lets cool, and passes through D101 type macroporous absorbent resin
Column discards aqueous with water 50ml elution, then is eluted to Diluted Alcohol colourless, collects eluent, is evaporated, residue adds methanol 1ml to make
Dissolution, as test solution；Loguat leaf control medicinal material 1g separately is taken, adds water 100ml, is decocted 1 hour, filtration, the same method of filtrate
Control medicinal material solution is made；It is tested according to thin-layered chromatography, draws each 20 μ l of above two solution, put respectively thin in same silica G
On laminate, with cyclohexane-ethyl acetate-glacial acetic acid (8:4:0.1) for solvent, it is unfolded, takes out, dry, spray with 5% vanillic aldehyde
It is clear to be heated to spot development at 105 DEG C for sulfuric acid solution；In sample chromatogram, in position corresponding with reference medicine chromatography
On, show the spot of same color.
5. a kind of method of quality control of Chinese medicine composition with cough-suppressing phlegm-dispelling functions according to claim 2, special
Sign is to use ephedrine hydrochloride for reference substance, method are as follows:
Take this product 10ml, few drops of enriching ammonia solution, then plus chloroform extraction 2 times, each 10ml, merge chloroform, be evaporated,
Residue adds methanol 1ml to make to dissolve, and filtration, filtrate is as test solution；Ephedrine hydrochloride reference substance separately is taken, methanol is added to be made
Solution of every 1ml containing 0.5mg, as reference substance solution；It is tested according to thin-layered chromatography, draws each 5 μ l of above two solution, point
Other point, with chloroform-methanol-strong ammonia solution (20:5:0.5) for solvent, is unfolded on same silica gel g thin-layer plate,
It takes out, dries, spray with ninhydrin solution, it is clear to be heated to spot development at 105 DEG C；In sample chromatogram, with reference substance color
It composes on corresponding position, shows identical punctation.
6. a kind of method of quality control of Chinese medicine composition with cough-suppressing phlegm-dispelling functions according to claim 2, special
Sign is to use aurantiamarin for reference substance, method are as follows:
This product 20ml is taken, sets and is steamed near dry in water-bath, diatomite 10g is added to grind well, adds ethyl alcohol 30ml, is ultrasonically treated 20 minutes, puts
Cold, filtration, filtrate is concentrated into about 5ml, as test solution；Aurantiamarin reference substance separately is taken, adds methanol that saturated solution is made, is made
For reference substance solution；
It is tested according to thin-layered chromatography, draws above-mentioned each 10 μ l of three kinds of solution, put respectively in same with 0.5% sodium hydroxide solution system
On standby silica gel g thin-layer plate, with acetate-methanol-water (100:17:13) be solvent, be unfolded, take out, dry, spray with
1% alchlor methanol solution is set and is inspected under ultraviolet lamp (365nm) with hot blast drying；In sample chromatogram, with compare
On the corresponding position of product chromatography, the fluorescence spot of same color is shown.
7. a kind of method of quality control of Chinese medicine composition with cough-suppressing phlegm-dispelling functions according to claim 2, special
Sign is to use benzaldehyde for reference substance, method are as follows:
This product 5ml is taken, is set in 10ml measuring bottle, adds ethyl acetate ultrasound 15min, shakes up, stands, takes supernatant molten as test sample
Liquid；Benzaldehyde reference substance separately is taken, adds ethyl acetate that solution of every ml containing 1mg is made, as reference substance solution；It is accurate respectively to draw
Above-mentioned each 1 μ l of solution injects gas chromatograph, measures according to gas chromatography；
Chromatographic condition: using crosslinking bonding polyethylene glycol as the chromatographic column (30m*320 μm, 0.25 μm) of stationary phase；Injector temperature:
250℃；Detector temperature: 270 DEG C；Split sampling, split ratio: 20:1；Carrier gas: nitrogen, flow velocity: 1ml/min；Temperature programming:
With 50 DEG C of holding 10min, then with the rate of 5 DEG C/min it is raised to 150 DEG C；Test solution is respectively with reference substance solution identical
Retention time appearance.
8. a kind of method of quality control of Chinese medicine composition with cough-suppressing phlegm-dispelling functions according to claim 2, special
Sign is to use benzaldehyde, methylnonanone, menthol, limonene for reference substance, method are as follows:
Semen armeniacae amarae, peppermint and the volatile oil of cordate houttuynia 0.1ml are taken, is set in 10ml measuring bottle, adds ethyl acetate constant volume, shake up as confession
Test sample solution；Benzaldehyde, methylnonanone, menthol, limonene reference substance separately are taken, adds ethyl acetate that every ml is made containing above-mentioned right
According to the solution of each 1mg of product, as reference substance solution；It is accurate respectively to draw above-mentioned each 1 μ l of solution, gas chromatograph is injected, according to gas
Phase chromatography measurement；
Chromatographic condition: using crosslinking bonding polyethylene glycol as the chromatographic column (30m*320 μm, 0.25 μm) of stationary phase；Injector temperature:
250℃；Detector temperature: 270 DEG C；Split sampling, split ratio: 20:1；Carrier gas: nitrogen, flow velocity: 1ml/min；Temperature programming:
With 50 DEG C of holding 10min, then with the rate of 5 DEG C/min it is raised to 150 DEG C；Test solution is respectively with reference substance solution identical
Retention time appearance.
