CN102038897A - Quality control method of traditional Chinese medical preparation - Google Patents
Quality control method of traditional Chinese medical preparation Download PDFInfo
- Publication number
- CN102038897A CN102038897A CN2009100709110A CN200910070911A CN102038897A CN 102038897 A CN102038897 A CN 102038897A CN 2009100709110 A CN2009100709110 A CN 2009100709110A CN 200910070911 A CN200910070911 A CN 200910070911A CN 102038897 A CN102038897 A CN 102038897A
- Authority
- CN
- China
- Prior art keywords
- solution
- reference substance
- female ball
- need testing
- layer chromatography
- 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.)
- Pending
Links
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a quality control method of a traditional Chinese medical preparation. The method comprises the following steps of: firstly, carrying out microscopic identification; secondly, identifying whether a honokiol pill prescription contains elecampane, magnolia, salvia, corydalis, white peony root and gentian or not by adopting a film chromatography; and finally, measuring the magnolia content in the honokiol pill prescription by adopting a high-efficiency liquid-phase method and using magnolol and honokiol as reference substances. The invention improves and perfects the quality standard of the honokiol pill, adds the film identification methods of the nolia, the salvia, the corydalis, the white peony root and the gentian on a basis of standards issued by ministry and draws up a magnolia content measuring method by using the magnolol (C18H18O2) and the honokiol (C18H18O2) as the reference substances. The revised quality standard improves the pharmaceutical quality control, can more accurately detect counterfeit and substandard drugs and be significant to the modernization and the export of traditional Chinese medicines.
Description
Technical field
The invention belongs to technical field of Chinese medicines, relate to the detection method of Chinese medicine, the help method of quality control of female ball of especially a kind of Chinese medicine preparation.
Background technology
Help female ball by Rhizoma Cyperi (vinegar system), Radix Rehmanniae Preparata, Semen Nelumbinis, Radix Angelicae Sinensis, the Herba Lycopi, Radix Rehmanniae, Poria, Radix Asparagi, Radix Ophiopogonis, Rhizoma Corydalis (vinegar system), Flos Carthami, the Radix Paeoniae Alba, Radix Gentianae, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens), Pericarpium Citri Reticulatae Viride (vinegar system), Radix Salviae Miltiorrhizae, Cortex Moutan, Periostracum Cicadae, Radix Platycodonis, Fructus Aurantii (parched with bran), Fructus Oryzae Germinatus (stir-fry), Caulis Akebiae, Fructus Alpiniae Oxyphyllae (processed with salt), the Radix Linderae, Pericarpium Citri Reticulatae, the Radix Aucklandiae, the Rhizoma Atractylodis Macrocephalae (parched with bran), Colla Corii Asini, Semen Ziziphi Spinosae (stir-fry), Radix Polygalae (system), Semen Alpiniae Katsumadai, Fructus Toosendan, form, preparation method: above 32 flavors, be ground into fine powder, sieve, mixing, every 100g powder adds refined honey 130～150g, make big honeyed pills, promptly, major function: regulating menstruation and nourishing blood, stomach function regulating is calmed the nerves, be used for menoxenia, dysmenorrhea, sleeplessness before menstruaion, incoordination between the liver and stomach, breast is given birth to tuberosity.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, a kind of help method of quality control of female ball of Chinese medicine preparation that can the qualitative and quantitative analysis ingredient is provided, this method has that detection means is simple, the testing result characteristic of accurate.
The objective of the invention is to be achieved through the following technical solutions:
The help method of quality control of female ball of a kind of Chinese medicine preparation, the step of method is:
(1) microscopical identification;
(2) with the Radix Aucklandiae be control medicinal material, thin layer chromatography differentiates in the female ball prescription of Ji whether contain the Radix Aucklandiae;
(3) be reference substance with paeonol, magnolol and honokiol, thin layer chromatography differentiates in the female ball prescription of Ji whether contain Cortex Magnoliae Officinalis;
(4) with the Radix Salviae Miltiorrhizae be control medicinal material, thin layer chromatography differentiates in the female ball prescription of Ji whether contain Radix Salviae Miltiorrhizae;
(5) with the tetrahydropalmatine be reference substance, thin layer chromatography differentiates in the female ball prescription of Ji whether contain Rhizoma Corydalis;
(6) with the peoniflorin be reference substance, thin layer chromatography differentiates in the female ball prescription of Ji whether contain the Radix Paeoniae Alba;
(7) with the gentiopicrin be reference substance, thin layer chromatography differentiates in the female ball prescription of Ji whether contain Radix Gentianae;
(8) be reference substance with magnolol and honokiol, high-efficient liquid phase technique is measured the content of the Cortex Magnoliae Officinalis in the female ball prescription of Ji
And the method for described microscopical identification is: put microscopically and observe: the parenchyma taupe brown is to dark brown, and the many shrinkages of cell include brown nuclear shape thing, and the dendritic agglomerate of irregular branch is colourless, meets the chloral hydrate test solution and dissolves; Hyphae colorless or light brown are elongated, crooked slightly, branch is arranged, diameter 4～6 μ m, the pollen grain class is spherical or oval, diameter is approximately to 60 μ m, 3 germinal aperatures of tool, and outer wall has dentation, the Cortex Magnoliae Officinalis stone cell divides dendritic, wall thickness, and laminated striation is obvious, Rhizoma Cyperi fibre bundle rufous or yellowish-brown, wall is very thick, and parenchyma cell contains prism of calcium oxalate around the Radix Glycyrrhizae fibre bundle, forms crystalline cellulose.
