CN107102093B - The detection method of compound pellet mattress cream - Google Patents
The detection method of compound pellet mattress cream Download PDFInfo
- Publication number
- CN107102093B CN107102093B CN201710366383.8A CN201710366383A CN107102093B CN 107102093 B CN107102093 B CN 107102093B CN 201710366383 A CN201710366383 A CN 201710366383A CN 107102093 B CN107102093 B CN 107102093B
- Authority
- CN
- China
- Prior art keywords
- solution
- methanol
- adds
- chromatography
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention provides a kind of detection methods of compound pellet mattress cream,This method includes character,Ingredient differentiates,It checks,Assay,It is not perfect for the compound pellet mattress cream original examination criteria,In standard in addition to the detection of general indicator is carried out according to rules of preparations,There is no other any quality testing measures,Drug quality cannot be monitored well,So as to add the discriminating to oriental wormwood and sweet wormwood,The discriminating of Radix Salviae Miltiorrhizae and bark of ash,The discriminating of radix bupleuri,The discriminating of Radix Glycyrrhizae,Add the assay to tanshinone IIA,The assay of tanshin polyphenolic acid B,The present invention can effectively detect corresponding medicinal raw material is thrown or do not thrown in illegal manufacturer whether less,Also confusing sweet wormwood is had detected,Bark of ash is mixed into,It prevents misuse and abuses,So as to effectively ensure the quality of compound pellet mattress cream,Make the drug safety effective,Ensure the clinical efficacy of the drug,Safeguard the interests of patient.
Description
Technical field
The present invention relates to a kind of detection method of Chinese medicine preparation, more particularly to a kind of detection method of compound pellet mattress cream.
Background technology
Compound pellet mattress cream is《The Sanitation Ministry medicine standard Traditional Chinese medicine historical preparation》Second drug recorded, standard number are
WS3-B-0339-90, prescription are oriental wormwood, Radix Salviae Miltiorrhizae, radix bupleuri, rhizoma imperatae, Radix Isatidis, Radix Glycyrrhizae, jujube, are the soft extracts of pure Chinese medicine,
It has clearing heat and promoting diuresis, and the effect for the removing jaundice that detoxifies is the profit of heat-clearing currently on the market clinically for treating acute infectious hepatitis
Wet, detoxify removing jaundice, for treating the common drug of acute infectious hepatitis, but since this standard was the upper end of the eighties in a century
It formulates, is limited to technical merit at that time and detecting instrument condition, primary standard are still far from perfect, removed in standard according to rules of preparations
Outside the detection for carrying out general indicator, without other any quality testing measures, it cannot ensure drug quality well.
On the one hand, one of medicinal material of dosage maximum is oriental wormwood in the prescription of this drug, accounts for a quarter of entire recipe quantity,
But oriental wormwood medicinal material is easily obscured with sweet wormwood and is used as medicine, and causes harmful effect to drug quality and curative effect, oriental wormwood is perennial for composite family
The seedling of herbaceous plant Artemisia capillaris or artemisia scoparia, taste bitter and cold, returns spleen, stomach, liver, gallbladder channel, it is main the effect of be exactly eliminating dampness and heat, disappear
Removing jaundice subcutaneous ulcer, also available for diseases such as wet sore itch, leaching stream yellow waters.And sweet wormwood is composite family annual herb plant sweet wormwood and artemisia annua
Herb, and using artemisia annua to be most common, most universal, nature and flavor bitter, acrid, cold, Return liver, courage, kidney channel, it is main the effect of for void of clearing up and discharging
Heat, cool blood preventing malaria, relieving summer-heat are antipyretic etc., for malaria fever and chills, fever due to yin deficiency, hectic fever due to yin labor illness, afternoon tidal fever, feverishness in palms and soles, hot summer weather
Diseases caused by external factors, fever without perspiration or have sweat, giddy headache, thirsty full and rapid pulse or warm heat disease later stage, the heresy of warm enter it is cloudy divide, night fever abating at dawn,
Heat moves back continuous low fever etc. after lossless card or warm heat disease.The effect of the two is different, it is necessary to have corresponding detection method to carry out
Monitoring.
On the other hand, one of medicinal material of another dosage maximum is Radix Salviae Miltiorrhizae in the prescription of this drug, also accounts for entire recipe quantity
A quarter, but red rooted salvia is often palmed off by bark of ash or is obscured and be used as medicine, and bad shadow is caused to drug quality and curative effect
It ringing, bark of ash is the dry root of gentianaceae plant, and Radix Salviae Miltiorrhizae is the drying root and rhizome of labiate, but due to the appearance of the two
Character is quite similar, and in recent years, it is often found that two kinds of medicinal materials are obscured use by people someone, but the effect of the two is different, it is necessary to
There is corresponding detection method to be monitored.
So the above problem can cause dosage dispensing of many illegal manufacturers when producing drug not in strict accordance with prescription,
The effect of even reducing the high raw material of price wantonly, causing drug is decreased obviously, and influences the safe and effective of drug, and serious damage is suffered from
The interests of person.
The content of the invention
The purpose of the present invention is to provide a kind of detection method of compound pellet mattress cream, and this method is by increasing main Chinese medicinal materials mattress
Old, Radix Salviae Miltiorrhizae, radix bupleuri, Radix Glycyrrhizae indentification by TLC and add and easily obscure the indentification by TLC of medicinal material sweet wormwood, bark of ash,
The assay of main component tanshinone IIA and tanshin polyphenolic acid B in red rooted salvia is added, is so as to effectively monitor illegal manufacturer
Whether no few throwing corresponding medicinal raw material or not, has also monitored confusing sweet wormwood, bark of ash is mixed into, it is therefore prevented that and it misapplies and abuses, from
And the quality of compound pellet mattress cream can be effectively monitored, make the drug safety effective, ensure the clinical efficacy of the drug, safeguard patient
Interests.
What the present invention was realized in：
The detection method of compound pellet mattress cream provided by the invention, including character, ingredient differentiate, check, assay project,
Wherein, ingredient discriminating is the discriminating to oriental wormwood and sweet wormwood, the discriminating of Radix Salviae Miltiorrhizae and bark of ash, the discriminating of radix bupleuri, the discriminating of Radix Glycyrrhizae, content
Measure is assay, the assay of tanshin polyphenolic acid B to tanshinone IIA.
