CN108614065A - A kind of method of quality control of mountain chrysanthemum Jiangya Granula - Google Patents
A kind of method of quality control of mountain chrysanthemum Jiangya Granula Download PDFInfo
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- CN108614065A CN108614065A CN201611157291.0A CN201611157291A CN108614065A CN 108614065 A CN108614065 A CN 108614065A CN 201611157291 A CN201611157291 A CN 201611157291A CN 108614065 A CN108614065 A CN 108614065A
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Abstract
The invention discloses a kind of method of quality control of mountain chrysanthemum Jiangya Granula, which is made of character, discriminating, inspection, assay.Wherein discriminating is the discriminating to salt rhizoma alismatis, chrysanthemum, Prunella vulgaris, field thistle and hawthorn, and assay is measured to the content of mountain chrysanthemum Jiangya Granula Content of Chlorogenic Acid using liquid chromatography.Method of quality control high sensitivity, the stability for the mountain chrysanthemum Jiangya Granula that the present invention establishes are good, quick, accurate, can ensure the quality " safe and stable, controllable " of product from many aspects.
Description
Technical field
The present invention relates to a kind of method for qualitative and quantitative detection of Chinese patent drug, specifically, the present invention relates to a kind of mountain chrysanthemum drops
Press the method for qualitative and quantitative detection of particle.
Background technology
Mountain chrysanthemum Jiangya Granula is made of hawthorn, chrysanthemum, salt rhizoma alismatis, Prunella vulgaris, field thistle, the sub- Six-element medicine of fried cassia, tool
Play the role of calming the liver.For the headache caused by hyperactivity of yang due to yin deficiency, dizziness, tinnitus is forgetful, Yao Xi Acid are soft, is not in the mood for dysphoria with smothery sensation, palpitaition
Insomnia and high blood pressure are shown in above-mentioned disease person.Mountain chrysanthemum hypertension pill that Chinese Pharmacopoeia 2005 editions records with the present invention relates to mountain chrysanthemum
Jiangya Granula has similar effect, but its taking dose is 5 pieces/times, and taking dose is big, and tablet disintegration times are long, shadow
The performance for ringing drug effect is unfavorable for patient's application.It is involved in the present invention to mountain chrysanthemum Jiangya Granula be by hawthorn, chrysanthemum, Prunella vulgaris,
Field thistle and fried cassia add water to be decocted, and are condensed into thick paste, pelletize after rhizoma alismatis fine powder, mixing is added, manufactured granule, this
Sample can not only make the extraction of medicinal material active ingredient abundant, and content increases, and solves the problems, such as that taking dose is big, and granule compared with
Tablet is easier to be conducive to absorb by human body.
Mountain chrysanthemum Jiangya Granula according to the present invention is reformed on the basis of the mountain chrysanthemum hypertension pill original dosage form that pharmacopeia is recorded
The kind developed, there is no to mountain chrysanthemum Jiangya Granula in the method for quality control of mountain chrysanthemum hypertension pill in original Chinese Pharmacopoeia
Character provided, and active ingredient discriminating it is not comprehensive the shortcomings of.Therefore the method for quality control of mountain chrysanthemum hypertension pill cannot be used
Otherwise the quality control of Yushan Hill chrysanthemum Jiangya Granula will influence the production and quality assurance of product.
In order to effectively control the quality of mountain chrysanthemum Jiangya Granula, the present invention establishes the method for quality control of the product.Respectively
The quality control of mountain chrysanthemum Jiangya Granula is established in terms of product characteristics, inspection, the discriminating of active ingredient and assay four
System.The control method comprehensively monitors the active ingredient of medicinal material, and high sensitivity, stability are good, quick, accurate, energy
Enough quality " safe and stable, controllable " for ensureing product from many aspects.Especially the present invention selects chlorogenic acid as quantitatively detecting
Object is the committed step of quality control.It is primarily due to：(1) chlorogenic acid is the active constituent of mountain chrysanthemum Jiangya Granula, has drop
The effect of blood pressure controls the content of chlorogenic acid, can control the quality of product；(2) chlorogenic acid is that hawthorn, chrysanthemum, summer are withered simultaneously
Careless, field thistle active ingredient can control the quality of four kinds of medicinal materials simultaneously by the detection to chlorogenic acid.
