A kind of quality of production control method of intensified loquet distillate
Technical field
The present invention relates to medicine quality of production detection technique field, and in particular to a kind of quality of production control of intensified loquet distillate
Method processed.
Background technology
Intensified loquet distillate main component is:Loquat leaf, pappy shell, the tuber of stemona, Cynanchum glaucescens, the root bark of white mulberry, balloonflower root, menthol.Auxiliary material
For sodium benzoate, Steviosin, citric acid, flavoring pineapple essence, it is mainly used in yin-nourishing and astringes the lung, cough-relieving apophlegmatic is used for bronchitis cough,
Chinese medicines quasi-word Z45020167
The content of the invention
It is an object of the invention to provide a kind of quality of production control method of intensified loquet distillate, so as to more comprehensive
The accurately quality of production, detection and control intensified loquet distillate.
The present invention is achieved by the following technical programs:
A kind of quality of production control method of intensified loquet distillate:This method includes production control method, method of quality control;
Production control method:
Loguat leaf 69g, pappy shell 50g, tuber of stemona 15g, Cynanchum glaucescens 9g, root bark of white mulberry 6g, balloonflower root 6g is taken to add water to cook three times, every time
1.5h, collecting decoction, filtration, about 750ml is concentrated into, adds sodium benzoate 2.5g, is stirred to dissolve, adds sucrose 600g, continue to add
Heat is kept for 20 minutes to boiling, and is stood, filtration, is added citric acid 0.5g, the essence and menthol 0.15g that are dissolved with ethanol, is stirred
Mix, mix, stand, add water to 1000ml, mix, produce;
Method of quality control:
A, discrimination method:Intensified loquet distillate 80ml is taken, is extracted 2 times, each 50ml with the n-butanol shaking of ammonia solution saturation,
Merge n-butanol extracting liquid, washed with the water 50ml of n-butanol saturation, discard water lotion, divide and take n-butanol layer, be evaporated, residue adds
Ethanol 1ml makes dissolving, as need testing solution;Loguat leaf control medicinal material 2g is taken, adds water 50ml, is heated to reflux 1h, let cool, use cotton
Flower filtration, takes filtrate, with the n-butanol shaking extraction 2 times, each 30ml of ammonia solution saturation, is merging the same of n-butanol extracting liquid
When, using being made in the same way of loguat leaf control medicinal material solution;Cynanchum glaucescens control medicinal material 1g is taken, is made in the same way of Cynanchum glaucescens control medicinal material solution;
Above-mentioned each 4-8 μ l of three kinds of solution are drawn according to thin-layered chromatography, are put respectively on same silica gel g thin-layer plate, with 5:2 toluene-
Acetone is solvent, is deployed, and takes out, dries, be placed under 365nm ultraviolet lamp and inspect;In test sample chromatogram, with Cynanchum glaucescens pair
According on the corresponding position of medicinal material chromatogram, show the fluorescence spot of same color;Spray is added with 20% phosphomolybdic acid ethanol solution at 105 DEG C
Heat is clear to spot development, is inspected under daylight, in test sample chromatogram, on position corresponding with loguat leaf control medicinal material chromatogram,
The spot of aobvious same color;Pappy shell control medicinal material 2g is taken, is made in the same way of control medicinal material solution.Tested according to thin-layered chromatography,
Cynanchum glaucescens control medicinal material solution and each 4-8 μ l of pappy shell medicinal material solution are taken, is put respectively on same silica gel g thin-layer plate, with 5:2 first
Benzene-acetone is solvent, is deployed, and takes out, dries, spray with dilute bismuth potassium iodide test solution;In test sample chromatogram, with comparison medicine wood color
Compose on corresponding position, show the spot of same color;
B, content detection:It is measured according to high performance liquid chromatography, including it is chromatographic condition and system suitability, right
The preparation of preparation, need testing solution according to product solution, measure.
In the step b chromatographic condition and system suitability be using octyl silane group silica gel as filler, with
Acetonitrile -0.01mol/L dipotassium hydrogen phosphate solution -0.005mol/L heptane sulfonic acid sodium salts are according to 20:40:40 volume ratio is stream
Dynamic phase, Detection wavelength 220nm, number of theoretical plate calculate >=2000 by morphine peak.