And described thin layer chromatography differentiates that the method for the Radix Aucklandiae in the female ball prescription of Ji is:
Get female ball sample 2 balls of Ji, add kieselguhr 6g, grind well, add petroleum ether 50ml, supersound process 30 minutes filters, and filtrate volatilizes, and its medicinal residues are standby, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 0.5g, adds petroleum ether 10ml, and supersound process 15 minutes filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, in contrast medical material solution; The thin layer chromatography test, draw need testing solution 6 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: chloroform=1: 5 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, it is clear to be heated to the speckle colour developing, detect need testing solution with the corresponding position of reference substance chromatograph on, whether show the speckle of same color, to determine whether contain the Radix Aucklandiae in the sample.
And described thin layer chromatography differentiates that the method for Cortex Magnoliae Officinalis in the female ball prescription of Ji is:
Get the paeonol reference substance, add ethyl acetate and make the solution that every 1ml contains 2mg, in contrast the product solution I; Other gets magnolol and honokiol reference substance, adds ethyl acetate and makes the mixed solution that every 1ml contains 0.5mg, in contrast the product solution II; The thin layer chromatography test, draw need testing solution 4～6 μ l in the Radix Aucklandiae discriminating, each 2～6 μ l of above-mentioned reference substance solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ethyl acetate=3: 1 is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp 254nm and inspect, detect need testing solution with reference substance magnolol and the corresponding position of honokiol chromatograph on, whether show the speckle of same color; Spray with the acid 5% ferric chloride alcoholic solution of hydrochloric acid, it is clear to be heated to the speckle colour developing again, detect the test sample chromatograph with the corresponding position of paeonol reference substance chromatograph on, whether show the speckle of same color, and then whether contain Cortex Magnoliae Officinalis in definite sample.
And described thin layer chromatography differentiates that the method for Radix Salviae Miltiorrhizae in the female ball prescription of Ji is:
Get residual medicine dreg in the Radix Aucklandiae discriminating, fling to solvent, add ethanol 50ml, supersound process 30 minutes filters the filtrate evaporate to dryness, add diethyl ether 15ml and 2% acetum 25ml of residue makes dissolving, is transferred in the separatory funnel jolting and extracts, and divides and gets ether layer, the 15ml that adds diethyl ether again extracts, merge ether solution, wherein aqueous acid is standby, volatilizes, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, adds ethanol 20ml, shines medical material solution in pairs with legal system; The thin layer chromatography test, draw need testing solution 6 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate: formic acid=5: 3: 1 is developing solvent, launches, take out, dry, spray is with 1% ferric chloride: the mixed solution of 1% potassium ferricyanide=1: 1, detect need testing solution with the corresponding position of reference substance chromatograph on, the speckle that whether shows same color is to determine whether contain Radix Salviae Miltiorrhizae in the sample.
And described thin layer chromatography differentiates that the method for Rhizoma Corydalis in the female ball prescription of Ji is:
Get the aqueous acid in the Radix Salviae Miltiorrhizae discriminating, regulate pH value to 9～10 with ammonia, with ether extraction twice, each 15ml merges ether solution, and evaporate to dryness, residue add ethanol 1ml makes dissolving, and as need testing solution, wherein remaining aqueous solution is standby; Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that 1ml contains 0.4mg, in contrast product solution; The thin layer chromatography test, draw need testing solution 6～10 μ l, reference substance solution 4 μ l, put respectively on same silica gel g thin-layer plate, with normal hexane: chloroform: methanol=15: 10: 1 is developing solvent, other adds isopyknic liquor ammoniae fortis, launch after saturated 15 minutes, take out, dry, smoked clear with iodine vapor to the speckle colour developing, take out, after waving the iodine that adsorbs on the most plate, put under the ultra-violet lamp 365nm and inspect, detect need testing solution with the corresponding position of reference substance chromatograph on, the speckle that whether shows same color is to determine whether contain Rhizoma Corydalis in the sample.