Invention content
In order to solve the above technical problems, the present invention provides a kind of method of quality control of mountain chrysanthemum Jiangya Granula.
The preparation prescription group of mountain chrysanthemum Jiangya Granula becomes：
【Prescription】Hawthorn 500g, chrysanthemum 83.3g, salt rhizoma alismatis 62.5g, Prunella vulgaris 62.5g, field thistle 83.3g, frying certainly
Pine torch：83.3g.
【Preparation method】The above Six-element, rhizoma alismatis powder：100 mesh fine powders, moisture≤5.0%；Remaining five tastes adds water to cook twice, often
Secondary plus 10 times of amount water, 3 hours for the first time, second 2 hours, collecting decoction, natural filtration, being concentrated under reduced pressure into relative density was
The thick paste of 1.30~1.40 (50 DEG C) is added rhizoma alismatis fine powder, mixing, vacuum drying, crushing, sieving, appropriate dextrin and sugarcane is added
Particle is made in sugar, dry, and 1000g is made；Or appropriate dextrin is added, and particle is made, it is dry, 600g (no sucrose) is made, i.e.,
.
The present invention be directed to the method for quality control that mountain chrysanthemum Jiangya Granula (including containing sucrose and no cane sugar type) proposes.Quality
Control method includes mainly four character, inspection, discriminating (including microexamination, indentification by TLC) and assay sides
Face.
Character：This product is brown granular；Sweet (containing sucrose) or sour (no sucrose), micro-puckery.
Differentiate：
Microexamination：This product is taken, microscopically observation is placed in：Parenchyma cell similar round has oval pit, integrates pit
Group；The wavy bending of endothelium confluent monolayer cells anticline, thicker, woodization have sparse pore ditch (salt rhizoma alismatis).
Indentification by TLC：
(1) take this product appropriate, it is finely ground, 5g (containing sucrose) or 3g (no sucrose) is weighed, adds methanol 20mL, is heated to reflux 15 points
Clock, filtration, filtrate are evaporated, and residue adds methanol 2mL to make dissolving, as test solution.Precision weighs galuteolin reference substance use
70% ethyl alcohol is configured to the 40 μ g/mL solution containing galuteolin, as a contrast product solution.According to thin-layered chromatography (Chinese Pharmacopoeia
The one annex VIB of version in 2005) experiment, 10 μ L of test solution are drawn, 5 μ L of reference substance solution are put thin in same silica G respectively
On laminate, using the upper solution of ethyl acetate-acetone-formic acid-water (7: 3: 1: 1.2) as solvent, it is unfolded, takes out, dry, spray
With 5% alchlor ethanol solution, sets and inspected under ultraviolet lamp (365nm).In test sample chromatography, corresponding to reference substance chromatography
Position on, show same color fluorescence spot.
(2) take this product appropriate, it is finely ground, 5g (containing sucrose) or 3g (no sucrose) is weighed, adds methanol 10mL, is ultrasonically treated 30 points
Clock, filtration, filtrate are evaporated, and residue adds methanol 2mL to make dissolving, as test solution.Separately take field thistle control medicinal material 1g, same to legal system
At control medicinal material solution.Control substance of Rutin is taken again, adds methanol that solution of every 1mL containing 0.5mg is made, as a contrast product solution.According to
Thin-layered chromatography (one annex VI B of China's coastal port) is tested, and is drawn above-mentioned each 2 μ L of three kinds of solution, is put respectively in same
On one polyamide film, with acetylacetone,2,4-pentanedione-butanone-alcohol-water (1: 3: 3: 13) be solvent, be unfolded, take out, dry, spray with
Alchlor test solution, dries, and sets and is inspected under ultraviolet lamp (365nm).In test sample chromatography, with control medicinal material and reference substance color
It composes on corresponding position, shows the fluorescence spot of same color.