（1）Oriental wormwood and the discriminating of sweet wormwood：This product 1g is taken, adds 8~12ml of methanol, is ultrasonically treated 20~40 minutes, is filtered, filter
Liquid is evaporated, and residue adds methanol 2ml to make dissolving, as test solution；Escoparone contrast product is taken, adds methanol that every 1ml is made and contains
The solution of 0.4mg, as escoparone contrast product solution；Qinghaosu is taken, adds methanol that every 1ml is made containing the molten of 0.2mg
Liquid, as Qinghaosu solution；Above-mentioned each 5 μ l of three kinds of solution are drawn, are put respectively on same silica gel g thin-layer plate, to press
60~90 DEG C of petroleum ethers of volume basis: ethyl acetate: acetone=6~8: 3~5: 1~3 be solvent, is unfolded, takes out, dry,
It puts and is inspected under the ultraviolet lamp of 365nm, in test sample chromatography, on position corresponding with escoparone contrast product chromatography, show phase
With the fluorescence spot of color；On position corresponding with Qinghaosu chromatography, the spot of not aobvious same color；
（2）The discriminating of Radix Salviae Miltiorrhizae and bark of ash：This product 2g is taken, adds 8~12ml of water, is stirred to dissolve, add diethyl ether 15~25ml, shakes
Shake, place 0.5~2 it is small when, point take ether layer, spare, raffinate adds diethyl ether 8~12ml again, shaking, place 0.5~2 it is small when, point
Ether layer is taken, mixes, volatilizes with the ether of front, residue adds ethyl acetate 1ml to make dissolving, as test solution；Take Radix Salviae Miltiorrhizae
II A reference substances of ketone, add ethyl acetate that solution of every 1ml containing 0.3mg is made, as tanshinone IIA reference substance solution；Take rough gentian bitter
Glycosides reference substance adds ethyl acetate that solution of every 1ml containing 0.2mg is made, as gentiamarin reference substance solution；According to thin-layered chromatography
Above-mentioned each 4 μ l of three kinds of solution are drawn in experiment, are put respectively on same silica gel g thin-layer plate, the benzene in terms of by volume: acetic acid second
Ester=20~22: 0.5~2 be solvent, be unfolded, take out, dry, in test sample chromatography, with tanshinone IIA reference substance chromatography
On corresponding position, the spot of same color is shown；With on gentiamarin reference substance chromatography corresponding position, not showing the spot of same color
Point；
（3）The discriminating of radix bupleuri：This product 3g is taken, adds 20~40ml of water, is stirred to dissolve, is centrifuged, is taken supernatant, be added in 100
~200 mesh, 8g, internal diameter is 2.5~3cm, on the polyamide column A of wet method dress post, respectively with water, 20% ethyl alcohol and 50% ethyl alcohol each 80
~120ml is eluted, and is collected 50% ethanol eluate, is evaporated, residue adds methanol 1ml to make dissolving, as test solution；Separately take bavin
Hu control medicinal material 1g, add water to cook 1.5 it is small when, filtration, filtrate is concentrated into 10ml, is added in 100~200 mesh, 4g, internal diameter 2cm,
It on the polyamide column B of wet method dress post, is eluted respectively with water 100ml and 50% ethyl alcohol 150ml, collects 50% ethanol eluate, be evaporated,
Residue adds methanol 1ml to make dissolving, as control medicinal material solution；According to thin-layered chromatography test, draw 2~10 μ l of test solution and
2 μ l of control medicinal material solution are put respectively on same silica gel g thin-layer plate, the ethyl acetate in terms of by volume: ethyl alcohol: water=11~
13: 1~3: 0.5~2 be solvent, is unfolded, takes out, dry, spray molten with 10% sulfuric acid ethyl alcohol of 5% paradime thylaminobenzaldehyde
Liquid, it is clear that hot wind is blown to spot development, puts and is inspected under 365nm ultraviolet lamps, in test sample chromatography, with control medicinal material chromatography phase
On the position answered, the fluorescence spot of same color is shown；
（4）The discriminating of Radix Glycyrrhizae：This product 10g is taken, adds 20~40ml of ethyl alcohol, is stirred to dissolve, is ultrasonically treated 10~30 minutes,
Filtration, filtrate are evaporated, and residue adds 10~30 ml of water to dissolve, and with hydrochloric acid tune pH value to 2~3,1~3 is extracted with ethyl acetate shaking
Secondary, 10~30 ml, combined ethyl acetate extracting solution are evaporated every time, and residue adds 1 ml of methanol to make dissolving, as test solution；
Another extracting liquorice control medicinal material 1g, adds appropriate amount of water, decocts 30 minutes, lets cool, and filters, and filtrate is concentrated into 20ml, with it is water saturated just
Butanol shaking extraction 2 times, each 20ml, merges n-butanol extracting liquid, with the water washing 2 times, each 10ml of n-butanol saturation,
N-butanol liquid is evaporated, and residue adds methanol 1ml to make dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws test sample
Solution and each 5~10 μ l of control medicinal material solution are put respectively on same silica gel g thin-layer plate, the chloroform in terms of by volume:
Methanol: water=38~42: 9~11: 0.5~2 be solvent, is unfolded, takes out, dry, spray with 5% vanillin-sulfuric acid solution,
105 DEG C to be heated to spot development clear, in test sample chromatography, on position corresponding with control medicinal material chromatography, shows same color
Spot；
（5）The assay of tanshinone IIA：It is filler with octadecylsilane chemically bonded silica；In terms of by volume
Methanol: water=75: 25 be mobile phase；Detection wavelength is 270nm；Number of theoretical plate is calculated by tanshinone IIA peak should be not less than 2000；
Precision weighs tanshinone IIA reference substance 10mg, puts in 50ml brown measuring bottles, methanol is added to shake up to scale, then again from shaking up
It is accurate in mixed liquor to measure 2ml, it puts in 25ml brown measuring bottles, methanol is added to shake up to contain tanshinone IIA in every 1ml to scale
The reference substance solution of 16 μ g；This product 2g is taken, is put in conical flask with cover, precision adds in methanol 50ml, weighed weight, in power
It is ultrasonically treated 10~30 minutes, lets cool, close plug under conditions of 120W, frequency 59KHz, then weighed weight, supply less loss with methanol
Weight shakes up, and filtration takes subsequent filtrate to get test solution；It is accurate respectively to draw reference substance solution and each 5 μ of test solution
L, inject liquid chromatograph, measure to get；
Every gram of this product contains tanshinone IIA（C19H18O3）0.4mg must not be less than；
（6）The assay of tanshin polyphenolic acid B：It is filler with octadecylsilane chemically bonded silica；First in terms of by volume
Alcohol: acetonitrile: formic acid: water=3O: 10: 1: 59 are mobile phase；Detection wavelength is 286nm；Number of theoretical plate is calculated by tanshin polyphenolic acid B peak should
Not less than 2000；Tanshin polyphenolic acid B reference substance is weighed, adds 75% methanol that solution of every 1ml containing 0.14mg is made molten to get reference substance
Liquid；This product 2g is taken, it is accurately weighed, it puts in conical flask with cover, precision adds in 75% methanol 50ml, weighed weight, in power 120W,
It is ultrasonically treated 10~30 minutes under conditions of frequency 59KHz, takes out, let cool, then weighed weight, supply less loss with 75% methanol
Weight shakes up, and filtration takes subsequent filtrate to get test solution；It is accurate respectively to draw reference substance solution and test solution each 10
μ l, inject liquid chromatograph, measure to get.
Every gram of (C containing tanshin polyphenolic acid B of this product36H30O16 ) 8mg must not be less than；
More specific detection method：
（1）The discriminating of oriental wormwood and sweet wormwood is：This product 1g is taken, adds methanol 10ml, is ultrasonically treated 30 minutes, filtration, filtrate is steamed
Dry, residue adds methanol 2ml to make dissolving, as test solution；Escoparone contrast product is taken, adds methanol that every 1ml is made containing 0.4mg
Solution, as escoparone contrast product solution；Qinghaosu is taken, adds methanol that solution of every 1ml containing 0.2mg is made, is made
For Qinghaosu solution；Above-mentioned each 5 μ l of three kinds of solution are drawn, are put respectively on same silica gel g thin-layer plate, with by volume
60~90 DEG C of petroleum ethers of meter: ethyl acetate: acetone=7: be solvent at 4: 2 are unfolded, and are taken out, are dried, put the ultraviolet light of 365nm