The preparation of reference substance solution is to take morphine reference substance is accurately weighed to put in brown measuring bottle in the step b, is added containing 5%
The solution that every 1ml contains 24 μ g is made in 20% methanol solution of acetic acid, produces.
The preparation of need testing solution is that precision measures intensified loquet distillate 3ml in the step b, is put in 10ml brown measuring bottles,
20% methanol solution containing 5% acetic acid is added to shake up to scale, filtered, produced with 0.45 μm of miillpore filter.
Measure is that precision draws reference substance solution and each 10 μ l of need testing solution respectively in the step b, injects liquid phase color
Spectrometer, determine and produce.
The intensified loquet distillate per 1ml containing pappy shell in terms of morphine >=15 μ g.
The beneficial effects of the present invention are:Production control method, discrimination method, content detection is respectively adopted to strong in this method
Power loquat dew carries out quality of production control, and it has the characteristics that, and stability is strong, measurement is accurate, speed is fast, more comprehensively, is a kind of excellent
Intensified loquet distillate quality of production control method.
Embodiment
Technical scheme is further described below in conjunction with specific embodiment, but claimed scope is not
It is confined to described.
Embodiment one
A kind of quality of production control method of intensified loquet distillate:This method includes production control method, method of quality control;
Production control method:
Loguat leaf 69g, pappy shell 50g, tuber of stemona 15g, Cynanchum glaucescens 9g, root bark of white mulberry 6g, balloonflower root 6g is taken to add water to cook three times, every time
1.5h, collecting decoction, filtration, about 750ml is concentrated into, adds sodium benzoate 2.5g, is stirred to dissolve, adds sucrose 600g, continue to add
Heat is kept for 20 minutes to boiling, and is stood, filtration, is added citric acid 0.5g, the essence and menthol 0.15g that are dissolved with ethanol, is stirred
Mix, mix, stand, add water to 1000ml, mix, produce;
Method of quality control:
A, discrimination method:Intensified loquet distillate 80ml is taken, is extracted 2 times, each 50ml with the n-butanol shaking of ammonia solution saturation,
Merge n-butanol extracting liquid, washed with the water 50ml of n-butanol saturation, discard water lotion, divide and take n-butanol layer, be evaporated, residue adds
Ethanol 1ml makes dissolving, as need testing solution;Loguat leaf control medicinal material 2g is taken, adds water 50ml, is heated to reflux 1h, let cool, use cotton
Flower filtration, takes filtrate, with the n-butanol shaking extraction 2 times, each 30ml of ammonia solution saturation, is merging the same of n-butanol extracting liquid
When, using being made in the same way of loguat leaf control medicinal material solution;Cynanchum glaucescens control medicinal material 1g is taken, is made in the same way of Cynanchum glaucescens control medicinal material solution;
Above-mentioned each 4 μ l of three kinds of solution are drawn according to thin-layered chromatography, are put respectively on same silica gel g thin-layer plate, with 5:2 toluene-the third
Ketone is solvent, is deployed, and takes out, dries, be placed under 365nm ultraviolet lamp and inspect;In test sample chromatogram, compareed with Cynanchum glaucescens
On the corresponding position of medicinal material chromatogram, show the fluorescence spot of same color;Spray is with 20% phosphomolybdic acid ethanol solution, in 105 DEG C of heating
It is clear to spot development, inspect under daylight, in test sample chromatogram, on position corresponding with loguat leaf control medicinal material chromatogram, show
The spot of same color;Pappy shell control medicinal material 2g is taken, is made in the same way of control medicinal material solution.Test, take according to thin-layered chromatography
Cynanchum glaucescens control medicinal material solution and each 4 μ l of pappy shell medicinal material solution, put respectively on same silica gel g thin-layer plate, with 5:2 toluene-
Acetone is solvent, is deployed, and takes out, dries, spray with dilute bismuth potassium iodide test solution;In test sample chromatogram, with control medicinal material chromatogram
On corresponding position, show the spot of same color;
B, content detection:It is measured according to high performance liquid chromatography, chromatographic condition and system suitability:With octane
Base silane bonded silica gel is filler, molten with acetonitrile -0.01mol/L dipotassium hydrogen phosphate solution -0.005mol/L sodium heptanesulfonates
Liquid is according to 20:40:40 volume ratio is mobile phase, and Detection wavelength 220nm, number of theoretical plate is by morphine peak calculating >=2000;It is right
According to the preparation of product solution;Take morphine reference substance is accurately weighed to put in brown measuring bottle, add 20% methanol solution containing 5% acetic acid to be made
Contain 24 μ g solution per 1ml, produce;The preparation of need testing solution:Precision measures intensified loquet distillate 3ml, puts 10ml brown measuring bottles
In, add 20% methanol solution containing 5% acetic acid to shake up to scale, filtered, produced with 0.45 μm of miillpore filter;Measure:Essence respectively
Close absorption reference substance solution and each 10 μ l of need testing solution, inject liquid chromatograph, determine and produce, intensified loquet distillate contains per 1ml
Pappy shell in terms of morphine >=15 μ g.