And described thin layer chromatography differentiates that the method for the Radix Paeoniae Alba in the female ball prescription of Ji is:
Get the aqueous solution in the Rhizoma Corydalis discriminating, to neutral, add water saturated n-butanol extraction twice, each 20ml with the hydrochloric acid adjust pH, merge n-butyl alcohol liquid, wash twice with water, each 20ml discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; It is an amount of that other gets the peoniflorin reference substance, adds ethanol and make the solution that 1ml contains 2mg, in contrast product solution; The thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 4 μ l, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: methanol: formic acid=40: 5: 10: 0.2 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, it is clear to be heated to the speckle colour developing, detect need testing solution with the corresponding position of reference substance chromatograph on, whether show the speckle of same color, to determine whether contain the Radix Paeoniae Alba in the sample.
And described thin layer chromatography differentiates that the method for Radix Gentianae in the female ball prescription of Ji is:
Get the gentiopicrin reference substance, add ethanol and make the solution that 1ml contains 1mg, in contrast product solution; The thin layer chromatography test, draw need testing solution 6 μ l, above-mentioned reference substance solution 4 μ l in the Radix Aucklandiae discriminating, put respectively on same silica gel g thin-layer plate, with ethyl acetate: methanol: water=20: 3: 1 is developing solvent, launches, take out, dry, put under the ultra-violet lamp 254nm and inspect, detect need testing solution with the corresponding position of reference substance chromatograph on, the speckle that whether shows same color is to determine whether contain Radix Gentianae in the sample.
And described high-efficient liquid phase technique is a reference substance with magnolol and honokiol, and the method for the content of the Cortex Magnoliae Officinalis in the female ball prescription of mensuration Ji is as follows:
1. chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With methanol: isopropyl alcohol: water=45: 20: 35 is mobile phase; The detection wavelength is 294nm; Number of theoretical plate calculates by the magnolol peak should be not less than 5000;
2. the preparation of reference substance solution: get magnolol and the honokiol reference substance is an amount of, accurately claim surely, add 70% ethanol and make the mixed solution that every 1ml contains each 30 μ g, promptly;
3. the preparation of need testing solution: it is an amount of to get this product, shreds, and gets 2g, the accurate title, decide, and the accurate 70% ethanol 50ml that adds claims to decide weight, supersound process 60 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with 70% ethanol, shake up, leave the heart 5 minutes with per minute 3000, get supernatant, promptly;
5. detect and result's mensuration: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, the injection chromatograph of liquid is measured, and its content is with magnolol (C
18H
18O
2) and honokiol (C
18H
18O
2) total, and be no less than 3.1mg.
Advantage of the present invention and good effect are:
1, detection method of the present invention is on the basis of first primary standard of " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation, increased the thin layer identification of test method of control medicinal material and reference substance, formulate high performance liquid chromatography and carried out the method for assay, revised quality standard control method, improved the controllability of the female ball quality standard that helps, further guarantee product inherent quality and curative effect, to promoting production marketing, increase the competitiveness of product in market, guaranteeing that patient's drug safety is significant.
2, the present invention has carried out raising, perfect to the female ball quality standard that helps, and on the ministry standard basis, has increased Cortex Magnoliae Officinalis, Rhizoma Cyperi, Radix Glycyrrhizae thin layer discrimination method, with magnolol (C
18H
18O
2) and honokiol (C
18H
18O
2) be reference substance, formulated the content assaying method of Cortex Magnoliae Officinalis, revised quality standard has improved the quality control of medicine, can check out counterfeit drug and substandard drug more exactly, and the modernization of Chinese medicine and Chinese medicine are gone abroad to be significant.
The specific embodiment
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
The help method of quality control of female ball of Chinese medicine preparation, the step of its method is:
(1) microscopical identification:
Putting microscopically observes: the parenchyma taupe brown is to dark brown, and the many shrinkages of cell include brown nuclear shape thing, and the dendritic agglomerate of irregular branch is colourless, meets the chloral hydrate test solution and dissolves; Hyphae colorless or light brown are elongated, crooked slightly, branch is arranged, diameter 4～6 μ m, the pollen grain class is spherical or oval, diameter is approximately to 60 μ m, 3 germinal aperatures of tool, and outer wall has dentation, the Cortex Magnoliae Officinalis stone cell divides dendritic, wall thickness, and laminated striation is obvious, Rhizoma Cyperi fibre bundle rufous or yellowish-brown, wall is very thick, and parenchyma cell contains prism of calcium oxalate around the Radix Glycyrrhizae fibre bundle, forms crystalline cellulose.