It is inspected under lamp, in test sample chromatography, on position corresponding with escoparone contrast product chromatography, shows the fluorescent spot of same color
Point；On position corresponding with Qinghaosu chromatography, the spot of not aobvious same color；
（2）The discriminating of Radix Salviae Miltiorrhizae and bark of ash is：This product 2g is taken, adds water 10ml, is stirred to dissolve, add diethyl ether 20ml, and shaking is put
Put 1 it is small when, point take ether layer, spare, raffinate adds diethyl ether 10ml again, shaking, place 1 it is small when, point take ether layer, the second with front
Ether mixes, and volatilizes, residue adds ethyl acetate 1ml to make dissolving, as test solution；Tanshinone IIA reference substance is taken, adds acetic acid second
Solution of every 1ml containing 0.3mg is made in ester, as tanshinone IIA reference substance solution；Gentiamarin reference substance is taken, adds ethyl acetate
Solution of every 1ml containing 0.2mg is made, as gentiamarin reference substance solution；It is tested according to thin-layered chromatography, above-mentioned three kinds of absorption is molten
Each 4 μ l of liquid are put respectively on same silica gel g thin-layer plate, the benzene in terms of by volume: ethyl acetate=21: 1 is solvent, exhibition
It opens, takes out, dry, in test sample chromatography, on tanshinone IIA reference substance chromatography corresponding position, showing the spot of same color；
With on gentiamarin reference substance chromatography corresponding position, not showing the spot of same color；
（3）The discriminating of radix bupleuri is：This product 3g is taken, adds water 30ml, is stirred to dissolve, centrifuges, takes supernatant, it is added in 100~
200 mesh, 8g, internal diameter is 2.5~3cm, each with water, 20% ethyl alcohol and 50% ethyl alcohol respectively on the polyamide column A of wet method dress post
100ml is eluted, and is collected 50% ethanol eluate, is evaporated, residue adds methanol 1ml to make dissolving, as test solution；Separately take radix bupleuri
Control medicinal material 1g, add water to cook 1.5 it is small when, filtration, filtrate is concentrated into 10ml, is added in 100~200 mesh, 4g, internal diameter 2cm, wet
On method dress column polyamide column B, eluted respectively with water 100ml and 50% ethyl alcohol 150ml, collect 50% ethanol eluate, be evaporated, residue
Methanol 1ml is added to make dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws 2~10 μ l of test solution and control
2 μ l of medicinal material solution are put respectively on same silica gel g thin-layer plate, the ethyl acetate in terms of by volume: ethyl alcohol: water=12: be at 2: 1
Solvent is unfolded, and takes out, dries, spray 10% ethanol solution of sulfuric acid with 5% paradime thylaminobenzaldehyde, hot wind is blown to spot and shows
Color is clear, puts and is inspected under 365nm ultraviolet lamps, in test sample chromatography, on position corresponding with control medicinal material chromatography, shows identical
The fluorescence spot of color；
（4）The discriminating of Radix Glycyrrhizae is：This product 10g is taken, adds ethyl alcohol 30ml, is stirred to dissolve, is ultrasonically treated 20 minutes, filtration,
Filtrate is evaporated, and residue adds 20 ml of water to dissolve, with hydrochloric acid tune pH value to 2~3, with ethyl acetate shaking extraction 2 times, and every time 20
Ml, combined ethyl acetate extracting solution, is evaporated, and residue adds 1 ml of methanol to make dissolving, as test solution；Another extracting liquorice comparison medicine
Material 1g adds appropriate amount of water, decocts 30 minutes, lets cool, and filters, and filtrate is concentrated into 20ml, with water saturated n-butanol shaking extraction 2
Secondary, each 20ml merges n-butanol extracting liquid, and with the water washing 2 times of n-butanol saturation, each 10ml, n-butanol liquid is evaporated, residual
Slag adds methanol 1ml to make dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws test solution and control medicinal material
Each 5~10 μ l of solution are put respectively on same silica gel g thin-layer plate, the chloroform in terms of by volume: methanol: water=40: 10:
1 is solvent, is unfolded, and takes out, dries, spray with 5% vanillin-sulfuric acid solution, and it is clear to be heated to spot development at 105 DEG C, is supplied
In test product chromatography, on position corresponding with control medicinal material chromatography, the spot of same color is shown；
（5）The assay of tanshinone IIA is：It is filler with octadecylsilane chemically bonded silica；In terms of by volume
Methanol: water=75: 25 be mobile phase；Detection wavelength is 270nm；Number of theoretical plate should be not less than by the calculating of tanshinone IIA peak
2000；Precision weighs tanshinone IIA reference substance 10mg, puts in 50ml brown measuring bottles, and methanol is added to shake up to scale, then again from
It is accurate in the mixed liquor shaken up to measure 2ml, it puts in 25ml brown measuring bottles, methanol is added to shake up to contain pellet in every 1ml to scale
Join the reference substance solution of II A of ketone, 16 μ g；This product 2g is taken, is put in conical flask with cover, precision addition methanol 50ml, weighed weight,
It is ultrasonically treated 20 minutes, lets cool, close plug under conditions of power 120W, frequency 59KHz, then weighed weight, supply less loss with methanol
Weight shakes up, and filtration takes subsequent filtrate to get test solution；It is accurate respectively to draw reference substance solution and each 5 μ of test solution
L, inject liquid chromatograph, measure to get；
Every gram of this product contains tanshinone IIA（C19H18O3）0.4mg must not be less than；
（6）The assay of tanshin polyphenolic acid B is：It is filler with octadecylsilane chemically bonded silica；In terms of by volume
Methanol: acetonitrile: formic acid: water=3O: 10: 1: 59 are mobile phase；Detection wavelength is 286nm；Number of theoretical plate is calculated by tanshin polyphenolic acid B peak
2000 should be not less than；Tanshin polyphenolic acid B reference substance is weighed, adds 75% methanol that solution of every 1ml containing 0.14mg is made to get reference substance
Solution；This product 2g is taken, it is accurately weighed, it puts in conical flask with cover, precision adds in 75% methanol 50ml, weighed weight, in power
It is ultrasonically treated 20 minutes under conditions of 120W, frequency 59KHz, takes out, let cool, then weighed weight, supply less loss with 75% methanol
Weight, shake up, filter, take subsequent filtrate to get test solution；Accurate absorption reference substance solution and test solution are each respectively
10 μ l, inject liquid chromatograph, measure to get；
Every gram of (C containing tanshin polyphenolic acid B of this product36H30O16 ) 8mg must not be less than.
Beneficial effects of the present invention：
The detection method of compound pellet mattress cream provided by the invention, by increasing main Chinese medicinal materials oriental wormwood, Radix Salviae Miltiorrhizae, radix bupleuri, Radix Glycyrrhizae
Indentification by TLC and add and easily obscure the indentification by TLC of medicinal material sweet wormwood, bark of ash, add main in red rooted salvia
The assay of ingredient tanshinone IIA and tanshin polyphenolic acid B is wanted, so as to which illegal manufacturer is effectively avoided to throw less or does not throw corresponding medicinal material
Raw material, avoid production drug when not in strict accordance with prescription dosage dispensing, while also accurately monitored confusing sweet wormwood,
Bark of ash is mixed into, it is therefore prevented that and it misapplies and abuses, it is avoided to influence drug quality and curative effect, meanwhile, the Components in Salvia miltiorrhiza in prescription
Effective monitoring has been obtained, ensure that the clinical efficacy of the safe and effective and drug of drug, has safeguarded the interests of patient, the present invention carries
The detection method of the compound pellet mattress cream of confession is scientific and reasonable, practical.
Specific embodiment
Embodiment 1：
Prescription：Oriental wormwood 240g, Radix Salviae Miltiorrhizae 240g, radix bupleuri 120g, rhizoma imperatae 120g, Radix Isatidis 120g, Radix Glycyrrhizae 60g, jujube
60g。
Preparation method：More than seven tastes, add water to cook three times, collecting decoction, stand, filtration, filtrate is concentrated into relative density and is
1.30（Heat is surveyed）More than, add sucrose 240g, heating fusing, mixing, be concentrated into relative density for 1.10~1.30 to get.
Character：This product be sepia stiff semifluid, sweet, slight bitter.
It checks：Relative density is 1.10~1.30.