(3) take this product appropriate, it is finely ground, 5g (containing sucrose) or 3g (no sucrose) is weighed, adds ethyl alcohol 20mL, it is small to be heated to reflux 1
When, filtration, filtrate is evaporated, and residue is impregnated 2 times for (30~60 DEG C) with petroleum ether, and each 15mL (about 2 minutes), incline petroleum ether
Liquid, residue adds ethyl alcohol 1mL to make dissolving, as test solution.Ursolic acid reference substance separately is taken, adds ethyl alcohol that every 1mL is made containing 1mg's
Solution, as a contrast product solution.It is tested according to thin-layered chromatography (one annex VI B of China's coastal port), draws above-mentioned two
Kind of each 2 μ L of solution, put respectively on same silica gel g thin-layer plate, with hexamethylene-chloroform-ethyl acetate-glacial acetic acid (20: 5:
8: 0.5) it is solvent, is unfolded, takes out, dry, with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot development at 100 DEG C for spray,
It sets and is inspected under daylight and ultraviolet lamp (365nm).In test sample chromatography, on position corresponding with reference substance chromatography, show respectively
Identical spot or fluorescence spot.
(4) it checks：Related every regulation (one annex I C of China's coastal port) under granule item should be met
(5) ethyl acetate extract：Take this product under content uniformity item appropriate, it is finely ground, take about 5g (containing sucrose) or 3g (nothings
Sucrose), accurately weighed, precision plus ethyl acetate 50mL, according to the hot dipping (China's coastal port one under Extract mensuration
Portion annex XA) it measures, make solvent with ethyl acetate, every bag of extract must not be less than 35.0mg.
Assay：It is measured according to high performance liquid chromatography (one annex VID of China's coastal port).
(1) chromatographic condition and system suitability test：Using octadecyl silane as filler；With -0.1% phosphorus of acetonitrile
Acid solution (10: 90) is mobile phase；Detection wavelength is 348nm.
(2) preparation of reference substance solution：Take chlorogenic acid reference substance appropriate, it is accurately weighed, add methanol that every 1mL is made and contains 150 μ
The solution of g to get.
(3) preparation of test solution：This product under content uniformity item is taken, it is finely ground, about 3g is taken, it is accurately weighed, set round bottom
In flask, methanol 50mL is added in precision, and weighed weight is heated to reflux 1 hour, puts to room temperature, then weighed weight, is supplied with methanol
The quality of less loss, shakes up, and filtration takes subsequent filtrate, with the filtration of (0.45 μm) of miillpore filter to get；
(4) accurate respectively to draw reference substance solution and each 20 μ L of test solution, inject liquid chromatograph, measure to get；
(5) every bag of (C containing chlorogenic acid of this product16H18O9) meter, 0.60mg must not be less than.
The beneficial effects of the present invention are：This method has the characteristics that high sensitivity, stability are good, quick, accurate, can
The quality of comprehensive reaction and control mountain chrysanthemum Jiangya Granula, is a kind of good quality of production control method.
Specific implementation mode
The embodiment of the present invention is described in detail below, it should be noted that the present embodiment is narrative, is not limited
, protection scope of the present invention cannot be limited with this.
Compare implementation 1
The mountain chrysanthemum Jiangya Granula that the lot number that applicant produces is 36151202 is taken to contain cane sugar type.
Character：It is brown granular to take mountain chrysanthemum Jiangya Granula one bag/5g containing cane sugar type of this lot number, observation form；Punching
Take mouthfeel：Sweet, micro-puckery.
Differentiate：
Microexamination：The mountain chrysanthemum Jiangya Granula product containing cane sugar type for taking this lot number, is placed in microscopically observation：Thin-walled is thin
Born of the same parents' similar round has oval pit, integrates integrated pit group；The wavy bending of endothelium confluent monolayer cells anticline, thicker, woodization have sparse thin
Hole ditch (salt rhizoma alismatis).
Indentification by TLC：
(1) take the mountain chrysanthemum Jiangya Granula product containing cane sugar type of this lot number appropriate, it is finely ground, 5g is weighed, adds methanol 20mL, adds
Heat reflux 15 minutes, filtration, filtrate is evaporated, and residue adds methanol 2mL to make dissolving, as test solution.Precision weighs reseda
Glycosides reference substance is configured to the 40 μ g/mL solution containing galuteolin with 70% ethyl alcohol, as a contrast product solution.According to thin-layered chromatography
(one annex VI B of China's coastal port) test, draw 10 μ L of test solution, 5 μ L of reference substance solution, put respectively in
On same silica gel g thin-layer plate, using the upper solution of ethyl acetate-acetone-formic acid-water (7: 3: 1: 1.2) as solvent, expansion,
It takes out, dries, spray with 5% alchlor ethanol solution, set and inspected under ultraviolet lamp (365nm).In test sample chromatography, with it is right
According on the corresponding position of product chromatography, the fluorescence spot of same color is shown.