(2) adopting thin layer chromatography, is control medicinal material with the Radix Aucklandiae, differentiates the Radix Aucklandiae in the female ball prescription of Ji.
Get female ball sample 2 balls of Ji, add kieselguhr 6g, grind well, add petroleum ether (30～60 ℃) 50ml, supersound process 30 minutes filters, and filtrate volatilizes (medicinal residues are standby), and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Radix Aucklandiae control medicinal material 0.5g, adds petroleum ether (30～60 ℃) 10ml, and supersound process 15 minutes filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, in contrast medical material solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw need testing solution 6 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: chloroform=1: 5 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(3) adopting thin layer chromatography, is reference substance with paeonol, magnolol and honokiol, differentiates Cortex Magnoliae Officinalis in the female ball prescription of Ji.
Get the paeonol reference substance, add ethyl acetate and make the solution that every 1ml contains 2mg, in contrast the product solution I; Other gets magnolol and honokiol reference substance, adds ethyl acetate and makes the mixed solution that every 1ml contains 0.5mg, in contrast the product solution II.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw need testing solution 4～6 μ l under step (2) item, each 2～6 μ l of above-mentioned reference substance solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ethyl acetate=3: 1 is developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect.In the test sample chromatograph, with magnolol and the corresponding position of honokiol reference substance chromatograph on, show the speckle of same color; Spray with the acid 5% ferric chloride alcoholic solution of hydrochloric acid, it is clear to be heated to the speckle colour developing again.In the test sample chromatograph, with the corresponding position of paeonol reference substance chromatograph on, show the speckle of same color.
(4) adopting thin layer chromatography, is control medicinal material with the Radix Salviae Miltiorrhizae, differentiates Radix Salviae Miltiorrhizae in the female ball prescription of Ji.
Get the medicinal residues of the female ball sample of Ji in the step (2), fling to solvent, add ethanol 50ml, supersound process 30 minutes filters the filtrate evaporate to dryness, add diethyl ether 15ml and 2% acetum 25ml of residue makes dissolving, be transferred to jolting extraction in the separatory funnel, divide and get ether layer, the 15ml that adds diethyl ether again extracts, merge ether solution (aqueous acid is standby), volatilize, residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, adds ethanol 20ml, shines medical material solution in pairs with legal system.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw need testing solution 6 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate: formic acid is developing solvent at 5: 3: 1, launch, take out, dry, spray is with the mixed solution (face with preceding mix) of 1% ferric chloride with 1% potassium ferricyanide (1: 1).In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(5) adopting thin layer chromatography, is reference substance with the tetrahydropalmatine, differentiates Rhizoma Corydalis in the female ball prescription of Ji.
Get the aqueous acid of the female ball sample of Ji in the step (4), regulate pH value to 9～10 with ammonia, with ether extraction twice, each 15ml merges ether solution (aqueous solution is standby), and evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that 1ml contains 0.4mg, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw need testing solution 6～10 μ l, reference substance solution 4 μ l, put respectively on same silica gel g thin-layer plate, with normal hexane: chloroform: methanol=15: 10: 1 is developing solvent, groove adds isopyknic liquor ammoniae fortis in addition, launch after saturated 15 minutes, take out, dry, smoked clear with iodine vapor to the speckle colour developing, take out, wave the iodine that adsorbs on the most plate after, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(6) adopting thin layer chromatography, is reference substance with the peoniflorin, differentiates the Radix Paeoniae Alba in the female ball prescription of Ji.
Get the aqueous solution of the female ball sample of Ji in the step (5), to neutral, add water saturated n-butanol extraction twice, each 20ml with the hydrochloric acid adjust pH, merge n-butyl alcohol liquid, wash twice with water, each 20ml discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.It is an amount of that other gets the peoniflorin reference substance, adds ethanol and make the solution that 1ml contains 2mg, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw need testing solution 10 μ l, reference substance solution 4 μ l, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: methanol: formic acid=40: 5: 10: 0.2 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(7) adopting thin layer chromatography, is reference substance with the gentiopicrin, differentiates Radix Gentianae in the female ball prescription of Ji.
Get the gentiopicrin reference substance, add ethanol and make the solution that 1ml contains 1mg, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw need testing solution 6 μ l, the above-mentioned reference substance solution 4 μ l of the female ball sample of Ji in the step (6), put respectively on same silica gel g thin-layer plate, with ethyl acetate: methanol: water=20: 3: 1 is developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(8) adopting high-efficient liquid phase technique, is reference substance with magnolol and honokiol, measures the content of the Cortex Magnoliae Officinalis in the female ball prescription of Ji.