Ingredient differentiates and assay：
（1）Oriental wormwood and the discriminating of sweet wormwood：This product 1g is taken, adds methanol 8ml, is ultrasonically treated 20 minutes, filtration, filtrate is evaporated,
Residue adds methanol 2ml to make dissolving, as test solution；Escoparone contrast product is taken, adds methanol that every 1ml is made containing 0.4mg's
Solution, as escoparone contrast product solution；Qinghaosu is taken, adds methanol that solution of every 1ml containing 0.2mg is made, as
Qinghaosu solution；Above-mentioned each 5 μ l of three kinds of solution are drawn, are put respectively on same silica gel g thin-layer plate, in terms of by volume
60~90 DEG C of petroleum ethers: ethyl acetate: acetone=6: be solvent at 3: 1, be unfolded, take out, dry, put the ultraviolet lamp of 365nm
Under inspect, in test sample chromatography, on position corresponding with escoparone contrast product chromatography, show same color fluorescence spot；
On position corresponding with Qinghaosu chromatography, the spot of not aobvious same color；
（2）The discriminating of Radix Salviae Miltiorrhizae and bark of ash：This product 2g is taken, adds water 8ml, is stirred to dissolve, add diethyl ether 15ml, shakes, and places
0.5 it is small when, point take ether layer, spare, raffinate adds diethyl ether 8ml again, shaking, place 0.5 it is small when, point ether layer is taken, with front
Ether mixes, and volatilizes, residue adds ethyl acetate 1ml to make dissolving, as test solution；Tanshinone IIA reference substance is taken, adds acetic acid
Solution of every 1ml containing 0.3mg is made in ethyl ester, as tanshinone IIA reference substance solution；Gentiamarin reference substance is taken, adds acetic acid second
Solution of every 1ml containing 0.2mg is made in ester, as gentiamarin reference substance solution；It is tested according to thin-layered chromatography, draws above-mentioned three kinds
Each 4 μ l of solution are put respectively on same silica gel g thin-layer plate, the benzene in terms of by volume: ethyl acetate=20: 0.5 is solvent,
Expansion is taken out, is dried, in test sample chromatography, on tanshinone IIA reference substance chromatography corresponding position, showing the spot of same color
Point；With on gentiamarin reference substance chromatography corresponding position, not showing the spot of same color；
（3）The discriminating of radix bupleuri：This product 3g is taken, adds water 20ml, is stirred to dissolve, is centrifuged, is taken supernatant, be added in 100~200
Mesh, 8g, internal diameter is 2.5~3cm, on the polyamide column A of wet method dress post, is washed respectively with water, 20% ethyl alcohol and each 80ml of 50% ethyl alcohol
It is de-, 50% ethanol eluate is collected, is evaporated, residue adds methanol 1ml to make dissolving, as test solution；Separately take radix bupleuri control medicinal material
1g, add water to cook 1.5 it is small when, filtration, filtrate is concentrated into 10ml, is added in 100~200 mesh, 4g, internal diameter 2cm, wet method dress post
It on polyamide column B, is eluted respectively with water 100ml and 50% ethyl alcohol 150ml, collects 50% ethanol eluate, be evaporated, residue adds methanol
1ml makes dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws 2~10 μ l of test solution and control medicinal material is molten
2 μ l of liquid are put respectively on same silica gel g thin-layer plate, the ethyl acetate in terms of by volume: ethyl alcohol: water=11: be expansion at 1: 0.5
Agent is unfolded, and takes out, dries, spray 10% ethanol solution of sulfuric acid with 5% paradime thylaminobenzaldehyde, it is clear that hot wind is blown to spot development
It is clear, it puts and is inspected under 365nm ultraviolet lamps, in test sample chromatography, on position corresponding with control medicinal material chromatography, show same color
Fluorescence spot；
（4）The discriminating of Radix Glycyrrhizae：This product 10g is taken, adds ethyl alcohol 20ml, is stirred to dissolve, is ultrasonically treated 10 minutes, is filtered, filter
Liquid is evaporated, and residue adds 10 ml of water to dissolve, and with hydrochloric acid tune pH value to 2~3, shakes extraction 1 time with ethyl acetate, every time 10 ml,
Combined ethyl acetate extracting solution, is evaporated, and residue adds methanol 1ml to make dissolving, as test solution；Another extracting liquorice control medicinal material
1g adds appropriate amount of water, decocts 30 minutes, lets cool, and filters, and filtrate is concentrated into 20ml, is extracted 2 times with the shaking of water saturated n-butanol,
Each 20ml merges n-butanol extracting liquid, and with the water washing 2 times of n-butanol saturation, each 10ml, n-butanol liquid is evaporated, residue
Methanol 1ml is added to make dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws test solution and control medicinal material is molten
Each 5~10 μ l of liquid are put respectively on same silica gel g thin-layer plate, the chloroform in terms of by volume: methanol: water=38: 9: 0.5
For solvent, it is unfolded, takes out, dry, spray with 5% vanillin-sulfuric acid solution, it is clear to be heated to spot development at 105 DEG C, for examination
In product chromatography, on position corresponding with control medicinal material chromatography, the spot of same color is shown；
（5）The assay of tanshinone IIA：It is filler with octadecylsilane chemically bonded silica；In terms of by volume
Methanol: water=75: 25 be mobile phase；Detection wavelength is 270nm；Number of theoretical plate is calculated by tanshinone IIA peak should be not less than 2000；
Precision weighs tanshinone IIA reference substance 10mg, puts in 50ml brown measuring bottles, methanol is added to shake up to scale, then again from shaking up
It is accurate in mixed liquor to measure 2ml, it puts in 25ml brown measuring bottles, methanol is added to shake up to contain tanshinone IIA in every 1ml to scale
The reference substance solution of 16 μ g；This product 2g is taken, is put in conical flask with cover, precision adds in methanol 50ml, weighed weight, in power
It is ultrasonically treated 10 minutes, lets cool, close plug under conditions of 120W, frequency 59KHz, then weighed weight, less loss weight is supplied with methanol,
It shakes up, filters, take subsequent filtrate to get test solution；It is accurate respectively to draw reference substance solution and each 5 μ l of test solution, note
Enter liquid chromatograph, measure to get.
Every gram of this product contains tanshinone IIA（C19H18O3）For 0.6mg.
（6）The assay of tanshin polyphenolic acid B：It is filler with octadecylsilane chemically bonded silica；First in terms of by volume
Alcohol: acetonitrile: formic acid: water=3O: 10: 1: 59 are mobile phase；Detection wavelength is 286nm；Number of theoretical plate is calculated by tanshin polyphenolic acid B peak should
Not less than 2000；Tanshin polyphenolic acid B reference substance is weighed, adds 75% methanol that solution of every 1ml containing 0.14mg is made molten to get reference substance
Liquid；This product 2g is taken, it is accurately weighed, it puts in conical flask with cover, precision adds in 75% methanol 50ml, weighed weight, in power 120W,
It is ultrasonically treated 10 minutes under conditions of frequency 59KHz, taking-up is let cool, then weighed weight, and the weight of less loss is supplied with 75% methanol
Amount, shakes up, and filters, takes subsequent filtrate to get test solution；It is accurate respectively to draw reference substance solution and each 10 μ of test solution
L, inject liquid chromatograph, measure to get.
Every gram of (C containing tanshin polyphenolic acid B of this product36H30O16 ) it is 9.1mg.
Embodiment 2：
In the present embodiment, except the step in ingredient discriminating and assay（1）To step（6）Outside 1 difference of embodiment,
Remaining method all same.
Ingredient differentiates and assay：
（1）Oriental wormwood and the discriminating of sweet wormwood：This product 1g is taken, adds methanol 12ml, is ultrasonically treated 40 minutes, filtration, filtrate is evaporated,
Residue adds methanol 2ml to make dissolving, as test solution；Escoparone contrast product is taken, adds methanol that every 1ml is made containing 0.4mg's
Solution, as escoparone contrast product solution；Qinghaosu is taken, adds methanol that solution of every 1ml containing 0.2mg is made, as
Qinghaosu solution；Above-mentioned each 5 μ l of three kinds of solution are drawn, are put respectively on same silica gel g thin-layer plate, in terms of by volume
60~90 DEG C of petroleum ethers: ethyl acetate: acetone=8: be solvent at 5: 3, be unfolded, take out, dry, put the ultraviolet light of 365nm
It is inspected under lamp, in test sample chromatography, on position corresponding with escoparone contrast product chromatography, shows the fluorescent spot of same color
Point；On position corresponding with Qinghaosu chromatography, the spot of not aobvious same color；
（2）The discriminating of Radix Salviae Miltiorrhizae and bark of ash：This product 2g is taken, adds water 12ml, is stirred to dissolve, add diethyl ether 25ml, shakes, and places
2 it is small when, point take ether layer, spare, raffinate adds diethyl ether 12ml again, shaking, place 2 it is small when, point take ether layer, the ether with front
Mixing, volatilizes, residue adds ethyl acetate 1ml to make dissolving, as test solution；Tanshinone IIA reference substance is taken, adds ethyl acetate
Solution of every 1ml containing 0.3mg is made, as tanshinone IIA reference substance solution；Gentiamarin reference substance is taken, adds ethyl acetate system
Into solution of every 1ml containing 0.2mg, as gentiamarin reference substance solution；It is tested according to thin-layered chromatography, draws above-mentioned three kinds of solution
Each 4 μ l are put respectively on same silica gel g thin-layer plate, the benzene in terms of by volume: ethyl acetate=22: 2 be solvent, expansion,
It takes out, dries, in test sample chromatography, on tanshinone IIA reference substance chromatography corresponding position, showing the spot of same color；
With on gentiamarin reference substance chromatography corresponding position, not showing the spot of same color；
（3）The discriminating of radix bupleuri：This product 3g is taken, adds water 40ml, is stirred to dissolve, is centrifuged, is taken supernatant, be added in 100~200
Mesh, 8g, internal diameter is 2.5~3cm, on the polyamide column A of wet method dress post, is washed respectively with water, 20% ethyl alcohol and each 120ml of 50% ethyl alcohol
It is de-, 50% ethanol eluate is collected, is evaporated, residue adds methanol 1ml to make dissolving, as test solution；Separately take radix bupleuri control medicinal material
1g, add water to cook 1.5 it is small when, filtration, filtrate is concentrated into 10ml, is added in 100~200 mesh, 4g, internal diameter 2cm, wet method dress post
It on polyamide column B, is eluted respectively with water 100ml and 50% ethyl alcohol 150ml, collects 50% ethanol eluate, be evaporated, residue adds methanol
1ml makes dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws 2~10 μ l of test solution and control medicinal material is molten