(2) take the mountain chrysanthemum Jiangya Granula product containing cane sugar type of this lot number appropriate, it is finely ground, 5g is weighed, methanol 10mL is added, is surpassed
Sonication 30 minutes, filtration, filtrate are evaporated, and residue adds methanol 2mL to make dissolving, as test solution.Separately take field thistle comparison medicine
Material 1g is made in the same way of control medicinal material solution.Control substance of Rutin is taken again, adds methanol that solution of every 1mL containing 0.5mg is made, as right
According to product solution.It is tested according to thin-layered chromatography (one annex VI B of China's coastal port), draws above-mentioned each 2 μ of three kinds of solution
L is put respectively on same polyamide film, and with acetylacetone,2,4-pentanedione-butanone-alcohol-water (1: 3: 3: 13) for solvent, expansion takes
Go out, dry, sprays with alchlor test solution, dry, set and inspected under ultraviolet lamp (365nm).In test sample chromatography, with comparison medicine
On material and the corresponding position of reference substance chromatography, the fluorescence spot of same color is shown.
(3) take the mountain chrysanthemum Jiangya Granula product containing cane sugar type of this lot number appropriate, it is finely ground, 5g is weighed, adds ethyl alcohol 20mL, adds
Heat reflux 1 hour, filtration, filtrate is evaporated, and residue is impregnated 2 times for (30~60 DEG C) with petroleum ether, and each 15mL (about 2 minutes) is inclined
Petroleum ether liquid is removed, residue adds ethyl alcohol 1mL to make dissolving, as test solution.Ursolic acid reference substance separately is taken, ethyl alcohol is added to be made often
Solution of the 1mL containing 1mg, as a contrast product solution.It is tested according to thin-layered chromatography (one annex VI B of China's coastal port),
Each 2 μ L of above two solution are drawn, are put respectively on same silica gel g thin-layer plate, with hexamethylene-chloroform-ethyl acetate-ice
Acetic acid (20: 5: 8: 0.5) is solvent, is unfolded, and takes out, dries, and sprays with 10% ethanol solution of sulfuric acid, spot is heated at 100 DEG C
Point colour developing is clear, sets and is inspected under daylight and ultraviolet lamp (365nm).In test sample chromatography, in position corresponding with reference substance chromatography
It sets, shows identical fluorescence spot respectively.
Ethyl acetate extract：Take the mountain chrysanthemum Jiangya Granula product containing cane sugar type of this lot number appropriate, it is finely ground, about 5g is taken,
It is accurately weighed, precision plus ethyl acetate 50mL, according to hot dipping (one annex of China's coastal port under Extract mensuration
XA it) measures, makees solvent with ethyl acetate, it is 38.4mg to measure extract.
Assay：It is measured according to high performance liquid chromatography (one annex VID of China's coastal port).
(1) chromatographic condition and system suitability test：Using octadecyl silane as filler；With -0.1% phosphorus of acetonitrile
Acid solution (10: 90) is mobile phase；Detection wavelength is 348nm.
(2) preparation of reference substance solution：Take chlorogenic acid reference substance appropriate, it is accurately weighed, add methanol that every 1mL is made and contains 150 μ
The solution of g to get.
(3) preparation of test solution：This product under content uniformity item is taken, it is finely ground, about 5g is taken, it is accurately weighed, set round bottom
In flask, methanol 50mL is added in precision, and weighed weight is heated to reflux 1 hour, puts to room temperature, then weighed weight, is supplied with methanol
The quality of less loss, shakes up, and filtration takes subsequent filtrate, with the filtration of (0.45 μm) of miillpore filter to get；
(4) accurate respectively to draw reference substance solution and each 20 μ L of test solution, inject liquid chromatograph, measure to get；
(5) every bag of (C containing chlorogenic acid of this product16H18O9) it is 0.66mg.