9. a kind of method of quality control of Chinese medicine composition with cough-suppressing phlegm-dispelling functions according to claim 1, special
Sign is to use Bergenin, ephedrine hydrochloride and pseudoephedrine hydrochloride, benzaldehyde for reference substance, carries out content assaying method quality
Control.
10. a kind of method of quality control of Chinese medicine composition with cough-suppressing phlegm-dispelling functions according to claim 9, special
Sign is that Bergenin is used to measure ardisia japonica content, method for reference substance are as follows:
Using octadecylsilane chemically bonded silica as filler；With acetonitrile-water (12:88) for mobile phase；Flow velocity 1.0ml/min；Inspection
Survey wavelength is 275nm；Theoretical cam curve is calculated by Bergenin peak should be not less than 3000；
The preparation of reference substance solution: taking Bergenin reference substance, accurately weighed, adds methanol that the solution that every 1ml contains 25 μ g is made, i.e.,
?；
The preparation of test solution: precision measures this product 1ml, sets on neutral alumina column (100 ~ 200 mesh, 1g, internal diameter 1cm),
Eluted with methanol, collect eluent about 30ml, set in 50ml measuring bottle, with methanol dilution to scale, shake up, filtration to get；
Measuring method: it is accurate respectively to draw reference substance solution and 20 μ l of test solution, liquid chromatograph is injected, is measured, is calculated, this
The every 1ml of product in terms of Bergenin, must not be less than 1.1mg containing ardisia japonica.
11. a kind of method of quality control of Chinese medicine composition with cough-suppressing phlegm-dispelling functions according to claim 9, special
Sign is that ephedrine hydrochloride and pseudoephedrine hydrochloride is used to measure Chinese ephedra content, method for reference substance are as follows:
Using octadecylsilane chemically bonded silica as filler, with acetonitrile: 0.1% phosphoric acid (4:96) is mobile phase, and Detection wavelength is
207nm；Number of theoretical plate is calculated by ephedrine hydrochloride and pseudoephedrine hydrochloride peak should be not less than 3000；
The preparation of reference substance solution: taking ephedrine hydrochloride, pseudoephedrine hydrochloride reference substance, accurately weighed, and methanol is added to be respectively prepared
The solution of every hydrochloric ephedrine 10ug and ephedrine hydrochloride 3ug of 1ml to get；
The preparation of test solution: precision measures this product 1ml, sets in separatory funnel, and ammonium hydroxide 5ml is added, shakes up, then the extraction that adds diethyl ether
It takes 5 times, each 10ml, merges ether solution, 5% methanol hydrochloride solution 5ml is added, shakes up, 40 DEG C of water-bath recycling designs, residue adds
Mobile phase makes to dissolve, and is quantitatively transferred in 25ml measuring bottle, adds mobile phase to be diluted to scale, shakes up, filtration to get；
Measuring method: it is accurate respectively to draw reference substance solution and 20 μ l of test solution, liquid chromatograph is injected, is measured, is calculated, this
The every 1ml of product in terms of ephedrine hydrochloride and pseudoephedrine hydrochloride, must not be less than 0.30mg containing Chinese ephedra.
12. a kind of method of quality control of Chinese medicine composition with cough-suppressing phlegm-dispelling functions according to claim 9, special
Sign is to use benzaldehyde for volatile oil content in reference substance measurement semen armeniacae amarae, peppermint and cordate houttuynia, method are as follows:
Chromatographic condition: using crosslinking bonding polyethylene glycol as the chromatographic column (30m*320 μm, 0.25 μm) of stationary phase；Injector temperature:
250℃；Detector temperature: 270 DEG C；Split sampling, split ratio: 20:1；Carrier gas: nitrogen, flow velocity: 1ml/min；Temperature programming:
With 50 DEG C of holding 10min, then with the rate of 5 DEG C/min it is raised to 150 DEG C；
The preparation of reference substance solution: taking benzaldehyde reference substance, accurately weighed, adds ethyl acetate that solution of every ml containing 1mg is made i.e.
?；
The preparation of test solution: volatile oil 0.5ml in precision measurement semen armeniacae amarae, peppermint and cordate houttuynia sets in 50ml measuring bottle, adds
Ethyl acetate dissolution, constant volume, shake up to get；
Measuring method: accurate absorption reference substance solution and each 1 μ l of test solution respectively, injection gas chromatograph, measurement, this product are every
1ml must not be less than 90mg containing benzaldehyde.
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