1. the test of chromatographic condition and system suitability is a filler with the octadecylsilane chemically bonded silica; With methanol: isopropyl alcohol: water=45: 20: 35 is mobile phase; The detection wavelength is 294nm; Number of theoretical plate calculates by the magnolol peak should be not less than 5000.
2. the preparation of reference substance solution is got magnolol and the honokiol reference substance is an amount of, accurately claims surely, adds 70% ethanol and makes the mixed solution that every 1ml contains each 30 μ g, promptly.
3. it is an amount of that the female ball sample of Ji is got in the preparation of need testing solution, shreds, and gets 2g, the accurate title, decide, and the accurate 70% ethanol 50ml that adds claims to decide weight, supersound process (power 240W, frequency 45kHz) 60 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, centrifugal (per minute 3000 changes) 5 minutes, get supernatant, promptly.
5. detect and result's mensuration: precision is drawn reference substance solution, need testing solution, negative sample solution and is used respectively 10 μ l of solvent respectively, injects chromatograph of liquid, mensuration, and the every ball of this product contains Cortex Magnoliae Officinalis with magnolol (C
18H
18O
2) and honokiol (C
18H
18O
2) the total amount meter, must not be less than 3.1mg.
Claims (9)
1. the Chinese medicine preparation method of quality control of female ball that helps, it is characterized in that: the step of its method is:
(1) microscopical identification;
(2) with the Radix Aucklandiae be control medicinal material, thin layer chromatography differentiates in the female ball prescription of Ji whether contain the Radix Aucklandiae;
(3) be reference substance with paeonol, magnolol and honokiol, thin layer chromatography differentiates in the female ball prescription of Ji whether contain Cortex Magnoliae Officinalis;
(4) with the Radix Salviae Miltiorrhizae be control medicinal material, thin layer chromatography differentiates in the female ball prescription of Ji whether contain Radix Salviae Miltiorrhizae;
(5) with the tetrahydropalmatine be reference substance, thin layer chromatography differentiates in the female ball prescription of Ji whether contain Rhizoma Corydalis;
(6) with the peoniflorin be reference substance, thin layer chromatography differentiates in the female ball prescription of Ji whether contain the Radix Paeoniae Alba;
(7) with the gentiopicrin be reference substance, thin layer chromatography differentiates in the female ball prescription of Ji whether contain Radix Gentianae;
(8) be reference substance with magnolol and honokiol, high-efficient liquid phase technique is measured the content of the Cortex Magnoliae Officinalis in the female ball prescription of Ji.
2. the help method of quality control of female ball of Chinese medicine preparation according to claim 1, it is characterized in that: the method for described microscopical identification is: put microscopically and observe: the parenchyma taupe brown is to dark brown, the many shrinkages of cell, include brown nuclear shape thing, the dendritic agglomerate of irregular branch is colourless, meets the chloral hydrate test solution and dissolves; Hyphae colorless or light brown are elongated, crooked slightly, branch is arranged, diameter 4～6 μ m, the pollen grain class is spherical or oval, diameter is approximately to 60 μ m, 3 germinal aperatures of tool, and outer wall has dentation, the Cortex Magnoliae Officinalis stone cell divides dendritic, wall thickness, and laminated striation is obvious, Rhizoma Cyperi fibre bundle rufous or yellowish-brown, wall is very thick, and parenchyma cell contains prism of calcium oxalate around the Radix Glycyrrhizae fibre bundle, forms crystalline cellulose.
3. the help method of quality control of female ball of Chinese medicine preparation according to claim 1, it is characterized in that: described thin layer chromatography differentiates that the method for the Radix Aucklandiae in the female ball prescription of Ji is:
Get female ball sample 2 balls of Ji, add kieselguhr 6g, grind well, add petroleum ether 50ml, supersound process 30 minutes filters, and filtrate volatilizes, and its medicinal residues are standby, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 0.5g, adds petroleum ether 10ml, and supersound process 15 minutes filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, in contrast medical material solution; The thin layer chromatography test, draw need testing solution 6 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: chloroform=1: 5 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, it is clear to be heated to the speckle colour developing, detect need testing solution with the corresponding position of reference substance chromatograph on, whether show the speckle of same color, to determine whether contain the Radix Aucklandiae in the sample.
4. the help method of quality control of female ball of Chinese medicine preparation according to claim 1, it is characterized in that: described thin layer chromatography differentiates that the method for Cortex Magnoliae Officinalis in the female ball prescription of Ji is:
Get the paeonol reference substance, add ethyl acetate and make the solution that every 1ml contains 2mg, in contrast the product solution I; Other gets magnolol and honokiol reference substance, adds ethyl acetate and makes the mixed solution that every 1ml contains 0.5mg, in contrast the product solution II; The thin layer chromatography test, draw need testing solution 4～6 μ l in the Radix Aucklandiae discriminating, each 2～6 μ l of above-mentioned reference substance solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ethyl acetate=3: 1 is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp 254nm and inspect, detect need testing solution with reference substance magnolol and the corresponding position of honokiol chromatograph on, whether show the speckle of same color; Spray with the acid 5% ferric chloride alcoholic solution of hydrochloric acid, it is clear to be heated to the speckle colour developing again, detect the test sample chromatograph with the corresponding position of paeonol reference substance chromatograph on, whether show the speckle of same color, and then whether contain Cortex Magnoliae Officinalis in definite sample.