Embodiment two
A kind of quality of production control method of intensified loquet distillate:This method includes production control method, method of quality control;
Production control method:
Loguat leaf 69g, pappy shell 50g, tuber of stemona 15g, Cynanchum glaucescens 9g, root bark of white mulberry 6g, balloonflower root 6g is taken to add water to cook three times, every time
1.5h, collecting decoction, filtration, about 750ml is concentrated into, adds sodium benzoate 2.5g, is stirred to dissolve, adds sucrose 600g, continue to add
Heat is kept for 20 minutes to boiling, and is stood, filtration, is added citric acid 0.5g, the essence and menthol 0.15g that are dissolved with ethanol, is stirred
Mix, mix, stand, add water to 1000ml, mix, produce;
Method of quality control:
A, discrimination method:Intensified loquet distillate 80ml is taken, is extracted 2 times, each 50ml with the n-butanol shaking of ammonia solution saturation,
Merge n-butanol extracting liquid, washed with the water 50ml of n-butanol saturation, discard water lotion, divide and take n-butanol layer, be evaporated, residue adds
Ethanol 1ml makes dissolving, as need testing solution;Loguat leaf control medicinal material 2g is taken, adds water 50ml, is heated to reflux 1h, let cool, use cotton
Flower filtration, takes filtrate, with the n-butanol shaking extraction 2 times, each 30ml of ammonia solution saturation, is merging the same of n-butanol extracting liquid
When, using being made in the same way of loguat leaf control medicinal material solution;Cynanchum glaucescens control medicinal material 1g is taken, is made in the same way of Cynanchum glaucescens control medicinal material solution;
Above-mentioned each 6 μ l of three kinds of solution are drawn according to thin-layered chromatography, are put respectively on same silica gel g thin-layer plate, with 5:2 toluene-the third
Ketone is solvent, is deployed, and takes out, dries, be placed under 365nm ultraviolet lamp and inspect;In test sample chromatogram, compareed with Cynanchum glaucescens
On the corresponding position of medicinal material chromatogram, show the fluorescence spot of same color;Spray is with 20% phosphomolybdic acid ethanol solution, in 105 DEG C of heating
It is clear to spot development, inspect under daylight, in test sample chromatogram, on position corresponding with loguat leaf control medicinal material chromatogram, show
The spot of same color;Pappy shell control medicinal material 2g is taken, is made in the same way of control medicinal material solution.Test, take according to thin-layered chromatography
Cynanchum glaucescens control medicinal material solution and each 6 μ l of pappy shell medicinal material solution, put respectively on same silica gel g thin-layer plate, with 5:2 toluene-
Acetone is solvent, is deployed, and takes out, dries, spray with dilute bismuth potassium iodide test solution;In test sample chromatogram, with control medicinal material chromatogram
On corresponding position, show the spot of same color;
B, content detection:It is measured according to high performance liquid chromatography, chromatographic condition and system suitability:With octane
Base silane bonded silica gel is filler, molten with acetonitrile -0.01mol/L dipotassium hydrogen phosphate solution -0.005mol/L sodium heptanesulfonates
Liquid is according to 20:40:40 volume ratio is mobile phase, and Detection wavelength 220nm, number of theoretical plate is by morphine peak calculating >=2000;It is right
According to the preparation of product solution;Take morphine reference substance is accurately weighed to put in brown measuring bottle, add 20% methanol solution containing 5% acetic acid to be made
Contain 24 μ g solution per 1ml, produce;The preparation of need testing solution:Precision measures intensified loquet distillate 3ml, puts 10ml brown measuring bottles
In, add 20% methanol solution containing 5% acetic acid to shake up to scale, filtered, produced with 0.45 μm of miillpore filter;Measure:Essence respectively
Close absorption reference substance solution and each 10 μ l of need testing solution, inject liquid chromatograph, determine and produce, intensified loquet distillate contains per 1ml
Pappy shell in terms of morphine >=15 μ g.