2 μ l of liquid are put respectively on same silica gel g thin-layer plate, the ethyl acetate in terms of by volume: ethyl alcohol: water=13: be expansion at 3: 2
Agent is unfolded, and takes out, dries, spray 10% ethanol solution of sulfuric acid with 5% paradime thylaminobenzaldehyde, it is clear that hot wind is blown to spot development
It is clear, it puts and is inspected under 365nm ultraviolet lamps, in test sample chromatography, on position corresponding with control medicinal material chromatography, show same color
Fluorescence spot；
（4）The discriminating of Radix Glycyrrhizae：This product 10g is taken, adds ethyl alcohol 40ml, is stirred to dissolve, is ultrasonically treated 30 minutes, is filtered, filter
Liquid is evaporated, and residue adds 30 ml of water to dissolve, and with hydrochloric acid tune pH value to 2~3, shakes extraction 3 times with ethyl acetate, every time 30 ml,
Combined ethyl acetate extracting solution, is evaporated, and residue adds 1 ml of methanol to make dissolving, as test solution；Another extracting liquorice control medicinal material
1g adds appropriate amount of water, decocts 30 minutes, lets cool, and filters, and filtrate is concentrated into 20ml, is extracted 2 times with the shaking of water saturated n-butanol,
Each 20ml merges n-butanol extracting liquid, and with the water washing 2 times of n-butanol saturation, each 10ml, n-butanol liquid is evaporated, residue
Methanol 1ml is added to make dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws test solution and control medicinal material is molten
Each 5~10 μ l of liquid are put respectively on same silica gel g thin-layer plate, the chloroform in terms of by volume: methanol: water=42: 11: 2
For solvent, it is unfolded, takes out, dry, spray with 5% vanillin-sulfuric acid solution, it is clear to be heated to spot development at 105 DEG C, for examination
In product chromatography, on position corresponding with control medicinal material chromatography, the spot of same color is shown；
（5）The assay of tanshinone IIA：It is filler with octadecylsilane chemically bonded silica；In terms of by volume
Methanol: water=75: 25 be mobile phase；Detection wavelength is 270nm；Number of theoretical plate is calculated by tanshinone IIA peak should be not less than 2000；
Precision weighs tanshinone IIA reference substance 10mg, puts in 50ml brown measuring bottles, methanol is added to shake up to scale, then again from shaking up
It is accurate in mixed liquor to measure 2ml, it puts in 25ml brown measuring bottles, methanol is added to shake up to contain tanshinone IIA in every 1ml to scale
The reference substance solution of 16 μ g；This product 2g is taken, is put in conical flask with cover, precision adds in methanol 50ml, weighed weight, in power
It is ultrasonically treated 30 minutes, lets cool, close plug under conditions of 120W, frequency 59KHz, then weighed weight, less loss weight is supplied with methanol,
It shakes up, filters, take subsequent filtrate to get test solution；It is accurate respectively to draw reference substance solution and each 5 μ l of test solution, note
Enter liquid chromatograph, measure to get.
Every gram of this product contains tanshinone IIA（C19H18O3）For 0.7mg.
（6）The assay of tanshin polyphenolic acid B：It is filler with octadecylsilane chemically bonded silica；First in terms of by volume
Alcohol: acetonitrile: formic acid: water=3O: 10: 1: 59 are mobile phase；Detection wavelength is 286nm；Number of theoretical plate is calculated by tanshin polyphenolic acid B peak should
Not less than 2000；Tanshin polyphenolic acid B reference substance is weighed, adds 75% methanol that solution of every 1ml containing 0.14mg is made molten to get reference substance
Liquid；This product 2g is taken, it is accurately weighed, it puts in conical flask with cover, precision adds in 75% methanol 50ml, weighed weight, in power 120W,
It is ultrasonically treated 30 minutes under conditions of frequency 59KHz, taking-up is let cool, then weighed weight, and the weight of less loss is supplied with 75% methanol
Amount, shakes up, and filters, takes subsequent filtrate to get test solution；It is accurate respectively to draw reference substance solution and each 10 μ of test solution
L, inject liquid chromatograph, measure to get.
Every gram of (C containing tanshin polyphenolic acid B of this product36H30O16 ) it is 9.7mg.
Embodiment 3：
In the present embodiment, except the step in ingredient discriminating and assay（1）To step（6）Outside 1 difference of embodiment,
Remaining method all same.
（1）The discriminating of oriental wormwood and sweet wormwood is：This product 1g is taken, adds methanol 10ml, is ultrasonically treated 30 minutes, filtration, filtrate is steamed
Dry, residue adds methanol 2ml to make dissolving, as test solution；Escoparone contrast product is taken, adds methanol that every 1ml is made containing 0.4mg
Solution, as escoparone contrast product solution；Qinghaosu is taken, adds methanol that solution of every 1ml containing 0.2mg is made, is made
For Qinghaosu solution；Above-mentioned each 5 μ l of three kinds of solution are drawn, are put respectively on same silica gel g thin-layer plate, with by volume
60~90 DEG C of petroleum ethers of meter: ethyl acetate: acetone=7: be solvent at 4: 2 are unfolded, and are taken out, are dried, put the ultraviolet light of 365nm
It is inspected under lamp, in test sample chromatography, on position corresponding with escoparone contrast product chromatography, shows the fluorescent spot of same color
Point；On position corresponding with Qinghaosu chromatography, the spot of not aobvious same color；
（2）The discriminating of Radix Salviae Miltiorrhizae and bark of ash is：This product 2g is taken, adds water 10ml, is stirred to dissolve, add diethyl ether 20ml, and shaking is put
Put 1 it is small when, point take ether layer, spare, raffinate adds diethyl ether 10ml again, shaking, place 1 it is small when, point take ether layer, the second with front
Ether mixes, and volatilizes, residue adds ethyl acetate 1ml to make dissolving, as test solution；Tanshinone IIA reference substance is taken, adds acetic acid second
Solution of every 1ml containing 0.3mg is made in ester, as tanshinone IIA reference substance solution；Gentiamarin reference substance is taken, adds ethyl acetate
Solution of every 1ml containing 0.2mg is made, as gentiamarin reference substance solution；It is tested according to thin-layered chromatography, above-mentioned three kinds of absorption is molten
Each 4 μ l of liquid are put respectively on same silica gel g thin-layer plate, the benzene in terms of by volume: ethyl acetate=21: 1 is solvent, exhibition
It opens, takes out, dry, in test sample chromatography, on tanshinone IIA reference substance chromatography corresponding position, showing the spot of same color；
With on gentiamarin reference substance chromatography corresponding position, not showing the spot of same color；
（3）The discriminating of radix bupleuri is：This product 3g is taken, adds water 30ml, is stirred to dissolve, centrifuges, takes supernatant, it is added in 100~
200 mesh, 8g, internal diameter is 2.5~3cm, each with water, 20% ethyl alcohol and 50% ethyl alcohol respectively on the polyamide column A of wet method dress post
100ml is eluted, and is collected 50% ethanol eluate, is evaporated, residue adds methanol 1ml to make dissolving, as test solution；Separately take radix bupleuri
Control medicinal material 1g, add water to cook 1.5 it is small when, filtration, filtrate is concentrated into 10ml, is added in 100~200 mesh, 4g, internal diameter 2cm, wet
On method dress column polyamide column B, eluted respectively with water 100ml and 50% ethyl alcohol 150ml, collect 50% ethanol eluate, be evaporated, residue
Methanol 1ml is added to make dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws 2~10 μ l of test solution and control
2 μ l of medicinal material solution are put respectively on same silica gel g thin-layer plate, the ethyl acetate in terms of by volume: ethyl alcohol: water=12: be at 2: 1
Solvent is unfolded, and takes out, dries, spray 10% ethanol solution of sulfuric acid with 5% paradime thylaminobenzaldehyde, hot wind is blown to spot and shows
Color is clear, puts and is inspected under 365nm ultraviolet lamps, in test sample chromatography, on position corresponding with control medicinal material chromatography, shows identical
The fluorescence spot of color；
（4）The discriminating of Radix Glycyrrhizae is：This product 10g is taken, adds ethyl alcohol 30ml, is stirred to dissolve, is ultrasonically treated 20 minutes, filtration,
Filtrate is evaporated, and residue adds 20 ml of water to dissolve, with hydrochloric acid tune pH value to 2~3, with ethyl acetate shaking extraction 2 times, and every time 20
Ml, combined ethyl acetate extracting solution, is evaporated, and residue adds 1 ml of methanol to make dissolving, as test solution；Another extracting liquorice comparison medicine
Material 1g adds appropriate amount of water, decocts 30 minutes, lets cool, and filters, and filtrate is concentrated into 20ml, with water saturated n-butanol shaking extraction 2
Secondary, each 20ml merges n-butanol extracting liquid, and with the water washing 2 times of n-butanol saturation, each 10ml, n-butanol liquid is evaporated, residual
Slag adds methanol 1ml to make dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws test solution and control medicinal material
Each 5~10 μ l of solution are put respectively on same silica gel g thin-layer plate, the chloroform in terms of by volume: methanol: water=40: 10:
1 is solvent, is unfolded, and takes out, dries, spray with 5% vanillin-sulfuric acid solution, and it is clear to be heated to spot development at 105 DEG C, is supplied
In test product chromatography, on position corresponding with control medicinal material chromatography, the spot of same color is shown；
（5）The assay of tanshinone IIA is：It is filler with octadecylsilane chemically bonded silica；In terms of by volume
Methanol: water=75: 25 be mobile phase；Detection wavelength is 270nm；Number of theoretical plate should be not less than by the calculating of tanshinone IIA peak
2000；Precision weighs tanshinone IIA reference substance 10mg, puts in 50ml brown measuring bottles, and methanol is added to shake up to scale, then again from
It is accurate in the mixed liquor shaken up to measure 2ml, it puts in 25ml brown measuring bottles, methanol is added to shake up to contain pellet in every 1ml to scale
Join the reference substance solution of II A of ketone, 16 μ g；This product 2g is taken, is put in conical flask with cover, precision addition methanol 50ml, weighed weight,
It is ultrasonically treated 20 minutes, lets cool, close plug under conditions of power 120W, frequency 59KHz, then weighed weight, supply less loss with methanol
Weight shakes up, and filtration takes subsequent filtrate to get test solution；It is accurate respectively to draw reference substance solution and each 5 μ of test solution
L, inject liquid chromatograph, measure to get；
Every gram of this product contains tanshinone IIA（C19H18O3）For 0.7mg.