5. the help method of quality control of female ball of Chinese medicine preparation according to claim 1, it is characterized in that: described thin layer chromatography differentiates that the method for Radix Salviae Miltiorrhizae in the female ball prescription of Ji is:
Get residual medicine dreg in the Radix Aucklandiae discriminating, fling to solvent, add ethanol 50ml, supersound process 30 minutes filters the filtrate evaporate to dryness, add diethyl ether 15ml and 2% acetum 25ml of residue makes dissolving, is transferred in the separatory funnel jolting and extracts, and divides and gets ether layer, the 15ml that adds diethyl ether again extracts, merge ether solution, wherein aqueous acid is standby, volatilizes, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, adds ethanol 20ml, shines medical material solution in pairs with legal system; The thin layer chromatography test, draw need testing solution 6 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate: formic acid=5: 3: 1 is developing solvent, launches, take out, dry, spray is with 1% ferric chloride: the mixed solution of 1% potassium ferricyanide=1: 1, detect need testing solution with the corresponding position of reference substance chromatograph on, the speckle that whether shows same color is to determine whether contain Radix Salviae Miltiorrhizae in the sample.
6. the help method of quality control of female ball of Chinese medicine preparation according to claim 1, it is characterized in that: described thin layer chromatography differentiates that the method for Rhizoma Corydalis in the female ball prescription of Ji is:
Get the aqueous acid in the Radix Salviae Miltiorrhizae discriminating, regulate pH value to 9～10 with ammonia, with ether extraction twice, each 15ml merges ether solution, and evaporate to dryness, residue add ethanol 1ml makes dissolving, and as need testing solution, wherein remaining aqueous solution is standby; Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that 1ml contains 0.4mg, in contrast product solution; The thin layer chromatography test, draw need testing solution 6～10 μ l, reference substance solution 4 μ l, put respectively on same silica gel g thin-layer plate, with normal hexane: chloroform: methanol=15: 10: 1 is developing solvent, other adds isopyknic liquor ammoniae fortis, launch after saturated 15 minutes, take out, dry, smoked clear with iodine vapor to the speckle colour developing, take out, after waving the iodine that adsorbs on the most plate, put under the ultra-violet lamp 365nm and inspect, detect need testing solution with the corresponding position of reference substance chromatograph on, the speckle that whether shows same color is to determine whether contain Rhizoma Corydalis in the sample.
7. the help method of quality control of female ball of Chinese medicine preparation according to claim 1, it is characterized in that: described thin layer chromatography differentiates that the method for the Radix Paeoniae Alba in the female ball prescription of Ji is:
Get the aqueous solution in the Rhizoma Corydalis discriminating, to neutral, add water saturated n-butanol extraction twice, each 20ml with the hydrochloric acid adjust pH, merge n-butyl alcohol liquid, wash twice with water, each 20ml discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; It is an amount of that other gets the peoniflorin reference substance, adds ethanol and make the solution that 1ml contains 2mg, in contrast product solution; The thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 4 μ l, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: methanol: formic acid=40: 5: 10: 0.2 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, it is clear to be heated to the speckle colour developing, detect need testing solution with the corresponding position of reference substance chromatograph on, whether show the speckle of same color, to determine whether contain the Radix Paeoniae Alba in the sample.
8. the help method of quality control of female ball of Chinese medicine preparation according to claim 1, it is characterized in that: described thin layer chromatography differentiates that the method for Radix Gentianae in the female ball prescription of Ji is:
Get the gentiopicrin reference substance, add ethanol and make the solution that 1ml contains 1mg, in contrast product solution; The thin layer chromatography test, draw need testing solution 6 μ l, above-mentioned reference substance solution 4 μ l in the Radix Aucklandiae discriminating, put respectively on same silica gel g thin-layer plate, with ethyl acetate: methanol: water=20: 3: 1 is developing solvent, launches, take out, dry, put under the ultra-violet lamp 254nm and inspect, detect need testing solution with the corresponding position of reference substance chromatograph on, the speckle that whether shows same color is to determine whether contain Radix Gentianae in the sample.