Compare implementation 2
Take the mountain chrysanthemum Jiangya Granula no cane sugar type that the lot number that applicant produces is 36150604.
Character：It is brown granular to take the mountain chrysanthemum Jiangya Granula one bag/3g of no cane sugar type of this lot number, observation form；Punching
Take mouthfeel：Sour, micro-puckery.
Differentiate：
Microexamination：The mountain chrysanthemum Jiangya Granula no cane sugar type product for taking this lot number, is placed in microscopically observation：Thin-walled is thin
Born of the same parents' similar round has oval pit, integrates integrated pit group；The wavy bending of endothelium confluent monolayer cells anticline, thicker, woodization have sparse thin
Hole ditch (salt rhizoma alismatis).
Indentification by TLC：
Take the mountain chrysanthemum Jiangya Granula no cane sugar type product of this lot number appropriate, it is finely ground, 3g is weighed, methanol 20mL is added, is heated
Reflux 15 minutes, filtration, filtrate are evaporated, and residue adds methanol 2mL to make dissolving, as test solution.Precision weighs galuteolin
Reference substance is configured to the 40 μ g/mL solution containing galuteolin with 70% ethyl alcohol, as a contrast product solution.According to thin-layered chromatography (in
One annex VI B of state's pharmacopeia version in 2005) experiment, 10 μ L of test solution are drawn, 5 μ L of reference substance solution are put in same respectively
On silica gel g thin-layer plate, using the upper solution of ethyl acetate-acetone-formic acid-water (7: 3: 1: 1.2) as solvent, it is unfolded, takes out,
It dries, sprays with 5% alchlor ethanol solution, set and inspected under ultraviolet lamp (365nm).In test sample chromatography, with reference substance
On the corresponding position of chromatography, the fluorescence spot of same color is shown.
Take the mountain chrysanthemum Jiangya Granula no cane sugar type product of this lot number appropriate, it is finely ground, 3g is weighed, methanol 10mL is added, ultrasound
Processing 30 minutes, filtration, filtrate are evaporated, and residue adds methanol 2mL to make dissolving, as test solution.Separately take field thistle control medicinal material
1g is made in the same way of control medicinal material solution.Control substance of Rutin is taken again, adds methanol that solution of every 1mL containing 0.5mg is made, as a contrast
Product solution.It is tested according to thin-layered chromatography (one annex VI B of China's coastal port), draws above-mentioned each 2 μ L of three kinds of solution,
It is put respectively on same polyamide film, with acetylacetone,2,4-pentanedione-butanone-alcohol-water (1: 3: 3: 13) for solvent, is unfolded, takes out,
It dries, sprays with alchlor test solution, dry, set and inspected under ultraviolet lamp (365nm).In test sample chromatography, with control medicinal material
On the corresponding position of reference substance chromatography, the fluorescence spot of same color is shown.
Take the mountain chrysanthemum Jiangya Granula no cane sugar type product of this lot number appropriate, it is finely ground, 3g is weighed, ethyl alcohol 20mL is added, is heated
Reflux 1 hour, filtration, filtrate are evaporated, and residue is impregnated 2 times for (30~60 DEG C) with petroleum ether, and each 15mL (about 2 minutes) is inclined
Petroleum ether liquid, residue adds ethyl alcohol 1mL to make dissolving, as test solution.Ursolic acid reference substance separately is taken, adds ethyl alcohol that every 1mL is made
Solution containing 1mg, as a contrast product solution.It tests, inhales according to thin-layered chromatography (one annex VI B of China's coastal port)
Each 2 μ L of above two solution are taken, are put respectively on same silica gel g thin-layer plate, with hexamethylene-chloroform-ethyl acetate-ice vinegar
Sour (20: 5: 8: 0.5) is solvent, is unfolded, and takes out, dries, and sprays with 10% ethanol solution of sulfuric acid, spot is heated at 100 DEG C
Colour developing is clear, sets and is inspected under daylight and ultraviolet lamp (365nm).In test sample chromatography, in position corresponding with reference substance chromatography
On, identical fluorescence spot is shown respectively.