（6）The assay of tanshin polyphenolic acid B is：It is filler with octadecylsilane chemically bonded silica；In terms of by volume
Methanol: acetonitrile: formic acid: water=3O: 10: 1: 59 are mobile phase；Detection wavelength is 286nm；Number of theoretical plate is calculated by tanshin polyphenolic acid B peak
2000 should be not less than；Tanshin polyphenolic acid B reference substance is weighed, adds 75% methanol that solution of every 1ml containing 0.14mg is made to get reference substance
Solution；This product 2g is taken, it is accurately weighed, it puts in conical flask with cover, precision adds in 75% methanol 50ml, weighed weight, in power
It is ultrasonically treated 20 minutes under conditions of 120W, frequency 59KHz, takes out, let cool, then weighed weight, supply less loss with 75% methanol
Weight, shake up, filter, take subsequent filtrate to get test solution；Accurate absorption reference substance solution and test solution are each respectively
10 μ l, inject liquid chromatograph, measure to get.
Every gram of (C containing tanshin polyphenolic acid B of this product36H30O16 ) it is 7.2mg.
Claims (2)
1. a kind of detection method of compound pellet mattress cream including character, ingredient discriminating, checks, assay, it is characterised in that：Into
Divide and differentiate it is the discriminating to oriental wormwood and sweet wormwood, the discriminating of Radix Salviae Miltiorrhizae and bark of ash, the discriminating of radix bupleuri, the discriminating of Radix Glycyrrhizae, assay is
The assay of assay, tanshin polyphenolic acid B to tanshinone IIA；
Wherein：
（1）Oriental wormwood and the discriminating of sweet wormwood：This product 1g is taken, adds 8~12ml of methanol, is ultrasonically treated 20~40 minutes, filtration, filtrate is steamed
Dry, residue adds methanol 2ml to make dissolving, as test solution；Escoparone contrast product is taken, adds methanol that every 1ml is made containing 0.4mg
Solution, as escoparone contrast product solution；Qinghaosu is taken, adds methanol that solution of every 1ml containing 0.2mg is made, is made
For Qinghaosu solution；Above-mentioned each 5 μ l of three kinds of solution are drawn, are put respectively on same silica gel g thin-layer plate, with by volume
60~90 DEG C of petroleum ethers of meter: ethyl acetate: acetone=6~8: 3~5: 1~3 be solvent, is unfolded, takes out, dry, put
It inspects under the ultraviolet lamp of 365nm, in test sample chromatography, on position corresponding with escoparone contrast product chromatography, shows identical
The fluorescence spot of color；On position corresponding with Qinghaosu chromatography, the spot of not aobvious same color；
（2）The discriminating of Radix Salviae Miltiorrhizae and bark of ash：This product 2g is taken, adds 8~12ml of water, is stirred to dissolve, add diethyl ether 15~25ml, shaking,
Place 0.5~2 it is small when, point take ether layer, spare, raffinate adds diethyl ether 8~12ml again, shaking, place 0.5~2 it is small when, point take second
Ether layer is mixed with the ether of front, volatilized, and residue adds ethyl acetate 1ml to make dissolving, as test solution；Take tanshinone IIA
Reference substance adds ethyl acetate that solution of every 1ml containing 0.3mg is made, as tanshinone IIA reference substance solution；Take gentiamarin pair
According to product, add ethyl acetate that solution of every 1ml containing 0.2mg is made, as gentiamarin reference substance solution；It is tried according to thin-layered chromatography
It tests, draws above-mentioned each 4 μ l of three kinds of solution, put respectively on same silica gel g thin-layer plate, the benzene in terms of by volume: ethyl acetate=
20~22: 0.5~2 be solvent, is unfolded, takes out, dry, in test sample chromatography, corresponding to tanshinone IIA reference substance chromatography
On position, the spot of same color is shown；With on gentiamarin reference substance chromatography corresponding position, not showing the spot of same color；
（3）The discriminating of radix bupleuri：This product 3g is taken, adds 20~40ml of water, is stirred to dissolve, is centrifuged, is taken supernatant, be added in 100~200
Mesh, 8g, internal diameter is 2.5~3cm, on the polyamide column A of wet method dress post, respectively with water, 20% ethyl alcohol and 50% ethyl alcohol each 80~
120ml is eluted, and is collected 50% ethanol eluate, is evaporated, residue adds methanol 1ml to make dissolving, as test solution；Separately take radix bupleuri
Control medicinal material 1g, add water to cook 1.5 it is small when, filtration, filtrate is concentrated into 10ml, is added in 100~200 mesh, 4g, internal diameter 2cm, wet
On the polyamide column B of method dress column, eluted respectively with water 100ml and 50% ethyl alcohol 150ml, collect 50% ethanol eluate, be evaporated, it is residual
Slag adds methanol 1ml to make dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws 2~10 μ l of test solution and right
According to 2 μ l of medicinal material solution, put respectively on same silica gel g thin-layer plate, the ethyl acetate in terms of by volume: ethyl alcohol: water=11~13
: 1~3: 0.5~2 be solvent, is unfolded, takes out, dry, spray 10% ethanol solution of sulfuric acid with 5% paradime thylaminobenzaldehyde,
It is clear that hot wind is blown to spot development, puts and is inspected under 365nm ultraviolet lamps, in test sample chromatography, corresponding to control medicinal material chromatography
Position on, show same color fluorescence spot；
（4）The discriminating of Radix Glycyrrhizae：This product 10g is taken, adds 20~40ml of ethyl alcohol, is stirred to dissolve, is ultrasonically treated 10~30 minutes, filter
It crosses, filtrate is evaporated, and residue adds 10~30 ml of water to dissolve, and with hydrochloric acid tune pH value to 2~3,1~3 is extracted with ethyl acetate shaking
Secondary, 10~30 ml, combined ethyl acetate extracting solution are evaporated every time, and residue adds methanol 1ml to make dissolving, as test solution；
Another extracting liquorice control medicinal material 1g, adds appropriate amount of water, decocts 30 minutes, lets cool, and filters, and filtrate is concentrated into 20ml, with it is water saturated just
Butanol shaking extraction 2 times, each 20ml, merges n-butanol extracting liquid, with the water washing 2 times, each 10ml of n-butanol saturation,
N-butanol liquid is evaporated, and residue adds methanol 1ml to make dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws test sample
Solution and each 5~10 μ l of control medicinal material solution are put respectively on same silica gel g thin-layer plate, the chloroform in terms of by volume:
Methanol: water=38~42: 9~11: 0.5~2 be solvent, is unfolded, takes out, dry, spray with 5% vanillin-sulfuric acid solution,
105 DEG C to be heated to spot development clear, in test sample chromatography, on position corresponding with control medicinal material chromatography, shows same color
Spot；
（5）The assay of tanshinone IIA：It is filler with octadecylsilane chemically bonded silica；Methanol in terms of by volume:
Water=75: 25 be mobile phase；Detection wavelength is 270nm；Number of theoretical plate is calculated by tanshinone IIA peak should be not less than 2000；Precision claims
Tanshinone IIA reference substance 10mg is taken, is put in 50ml brown measuring bottles, methanol is added to be shaken up, then again from the mixed liquor shaken up to scale
Middle accurate measurement 2ml, puts in 25ml brown measuring bottles, methanol is added to be shaken up to scale to get the 16 μ g containing tanshinone IIA in every 1ml
Reference substance solution；This product 2g is taken, is put in conical flask with cover, precision adds in methanol 50ml, weighed weight, in power 120W, frequency
It is ultrasonically treated 10~30 minutes, lets cool, close plug under conditions of rate 59KHz, then weighed weight, less loss weight is supplied with methanol, is shaken