9. the help method of quality control of female ball of Chinese medicine preparation according to claim 1, it is characterized in that: described high-efficient liquid phase technique is a reference substance with magnolol and honokiol, the method for content of measuring the Cortex Magnoliae Officinalis in the female ball prescription of Ji is as follows:
1. chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With methanol: isopropyl alcohol: water=45: 20: 35 is mobile phase; The detection wavelength is 294nm; Number of theoretical plate calculates by the magnolol peak should be not less than 5000;
2. the preparation of reference substance solution: get magnolol and the honokiol reference substance is an amount of, accurately claim surely, add 70% ethanol and make the mixed solution that every 1ml contains each 30 μ g, promptly;
3. the preparation of need testing solution: it is an amount of to get this product, shreds, and gets 2g, the accurate title, decide, and the accurate 70% ethanol 50ml that adds claims to decide weight, supersound process 60 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with 70% ethanol, shake up, leave the heart 5 minutes with per minute 3000, get supernatant, promptly;
5. detect and result's mensuration: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, the injection chromatograph of liquid is measured, and its content is with magnolol (C
18H
18O
2) and honokiol (C
18H
18O
2) total, and be no less than 3.1mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100709110A CN102038897A (en) | 2009-10-22 | 2009-10-22 | Quality control method of traditional Chinese medical preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100709110A CN102038897A (en) | 2009-10-22 | 2009-10-22 | Quality control method of traditional Chinese medical preparation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102038897A true CN102038897A (en) | 2011-05-04 |
Family
ID=43905658
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100709110A Pending CN102038897A (en) | 2009-10-22 | 2009-10-22 | Quality control method of traditional Chinese medical preparation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102038897A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102353744A (en) * | 2011-06-15 | 2012-02-15 | 贵州弘康药业有限公司 | Method for detecting quality of Tong Jingning capsule |
| CN102641361A (en) * | 2012-02-21 | 2012-08-22 | 常熟市方塔涂料化工有限公司 | Chinese herb preparation for treating abnormal menstruation |
| CN102818875A (en) * | 2011-06-10 | 2012-12-12 | 天津同仁堂集团股份有限公司 | Quality control method of vessel rehabilitation tablets |
| CN104407092A (en) * | 2014-08-29 | 2015-03-11 | 湖南九典制药有限公司 | Quality detection method of traditional Chinese medicinal composition with efficacy of appetizing and invigorating spleen |
| CN107515266A (en) * | 2017-09-01 | 2017-12-26 | 北京同仁堂科技发展股份有限公司 | A kind of detection method of the pharmaceutical preparation of the thing soup of the bark of official magnolia seven |
| CN108562656A (en) * | 2018-01-10 | 2018-09-21 | 广西壮族自治区食品药品检验所 | The content assaying method of alkaloid and Paeonol in Chinese medicine preparation |
| CN110780018A (en) * | 2019-11-29 | 2020-02-11 | 广东红珊瑚药业有限公司 | Quality control method of Jinggan granules |
| CN112263664A (en) * | 2020-11-12 | 2021-01-26 | 珂蓝(重庆)化妆品有限公司 | Composition for soothing liver-qi stagnation, nourishing yin and nourishing blood and application thereof |
| CN114674970A (en) * | 2022-05-26 | 2022-06-28 | 江西省药品检验检测研究院 | One-plate multi-information rapid thin-layer chromatography identification and inspection method for ginseng spleen-invigorating pills |
| CN115097058A (en) * | 2022-06-24 | 2022-09-23 | 广西新桂环保科技集团有限公司 | Thin-layer chromatography identification method for choerospondias axillaris |
| CN117233306A (en) * | 2023-11-16 | 2023-12-15 | 江西省药品检验检测研究院 | Fingerprint establishment and component content determination method for jindan Fuyan particles |
-
2009
- 2009-10-22 CN CN2009100709110A patent/CN102038897A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102818875A (en) * | 2011-06-10 | 2012-12-12 | 天津同仁堂集团股份有限公司 | Quality control method of vessel rehabilitation tablets |
| CN102353744A (en) * | 2011-06-15 | 2012-02-15 | 贵州弘康药业有限公司 | Method for detecting quality of Tong Jingning capsule |
| CN102641361A (en) * | 2012-02-21 | 2012-08-22 | 常熟市方塔涂料化工有限公司 | Chinese herb preparation for treating abnormal menstruation |
| CN102641361B (en) * | 2012-02-21 | 2014-02-26 | 常熟华港制药有限公司 | Chinese herb preparation for treating abnormal menstruation |
| CN104407092A (en) * | 2014-08-29 | 2015-03-11 | 湖南九典制药有限公司 | Quality detection method of traditional Chinese medicinal composition with efficacy of appetizing and invigorating spleen |