Ethyl acetate extract：Take the mountain chrysanthemum Jiangya Granula no cane sugar type product of this lot number appropriate, it is finely ground, 3g is weighed,
It is accurately weighed, precision plus ethyl acetate 50mL, according to hot dipping (one annex of China's coastal port under Extract mensuration
XA it) measures, makees solvent with ethyl acetate, it is 36.2mg to measure extract.
Assay：It is measured according to high performance liquid chromatography (one annex VID of China's coastal port).
(1) chromatographic condition and system suitability test：Using octadecyl silane as filler；With -0.1% phosphorus of acetonitrile
Acid solution (10: 90) is mobile phase；Detection wavelength is 348nm.
(2) preparation of reference substance solution：Take chlorogenic acid reference substance appropriate, it is accurately weighed, add methanol that every 1mL is made and contains 150 μ
The solution of g to get.
(3) preparation of test solution：This product under content uniformity item is taken, it is finely ground, about 3g is taken, it is accurately weighed, set round bottom
In flask, methanol 50mL is added in precision, and weighed weight is heated to reflux 1 hour, puts to room temperature, then weighed weight, is supplied with methanol
The quality of less loss, shakes up, and filtration takes subsequent filtrate, with the filtration of (0.45 μm) of miillpore filter to get；
(4) accurate respectively to draw reference substance solution and each 20 μ L of test solution, inject liquid chromatograph, measure to get；
(5) every bag of (C containing chlorogenic acid of this product16H18O9) it is 0.64mg.
Compare implementation 3
It is respectively 36150201,36150203,36150204,36151201,36151202 to take the lot number that applicant produces
Mountain chrysanthemum Jiangya Granula five batches, check.Wherein, granularity is double with reference to one annex XI the second method of B of China's coastal port
Sieve method measures；Moisture is measured with reference to one annex IX H determination of moisture method of China's coastal port；The measurement of melting：
1 bag of test sample is taken, water 200mL is heated, stirs 5 minutes, observes solution state immediately；Content uniformity reference Chinese Pharmacopoeia 2005
One annex I C of version is carried out；The detection of microorganism is carried out with reference to one annex XIII C of China's coastal port.
Inspection result meets regulation, is shown in Table 1.
1 five batches of sample inspection results of table
Claims (3)
1. a kind of method of quality control of mountain chrysanthemum Jiangya Granula, this method from product characteristics, inspection, the discriminating of active ingredient and
Four aspects of assay establish the quality control system of mountain chrysanthemum Jiangya Granula.Specifically detection method is：
Character：This product is brown granular；Sweet (containing sucrose) or sour (no sucrose), micro-puckery.
Differentiate：
(1) microexamination：This product is taken, microscopically observation is placed in：Parenchyma cell similar round has oval pit, integrates pit
Group；The wavy bending of endothelium confluent monolayer cells anticline, thicker, woodization have sparse pore ditch (salt rhizoma alismatis).
(2) indentification by TLC：
A, take this product appropriate, it is finely ground, 5g (containing sucrose) or 3g (no sucrose) is weighed, adds methanol 20mL, is heated to reflux 15 minutes, filter
It crosses, filtrate is evaporated, and residue adds methanol 2mL to make dissolving, as test solution.Precision weighs galuteolin reference substance with 70%
Ethyl alcohol is configured to the 40 μ g/mL solution containing galuteolin, as a contrast product solution.According to thin-layered chromatography (China's coastal port
One annex VI B) experiment, 10 μ L of test solution, 5 μ L of reference substance solution are drawn, is put respectively on same silica gel g thin-layer plate,
Using the upper solution of ethyl acetate-acetone-formic acid-water (7: 3: 1: 1.2) as solvent, it is unfolded, takes out, dry, sprays with 5%
Alchlor ethanol solution is set and is inspected under ultraviolet lamp (365nm).In test sample chromatography, in position corresponding with reference substance chromatography
On, show the fluorescence spot of same color.