Embodiment three
A kind of quality of production control method of intensified loquet distillate:This method includes production control method, method of quality control;
Production control method:
Loguat leaf 69g, pappy shell 50g, tuber of stemona 15g, Cynanchum glaucescens 9g, root bark of white mulberry 6g, balloonflower root 6g is taken to add water to cook three times, every time
1.5h, collecting decoction, filtration, about 750ml is concentrated into, adds sodium benzoate 2.5g, is stirred to dissolve, adds sucrose 600g, continue to add
Heat is kept for 20 minutes to boiling, and is stood, filtration, is added citric acid 0.5g, the essence and menthol 0.15g that are dissolved with ethanol, is stirred
Mix, mix, stand, add water to 1000ml, mix, produce;
Method of quality control:
A, discrimination method:Intensified loquet distillate 80ml is taken, is extracted 2 times, each 50ml with the n-butanol shaking of ammonia solution saturation,
Merge n-butanol extracting liquid, washed with the water 50ml of n-butanol saturation, discard water lotion, divide and take n-butanol layer, be evaporated, residue adds
Ethanol 1ml makes dissolving, as need testing solution;Loguat leaf control medicinal material 2g is taken, adds water 50ml, is heated to reflux 1h, let cool, use cotton
Flower filtration, takes filtrate, with the n-butanol shaking extraction 2 times, each 30ml of ammonia solution saturation, is merging the same of n-butanol extracting liquid
When, using being made in the same way of loguat leaf control medicinal material solution;Cynanchum glaucescens control medicinal material 1g is taken, is made in the same way of Cynanchum glaucescens control medicinal material solution;
Above-mentioned each 8 μ l of three kinds of solution are drawn according to thin-layered chromatography, are put respectively on same silica gel g thin-layer plate, with 5:2 toluene-the third
Ketone is solvent, is deployed, and takes out, dries, be placed under 365nm ultraviolet lamp and inspect;In test sample chromatogram, compareed with Cynanchum glaucescens
On the corresponding position of medicinal material chromatogram, show the fluorescence spot of same color;Spray is with 20% phosphomolybdic acid ethanol solution, in 105 DEG C of heating
It is clear to spot development, inspect under daylight, in test sample chromatogram, on position corresponding with loguat leaf control medicinal material chromatogram, show
The spot of same color;Pappy shell control medicinal material 2g is taken, is made in the same way of control medicinal material solution.Test, take according to thin-layered chromatography
Cynanchum glaucescens control medicinal material solution and each 8 μ l of pappy shell medicinal material solution, put respectively on same silica gel g thin-layer plate, with 5:2 toluene-
Acetone is solvent, is deployed, and takes out, dries, spray with dilute bismuth potassium iodide test solution;In test sample chromatogram, with control medicinal material chromatogram
On corresponding position, show the spot of same color;
B, content detection:It is measured according to high performance liquid chromatography, chromatographic condition and system suitability:With octane
Base silane bonded silica gel is filler, molten with acetonitrile -0.01mol/L dipotassium hydrogen phosphate solution -0.005mol/L sodium heptanesulfonates
Liquid is according to 20:40:40 volume ratio is mobile phase, and Detection wavelength 220nm, number of theoretical plate is by morphine peak calculating >=2000;It is right
According to the preparation of product solution;Take morphine reference substance is accurately weighed to put in brown measuring bottle, add 20% methanol solution containing 5% acetic acid to be made
Contain 24 μ g solution per 1ml, produce;The preparation of need testing solution:Precision measures intensified loquet distillate 3ml, puts 10ml brown measuring bottles
In, add 20% methanol solution containing 5% acetic acid to shake up to scale, filtered, produced with 0.45 μm of miillpore filter;Measure:Essence respectively
Close absorption reference substance solution and each 10 μ l of need testing solution, inject liquid chromatograph, determine and produce, intensified loquet distillate contains per 1ml
Pappy shell in terms of morphine >=15 μ g.