Even, filtration takes subsequent filtrate to get test solution；It is accurate respectively to draw reference substance solution and each 5 μ l of test solution, injection
Liquid chromatograph, measure to get；
（6）The assay of tanshin polyphenolic acid B：It is filler with octadecylsilane chemically bonded silica；Methanol in terms of by volume: second
Nitrile: formic acid：Water=30: be mobile phase at 10: 1: 59；Detection wavelength is 286nm；Number of theoretical plate should be not less than by the calculating of tanshin polyphenolic acid B peak
2000；Tanshin polyphenolic acid B reference substance is weighed, adds 75% methanol that solution of every 1ml containing 0.14mg is made to get reference substance solution；Take this
Product 2g, it is accurately weighed, it puts in conical flask with cover, precision adds in 75% methanol 50ml, weighed weight, in power 120W, frequency
It is ultrasonically treated 10~30 minutes under conditions of 59KHz, taking-up is let cool, then weighed weight, and the weight of less loss is supplied with 75% methanol
Amount, shakes up, and filters, takes subsequent filtrate to get test solution；It is accurate respectively to draw reference substance solution and each 10 μ of test solution
L, inject liquid chromatograph, measure to get.
2. the detection method of compound pellet mattress cream according to claim 1, it is characterised in that：
Step（1）The oriental wormwood and the discriminating of sweet wormwood are：This product 1g is taken, adds methanol 10ml, is ultrasonically treated 30 minutes, filtration,
Filtrate is evaporated, and residue adds methanol 2ml to make dissolving, as test solution；Escoparone contrast product is taken, adds methanol that every 1ml is made
Solution containing 0.4mg, as escoparone contrast product solution；Qinghaosu is taken, adds methanol that every 1ml is made containing 0.2mg's
Solution, as Qinghaosu solution；Above-mentioned each 5 μ l of three kinds of solution are drawn, are put respectively on same silica gel g thin-layer plate, with
60~90 DEG C of petroleum ethers counted by volume: ethyl acetate: acetone=7: be solvent at 4: 2 are unfolded, and are taken out, are dried, put 365nm
Ultraviolet lamp under inspect, in test sample chromatography, on the position corresponding with escoparone contrast product chromatography, show same color
Fluorescence spot；On position corresponding with Qinghaosu chromatography, the spot of not aobvious same color；
Step（2）The discriminating of the Radix Salviae Miltiorrhizae and bark of ash is：This product 2g is taken, adds water 10ml, is stirred to dissolve, add diethyl ether 20ml,
Shaking, place 1 it is small when, point take ether layer, spare, raffinate adds diethyl ether 10ml again, shaking, place 1 it is small when, point take ether layer, with
The ether mixing of front, volatilizes, residue adds ethyl acetate 1ml to make dissolving, as test solution；Tanshinone IIA reference substance is taken,
Add ethyl acetate that solution of every 1ml containing 0.3mg is made, as tanshinone IIA reference substance solution；Gentiamarin reference substance is taken, is added
Solution of every 1ml containing 0.2mg is made in ethyl acetate, as gentiamarin reference substance solution；It is tested according to thin-layered chromatography, in absorption
Each 4 μ l of three kinds of solution are stated, are put respectively on same silica gel g thin-layer plate, the benzene in terms of by volume：Ethyl acetate=21: 1 is exhibition
Agent is opened, is unfolded, takes out, dries, in test sample chromatography, on tanshinone IIA reference substance chromatography corresponding position, showing same color
Spot；With on gentiamarin reference substance chromatography corresponding position, not showing the spot of same color；
Step（3）The discriminating of the radix bupleuri is：This product 3g is taken, adds water 30ml, is stirred to dissolve, is centrifuged, is taken supernatant, be added in
100~200 mesh, 8g, internal diameter is 2.5~3cm, on the polyamide column A of wet method dress post, respectively with water, 20% ethyl alcohol and 50% ethyl alcohol
Each 100ml elutions, collect 50% ethanol eluate, are evaporated, residue adds methanol 1ml to make dissolving, as test solution；Separately take bavin
Hu control medicinal material 1g, add water to cook 1.5 it is small when, filtration, filtrate is concentrated into 10ml, is added in 100~200 mesh, 4g, internal diameter 2cm,
It on wet method dress post polyamide column B, is eluted respectively with water 100ml and 50% ethyl alcohol 150ml, collects 50% ethanol eluate, be evaporated, it is residual
Slag adds methanol 1ml to make dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws 2~10 μ l of test solution and right
According to 2 μ l of medicinal material solution, put respectively on same silica gel g thin-layer plate, the ethyl acetate in terms of by volume: ethyl alcohol: water=12: 2: 1
For solvent, it is unfolded, takes out, dry, spray 10% ethanol solution of sulfuric acid with 5% paradime thylaminobenzaldehyde, hot wind is blown to spot
Colour developing is clear, puts and is inspected under 365nm ultraviolet lamps, in test sample chromatography, on position corresponding with control medicinal material chromatography, shows phase
With the fluorescence spot of color；
Step（4）The discriminating of the Radix Glycyrrhizae is：This product 10g is taken, adds ethyl alcohol 30ml, is stirred to dissolve, is ultrasonically treated 20 minutes,
Filtration, filtrate are evaporated, and residue adds 20 ml of water to dissolve, and with hydrochloric acid tune pH value to 2~3, shake extraction 2 times with ethyl acetate, every time
20 ml, combined ethyl acetate extracting solution, are evaporated, and residue adds 1 ml of methanol to make dissolving, as test solution；Another extracting liquorice pair
According to medicinal material 1g, add appropriate amount of water, decoct 30 minutes, let cool, filter, filtrate is concentrated into 20ml, is carried with the shaking of water saturated n-butanol
It takes 2 times, each 20ml, merges n-butanol extracting liquid, with the water washing 2 times, each 10ml of n-butanol saturation, n-butanol liquid steams
Dry, residue adds methanol 1ml to make dissolving, as control medicinal material solution；It is tested according to thin-layered chromatography, draws test solution and control
Each 5~10 μ l of medicinal material solution are put respectively on same silica gel g thin-layer plate, the chloroform in terms of by volume: methanol: water=40
: be solvent at 10: 1, is unfolded, and takes out, dries, spray with 5% vanillin-sulfuric acid solution, it is clear to be heated to spot development at 105 DEG C
It is clear, in test sample chromatography, on position corresponding with control medicinal material chromatography, show the spot of same color；
Step（5）The assay of the tanshinone IIA is：It is filler with octadecylsilane chemically bonded silica；To press body
Product is than the methanol of meter: water=75: 25 be mobile phase；Detection wavelength is 270nm；Number of theoretical plate should not be low by the calculating of tanshinone IIA peak
In 2000；Precision weighs tanshinone IIA reference substance 10mg, puts in 50ml brown measuring bottles, and methanol is added to be shaken up, Ran Houzai to scale
It is accurate from the mixed liquor shaken up to measure 2ml, it puts in 25ml brown measuring bottles, methanol is added to shake up and contain to get in every 1ml to scale
The reference substance solution of 16 μ g of tanshinone IIA；This product 2g is taken, is put in conical flask with cover, precision addition methanol 50ml, weighed weight,
It is ultrasonically treated 20 minutes, lets cool, close plug under conditions of power 120W, frequency 59KHz, then weighed weight, it is supplied and subtracted with methanol