B, take this product appropriate, it is finely ground, 5g (containing sucrose) or 3g (no sucrose) is weighed, adds methanol 10mL, is ultrasonically treated 30 minutes, filter
It crosses, filtrate is evaporated, and residue adds methanol 2mL to make dissolving, as test solution.Field thistle control medicinal material 1g separately is taken, is made in the same way of pair
According to medicinal material solution.Control substance of Rutin is taken again, adds methanol that solution of every 1mL containing 0.5mg is made, as a contrast product solution.According to thin layer
Chromatography (one annex VI B of China's coastal port) is tested, and above-mentioned each 2 μ L of three kinds of solution are drawn, and is put respectively in same poly-
On amide film, with acetylacetone,2,4-pentanedione-butanone-alcohol-water (1: 3: 3: 13) for solvent, it is unfolded, takes out, dry, spray with trichlorine
Change aluminium test solution, dries, set and inspected under ultraviolet lamp (365nm).In test sample chromatography, with control medicinal material and reference substance chromatography phase
On the position answered, the fluorescence spot of same color is shown.
C, take this product appropriate, it is finely ground, 5g (containing sucrose) or 3g (no sucrose) is weighed, adds ethyl alcohol 20mL, is heated to reflux 1 hour, filter
It crosses, filtrate is evaporated, and residue is impregnated 2 times for (30~60 DEG C) with petroleum ether, and each 15mL (about 2 minutes), incline petroleum ether liquid, residue
Ethyl alcohol 1mL is added to make dissolving, as test solution.Ursolic acid reference substance separately is taken, adds ethyl alcohol that solution of every 1mL containing 1mg is made, is made
For reference substance solution.It is tested according to thin-layered chromatography (one annex VI B of China's coastal port), draws above two solution
Each 2 μ L are put respectively on same silica gel g thin-layer plate, with hexamethylene-chloroform-ethyl acetate-glacial acetic acid (20: 5: 8: 0.5)
For solvent, it is unfolded, takes out, dry, with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot development at 100 DEG C, sets daylight for spray
And it is inspected under ultraviolet lamp (365nm).In test sample chromatography, on position corresponding with reference substance chromatography, show respectively identical
Spot or fluorescence spot.
D, it checks：Related every regulation (one annex I C of China's coastal port) under granule item should be met
E, ethyl acetate extract：Take this product under content uniformity item appropriate, it is finely ground, take about 5g (containing sucrose) or 3g (no sugarcanes
Sugar), accurately weighed, precision plus ethyl acetate 50mL, according to the hot dipping (China's coastal port one under Extract mensuration
Annex XA) it measures.
(3) assay：It is measured according to high performance liquid chromatography (one annex VID of China's coastal port).
A, chromatographic condition and system suitability test：Using octadecyl silane as filler；It is molten with -0.1% phosphoric acid of acetonitrile
Liquid (10: 90) is mobile phase；Detection wavelength is 348nm.
B, the preparation of reference substance solution：Take chlorogenic acid reference substance appropriate, it is accurately weighed, add methanol that every 1mL is made molten containing 150 μ g
Liquid to get.
C, the preparation of test solution：This product under content uniformity item is taken, it is finely ground, about 3g is taken, it is accurately weighed, set round-bottomed flask
In, methanol 50mL is added in precision, and weighed weight is heated to reflux 1 hour, puts to room temperature, then weighed weight, and less loss is supplied with methanol
Quality, shake up, filter, take subsequent filtrate, with the filtration of (0.45 μm) of miillpore filter to get；
D, accurate respectively to draw reference substance solution and each 20 μ L of test solution, inject liquid chromatograph, measure to get.
2. a kind of method of quality control of mountain chrysanthemum Jiangya Granula according to claim 1, it is characterised in that：Every bag of this product is green
Ortho acid (C16H18O9) meter, 0.60mg must not be less than.
3. a kind of method of quality control of mountain chrysanthemum Jiangya Granula according to claim 1, it is characterised in that：Use ethyl acetate
Make solvent, every bag must not be less than 35.0mg containing extract.
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| CN201611157291.0A CN108614065A (en) | 2016-12-09 | 2016-12-09 | A kind of method of quality control of mountain chrysanthemum Jiangya Granula |
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| CN201611157291.0A CN108614065A (en) | 2016-12-09 | 2016-12-09 | A kind of method of quality control of mountain chrysanthemum Jiangya Granula |
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| CN201611157291.0A Pending CN108614065A (en) | 2016-12-09 | 2016-12-09 | A kind of method of quality control of mountain chrysanthemum Jiangya Granula |
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