| CN107515266B (en) * | 2017-09-01 | 2020-10-27 | 北京同仁堂科技发展股份有限公司 | Detection method of medicinal preparation of magnolia officinalis seven-ingredient decoction |
| CN107515266A (en) * | 2017-09-01 | 2017-12-26 | 北京同仁堂科技发展股份有限公司 | A kind of detection method of the pharmaceutical preparation of the thing soup of the bark of official magnolia seven |
| CN108562656A (en) * | 2018-01-10 | 2018-09-21 | 广西壮族自治区食品药品检验所 | The content assaying method of alkaloid and Paeonol in Chinese medicine preparation |
| CN108562656B (en) * | 2018-01-10 | 2020-11-17 | 广西壮族自治区食品药品检验所 | Method for measuring content of alkaloid and paeonol in traditional Chinese medicine preparation |
| CN110780018A (en) * | 2019-11-29 | 2020-02-11 | 广东红珊瑚药业有限公司 | Quality control method of Jinggan granules |
| CN112263664A (en) * | 2020-11-12 | 2021-01-26 | 珂蓝(重庆)化妆品有限公司 | Composition for soothing liver-qi stagnation, nourishing yin and nourishing blood and application thereof |
| CN114674970A (en) * | 2022-05-26 | 2022-06-28 | 江西省药品检验检测研究院 | One-plate multi-information rapid thin-layer chromatography identification and inspection method for ginseng spleen-invigorating pills |
| CN115097058A (en) * | 2022-06-24 | 2022-09-23 | 广西新桂环保科技集团有限公司 | Thin-layer chromatography identification method for choerospondias axillaris |
| CN115097058B (en) * | 2022-06-24 | 2023-08-04 | 广西新桂环保科技集团有限公司 | Thin-layer chromatography identification method for Choerospondias axillaris |
| CN117233306A (en) * | 2023-11-16 | 2023-12-15 | 江西省药品检验检测研究院 | Fingerprint establishment and component content determination method for jindan Fuyan particles |
| CN117233306B (en) * | 2023-11-16 | 2024-01-30 | 江西省药品检验检测研究院 | Fingerprint establishment and component content determination method for jindan Fuyan particles |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102038897A (en) | Quality control method of traditional Chinese medical preparation | |
| CN101513519B (en) | Chinese medicinal composition for invigorating Qi and nourishing blood, preparation method and quality control method thereof | |
| CN102048941B (en) | Quality control method of children-welfare tablets serving as Chinese medicinal preparation | |
| CN101579500A (en) | Gynaecologic restorative pharmaceutic preparation and preparation technology and quality control method thereof | |
| CN102038795B (en) | Detection method of five-nut demulcent pill as traditional Chinese medical preparation | |
| CN102038908B (en) | Detection method of tambac depression-alleviating pill as traditional Chinese medical preparation | |
| CN102068600A (en) | Quality control method of venation relaxing and heart-nourishing pill as Chinese herbal preparation | |
| CN100493579C (en) | Chinese medicine composition, and its preparing method and quality control method | |
| CN102038785B (en) | Detection method for traditional Chinese medicinal preparation of children eyesight pills | |
| CN102048864B (en) | Detection method of children lung clearing pills of Chinese medicinal preparation | |
| CN101732553B (en) | Quality inspection method of cough pills | |
| CN102068598A (en) | Quality control method of Yangrong Baicao Wan for treating irregular menses caused by hemophthisis | |
| CN101732552B (en) | Method for detecting quality of lung clearing and phlegm eliminating pill | |
| CN102038921A (en) | Quality control method of meridian warming pill as traditional Chinese medical preparation | |
| CN102707010A (en) | Quality detection method of Chinese medicinal preparation fetal lie pill | |
| CN101716270A (en) | Method for detecting quality of traditional Chinese herbal medicament compound preparation for invigorating blood and regulating menses | |
| CN102038869B (en) | Quality control method of traditional Chinese medical preparation | |
| CN104034839A (en) | Quality detection method of hepatitis B treatment capsule | |
| CN100523803C (en) | Method for detecting active ingredient of Rukuaixiao Chewing tablet | |
| CN102038892A (en) | Quality control method for traditional Chinese medicinal preparation of galactagogue pills | |
| CN102028839B (en) | Quality control method of Chinese medicinal preparation for regulating menstruation in Department of Obstetrics and Gynecology | |
| CN107014945B (en) | A kind of detection method of Chinese medicine preparation that treating acute infectious hepatitis | |
| CN101703728B (en) | Quality detection method for stomach warming and soothing capsules | |
| CN102068566B (en) | Detection method for Yinchen Wudan pills for treating damp-heat jaundice | |
| CN101274053B (en) | Detection method of capsules for curing waist pain |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110504 |