Weight loss shakes up, and filtration takes subsequent filtrate to get test solution；Accurate absorption reference substance solution and test solution are each respectively
5 μ l, inject liquid chromatograph, measure to get；
Step（6）The assay of the tanshin polyphenolic acid B is：It is filler with octadecylsilane chemically bonded silica；To press volume
Than the methanol of meter: acetonitrile: formic acid: water=30: be mobile phase at 10: 1: 59；Detection wavelength is 286nm；Number of theoretical plate presses tanshin polyphenolic acid B
Peak, which calculates, should be not less than 2000；Weigh tanshin polyphenolic acid B reference substance, add 75% methanol be made solution of every 1ml containing 0.14mg to get
Reference substance solution；This product 2g is taken, it is accurately weighed, it puts in conical flask with cover, precision adds in 75% methanol 50ml, weighed weight,
It is ultrasonically treated 20 minutes under conditions of power 120W, frequency 59KHz, takes out, let cool, then weighed weight, it is supplied with 75% methanol
The weight of less loss, shakes up, and filtration takes subsequent filtrate to get test solution；Accurate absorption reference substance solution and test sample are molten respectively
Each 10 μ l of liquid, inject liquid chromatograph, measure to get.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710366383.8A CN107102093B (en) | 2017-05-23 | 2017-05-23 | The detection method of compound pellet mattress cream |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710366383.8A CN107102093B (en) | 2017-05-23 | 2017-05-23 | The detection method of compound pellet mattress cream |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107102093A CN107102093A (en) | 2017-08-29 |
| CN107102093B true CN107102093B (en) | 2018-05-22 |
Family
ID=59669736
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710366383.8A Active CN107102093B (en) | 2017-05-23 | 2017-05-23 | The detection method of compound pellet mattress cream |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107102093B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108445139B (en) * | 2018-03-26 | 2022-10-21 | 河南省洛正药业有限责任公司 | Identification method of traditional Chinese medicine preparation for treating synovitis |
| CN113049732B (en) * | 2021-03-26 | 2022-04-08 | 正大青春宝药业有限公司 | Rapid thin-layer identification method for astragalus root and poria cocos granules with one detection and multiple medicines |
| CN113588648B (en) * | 2021-09-01 | 2024-01-02 | 石河子大学 | Quality detection method for gentiana macrophylla flower Mongolian medicinal material |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337060A (en) * | 2008-08-08 | 2009-01-07 | 广西博科药业有限公司 | Quality control method of Gongyankang grannule |
| CN101850070A (en) * | 2009-04-03 | 2010-10-06 | 上海百岁行药业有限公司 | Quality standard and detection method for Chinese medicament Tangcao tablets |
| CN103954723A (en) * | 2014-04-28 | 2014-07-30 | 四川逢春制药有限公司 | Detection method of common goldenrop particles |
| CN104678036A (en) * | 2014-05-04 | 2015-06-03 | 普正药业股份有限公司 | Method for detecting quality of woman dysmenorrheal granules |
| CN105929102A (en) * | 2016-05-18 | 2016-09-07 | 四川逢春制药有限公司 | Detection method of bear gall pills |
| CN105974045A (en) * | 2016-05-18 | 2016-09-28 | 四川逢春制药有限公司 | Detection method of traditional Chinese medicine pills |
| CN106053700A (en) * | 2016-07-25 | 2016-10-26 | 山东省中医药研究院 | Fingerprint spectrum detection method of polygonum multiflorum-Alpinia oxyphylla capsules |
-
2017
- 2017-05-23 CN CN201710366383.8A patent/CN107102093B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337060A (en) * | 2008-08-08 | 2009-01-07 | 广西博科药业有限公司 | Quality control method of Gongyankang grannule |
| CN101850070A (en) * | 2009-04-03 | 2010-10-06 | 上海百岁行药业有限公司 | Quality standard and detection method for Chinese medicament Tangcao tablets |
| CN103954723A (en) * | 2014-04-28 | 2014-07-30 | 四川逢春制药有限公司 | Detection method of common goldenrop particles |
| CN104678036A (en) * | 2014-05-04 | 2015-06-03 | 普正药业股份有限公司 | Method for detecting quality of woman dysmenorrheal granules |
| CN105929102A (en) * | 2016-05-18 | 2016-09-07 | 四川逢春制药有限公司 | Detection method of bear gall pills |
| CN105974045A (en) * | 2016-05-18 | 2016-09-28 | 四川逢春制药有限公司 | Detection method of traditional Chinese medicine pills |
| CN106053700A (en) * | 2016-07-25 | 2016-10-26 | 山东省中医药研究院 | Fingerprint spectrum detection method of polygonum multiflorum-Alpinia oxyphylla capsules |
Non-Patent Citations (2)
| Title |
|---|
| 筋骨痛消丸质量标准研究;郭强;《中医临床研究》;20150120;第7卷(第2期);第7-10页 * |
| 青蒿的质量及其与伪品臭蒿和易混品茵陈的HPLC鉴别;令亚萍 等;《中药材》;20061130;第29卷(第11期);第1164-1166页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107102093A (en) | 2017-08-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105477166B (en) | A kind of preparation method and its method of quality control of duhuo jisheng decoction granule | |
| CN110455965A (en) | The preparation method and its HPLC fingerprint of pharmaceutical composition | |
| CN103071006B (en) | Preparation method and quality inspection method of traditional Chinese medicine for treating kidney failure | |
| CN107102093B (en) | The detection method of compound pellet mattress cream | |
| CN101732463B (en) | Quality detection method for Jinhuaxiaocuo pills | |
| CN104483417B (en) | The quality determining method of the Chinese medicine composition of a kind of dispelling wind cough-relieving and application thereof | |
| CN105640893B (en) | A kind of preparation method and its method of quality control of Longdan Xiegan Tang granule | |
| CN100525809C (en) | Medicinal composition of milkvetch root, chinaroot greenbrier and Hong Jingtian and its making method | |
| CN102091168A (en) | Quality control method for Chinese medicine preparation Xuefuzhuyu capsule | |
| CN101829216B (en) | Preparation method and quality control method of traditional Chinese medicine preparation for treating bronchitis and bronchial asthma | |
| CN107648369A (en) | A kind of clarification process and method of quality control of the pharmaceutical composition that there is treatment acne to act on | |
| CN101269182B (en) | Pharmaceutical composition for treating children's wind-heat cold | |
| CN1806832B (en) | Pharmaceutical composition, its preparation process and quality control method | |
| CN101439172A (en) | Chinese medicinal composition and preparation method thereof and quality control method | |
| CN107202856B (en) | A kind of detection method of Chinese medicine preparation that treating flu | |
| CN1887324B (en) | Chinese medicine composition for treating liver and kidney defect, and its preparation process and analysis method | |
| CN101716270B (en) | Method for detecting quality of traditional Chinese herbal medicament compound preparation for invigorating blood and regulating menses | |
| CN107014945B (en) | A kind of detection method of Chinese medicine preparation that treating acute infectious hepatitis | |
| CN101732527A (en) | Quality detection method for liver-soothing granules | |
| CN101869675B (en) | Chinese medicinal composition granules for treating summer-heat damp cold and preparation method thereof | |
| CN1907321B (en) | Medicinal composition for treating exterior deficiency and preparation method thereof | |
| CN100515476C (en) | Compound capsule with pseudo-ginseng and Chinese fanpalm seed, its preparation process and quality control method | |
| CN107669751A (en) | A kind of clarification process and method of quality control of the pharmaceutical composition that there is treatment red blood trace on face to act on | |
| CN103316074A (en) | Medicine composite of halenia corni extract, astragalus extract and liquorice extract as well as preparation and application of medicine composite | |
| CN106728651A (en) | The preparation method and its method of quality control of a kind of rhizoma cyperi SIWU KELI |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |