CN101987115A - Jade screen oral preparation as well as preparation method and detection method thereof - Google Patents
Jade screen oral preparation as well as preparation method and detection method thereof Download PDFInfo
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Abstract
The invention provides a jade screen oral preparation as well as a preparation method and a detection method thereof. The jade screen oral preparation provided by the invention is preferably a granular formulation and is prepared from milkvetch roots, white atractylodes rhizomes and divaricate saposhnikovia roots, the weight ratio of the three raw medicinal materials is 3:1:1, and the content of astragaloside in the preparation is more than 0.7 mg/g. The three components of milkvetch roots, atractylodes rhizomes and divaricate saposhnikovia roots in the jade screen oral preparation are identified through thin layer chromatography, and the content of effective ingredient astragaloside is measured by using liquid chromatography. The detection method provided by the invention can be applied to the quality control of jade screen related preparations, can effectively control the quality of related products and ensures the effectiveness of the products.
Description
Technical field
The present invention relates to field of traditional Chinese, particularly, the present invention relates to jade screen air port formulation and preparation thereof and detection method.
Background technology
Modern jade screen wind preparation all is to stem from the YUPINGFENG SAN that Yuan Dynasty's well-known doctor's Zhu Zhenheng is shown " danxi's experiential therapy ", is made up of the Radix Astragali, the Rhizoma Atractylodis Macrocephalae, Radix Saposhnikoviae three flavor medicines, and the effect of QI invigorating, consolidating superficial resistance, hidroschesis is arranged, and is empty people's easy catching a cold person's side commonly used.Studies show that YUPINGFENG SAN has mediator's body immunity function, the effect of building up one's resistance to disease.Be usually used in the exterior deficiency spontaneous perspiration, the disease of susceptible ailment said due to cold or exposure is one of traditional Chinese medical science classics recipe of being used to set upright.Jade screen wind listing kind has pill, medicinal tea, oral liquid, granule and capsule etc., and wherein Yupingfeng Koufuye is that traditional Chinese Pharmacopoeia records kind, is recorded in " in one one of 2005 years version of Chinese pharmacopoeia.
The detection method of each component composition Radix Astragali of jade screen wind, the Rhizoma Atractylodis Macrocephalae and Radix Saposhnikoviae, and the content of active ingredient astragaloside, generally all be to measure, the examination criteria of Astragaloside content be generally be not less than 0.12mg/g according to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B).
Summary of the invention
Therefore, the purpose of this invention is to provide a kind of jade screen air port formulation.
Another object of the present invention is, the preparation method of above-mentioned jade screen air port formulation is provided.
Another purpose of the present invention is, the detection method of above-mentioned jade screen air port formulation is provided, and comprises three kinds of the prescription Radixs Astragali, the Rhizoma Atractylodis Macrocephalae and Radix Saposhnikoviaes differentiating in the formulation of jade screen air port and measures effective ingredient Astragaloside content in the preparation.
The objective of the invention is to realize by the following technical solutions.On the one hand, the invention provides a kind of jade screen air port formulation, said preparation is preferably granule, and it is made by the Radix Astragali, the Rhizoma Atractylodis Macrocephalae and Radix Saposhnikoviae, and the parts by weight proportioning of above-mentioned three kinds of raw medicinal materials is 3: 1: 1, and the content of astragaloside is more than the 0.7mg/g in the said preparation.
On the other hand, the invention provides the above-mentioned method of stating jade screen air port formulation of preparation, this method may further comprise the steps: get the Radix Saposhnikoviae medicinal residues that extract behind the volatile oil, with the Radix Astragali, Rhizoma Atractylodis Macrocephalae extracting in water twice, the gained decocting liquid is concentrated in right amount, adds ethanol and makes that to contain alcohol amount be 70%, stir, leave standstill; Filter, decompression filtrate recycling ethanol adds the water distillate when extracting volatile oil, stirs evenly, and leaves standstill, get supernatant and filter, filtrate is concentrated into relative density 1.30～1.33 (70 ℃), and is an amount of with mannitol, dextrin and correctives, makes granule, drying, put cold, the spray add Radix Saposhnikoviae volatile oil, mixing, promptly.Preferably, wherein said correctives is selected from one or more in sucrose, aspartame, steviosin, cyclamate and the edible essence.
Another aspect the invention provides the detection method of above-mentioned jade screen air port formulation, and this method adopts thin layer chromatography to detect the Radix Astragali, the Rhizoma Atractylodis Macrocephalae and Radix Saposhnikoviae in the preparation respectively, and this method comprises the step of following preparation control sample:
(1) control sample of the preparation Radix Astragali: get Radix Astragali control medicinal material 3～10g, decoct with water secondary (each 100～500ml), each 30 minutes, collecting decoction filters, and filtrate is concentrated into about 5ml, add 3 times of amounts of ethanol and make precipitation, leave standstill, filter, filtrate evaporate to dryness, residue add water 10ml dissolving, filter, filter washs with 5ml moisture, and filtrate and washing liquid merge, and extracts 2 times (each 5～50ml) with the chloroform jolting, merge chloroform extraction liquid, evaporate to dryness, residue add methanol 1ml makes dissolving; (2) control sample of the preparation Rhizoma Atractylodis Macrocephalae: get Rhizoma Atractylodis Macrocephalae control medicinal material 1～5g, add water 250ml, decocted 30 minutes, filter, filtrate is concentrated into about 10ml, adds ethanol 30ml jolting, leave standstill, filter, filtrate is steamed to there not being the alcohol flavor, extracts 2 times (each 10～50ml) with petroleum ether (30～60 ℃) jolting, centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving; And/or the control sample of (3) preparation Radix Saposhnikoviae: get Radix Saposhnikoviae control medicinal material 1～5g, add water 250ml, decocted 30 minutes, filter, filtrate is concentrated into about 10ml, adds ethanol 30ml jolting, leave standstill, filter, filtrate is steamed to there not being the alcohol flavor, extracts 2 times (each 10～50ml) with petroleum ether (30～60 ℃) jolting, centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving.
Preferably, said method comprising the steps of: (1) differentiates the thin layer chromatography of the Radix Astragali: get preparation 5g, add water 20ml and make dissolving, filter, filter washs with 5ml moisture, filtrate and washing liquid merge, and extract secondary (25ml, 15ml for the second time for the first time) with the chloroform jolting, merge chloroform extraction liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as Radix Astragali need testing solution; Get Radix Astragali control medicinal material 6g, decoct with water secondary (250ml, 150ml for the second time for the first time), each 30 minutes, collecting decoction filters, and filtrate is concentrated into about 5ml, add 3 times of amounts of ethanol and make precipitation, leave standstill, filter the filtrate evaporate to dryness, residue adds water 10ml dissolving, filter, filter washs with 5ml moisture, and filtrate and washing liquid merge, extract secondary (25ml for the first time with the chloroform jolting, 15ml for the second time), merge chloroform extraction liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as Radix Astragali control medicinal material solution; Draw described Radix Astragali need testing solution 8 μ l, Radix Astragali control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃)-ethyl acetate (2: 1) is developing solvent, launch, take out, dry, spray is inspected under the daylight with the mixed solution of 1% potassium ferricyanide-2% ferric chloride test solution (1: 1); (2) thin layer chromatography of the discriminating Rhizoma Atractylodis Macrocephalae: get preparation 5g, add water 20ml and make dissolving, filter, filter washs with 5ml moisture, washing liquid and filtrate merge, with petroleum ether (30～60 ℃) jolting extract 2 times (25ml, 20ml), centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving, as Rhizoma Atractylodis Macrocephalae need testing solution; Get Rhizoma Atractylodis Macrocephalae control medicinal material 2g, add water 250ml, decocted 30 minutes, filter, filtrate is concentrated into about 10ml, adds ethanol 30ml jolting, leave standstill, filter, filtrate is steamed to there not being the alcohol flavor, extract secondary (25ml, 20ml for the second time for the first time) with petroleum ether (30～60 ℃) jolting, centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving, makes Rhizoma Atractylodis Macrocephalae control medicinal material solution; Draw described Rhizoma Atractylodis Macrocephalae need testing solution 10 μ l, Rhizoma Atractylodis Macrocephalae control medicinal material solution 3 μ l, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (7: 3) is developing solvent, launch, take out, dry, spray is with 10% sulfuric acid solution of 5% paradime thylaminobenzaldehyde, in about 7～10 minutes of 105 ℃ of heating, put under the ultra-violet lamp (365nm) and inspect; And/or (3) differentiate the thin layer chromatography of Radix Saposhnikoviae: get preparation 5g, add water 20ml and make dissolving, filter, filter washs with 5ml moisture, washing liquid and filtrate merge, extract secondary (25ml, 20ml for the second time for the first time) with petroleum ether (30～60 ℃) jolting, centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving, as the Radix Saposhnikoviae need testing solution; Get Radix Saposhnikoviae control medicinal material 2g, add water 250ml, decocted 30 minutes, filter, filtrate is concentrated into about 10ml, adds ethanol 30ml jolting, leave standstill, filter, filtrate is steamed to there not being the alcohol flavor, extract secondary (25ml, 20ml for the second time for the first time) with petroleum ether (30～60 ℃) jolting, centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving, makes Radix Saposhnikoviae control medicinal material solution; Drawing described Radix Saposhnikoviae need testing solution 10 μ l, Radix Saposhnikoviae control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, is developing solvent with petroleum ether (60～90 ℃)-ethyl acetate (1: 1), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.
Also on the one hand, the invention provides the detection method of astragaloside in the formulation of above-mentioned jade screen air port, this method adopts high performance liquid chromatography to detect the content of astragaloside.
Preferably, the need testing solution preparation at first adopts the methanol Soxhlet to extract in the described method, and next adopts saturated n-butanol extraction, adopts ammoniacal liquor to wash at last.
Preferably, described need testing solution preparation may further comprise the steps:
Get the preparation porphyrize, get the preferred 2.5g of about 1～10g, the accurate title, decide, and puts in the apparatus,Soxhlet's, add the preferred 100ml of methanol 10～300ml, reflux is to extracting liquid colourless, and extracting solution reclaims solvent and is concentrated into driedly, and residue adds water 20ml, slight fever makes dissolving, extract 4 times with the water-saturated n-butanol jolting, the preferred 40ml of each 10～100ml merges n-butyl alcohol liquid, with ammoniacal liquor thorough washing 2 times, the preferred 40ml of each 10～100ml merges ammoniacal liquor and extracts the preferred 20ml of each 5～50ml 2 times with the water-saturated n-butanol jolting, discard ammoniacal liquor, merge n-butyl alcohol liquid, evaporate to dryness, residue add methanol to be made dissolving and is transferred in the 10ml measuring bottle, be diluted to scale with methanol, shake up, filter, get subsequent filtrate.
Preferably, the time that described methanol Soxhlet is extracted is more than 3 hours, is preferably 6 hours.
Preferably, the chromatographic condition of described method is:
Filler is an octadecylsilane chemically bonded silica; Mobile phase is acetonitrile-water (20～50: 50～80, preferred 32: 68); Detector is an evaporative light scattering detector; Drift tube temperature is 103 ℃; Carrier gas flux is 2.8L/min; And/or column temperature is 35 ℃.
Preferably, the Astragaloside content scope of described method mensuration is that every gram granule contains astragaloside 0.35mg～2.75mg.
Again on the one hand, the invention provides said method application aspect the quality control in jade screen air port formulation is produced, described oral formulations is preferably granular preparation.
This shows, YUPINGFENG KELI preparation provided by the present invention, its character is light yellow to henna granule, puckery is then sweet.The present invention has improved the detection method of the prescription composition of YUPINGFENG KELI preparation, and is specific as follows:
(1) get this product 5g, add water 20ml and make dissolving, filter, filter 5ml moisture time washing, filtrate and washing liquid merge, and with chloroform jolting extraction 2 times (25ml, 15ml for the second time for the first time), merge chloroform extraction liquid, evaporate to dryness.Residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Astragali control medicinal material 6g, decocts with water secondary (250ml, 150ml for the second time for the first time), each 30 minutes, collecting decoction filtered, filtrate is concentrated into about 5ml, add 3 times of amounts of ethanol and make precipitation, leave standstill, filter, the filtrate evaporate to dryness, residue adds water 10ml dissolving, rises and shines medical material solution in pairs with legal system from " filtering filter 5ml moisture time washing ... ".Test according to thin layer chromatography (appendix VI B), draw above-mentioned need testing solution 8 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃)-ethyl acetate (2: 1) is developing solvent, launch, take out, dry, spray is with the mixed solution of 1% potassium ferricyanide-2% ferric chloride test solution (1: 1).In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get this product 5g, add water 20ml and make dissolving, filter, filter washs with 5ml moisture, washing liquid and filtrate merge, with petroleum ether (30～60 ℃) jolting extract 2 times (25ml, 20ml), centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving, as need testing solution.Other gets Rhizoma Atractylodis Macrocephalae control medicinal material 2g, adds water 250ml, decocts 30 minutes, filters, filtrate is concentrated into about 10ml, adds ethanol 30ml jolting, leaves standstill, filter, filtrate is steamed to there not being the alcohol flavor, shines medical material solution from " extracting 2 times with petroleum ether (30～60 ℃) jolting ... " in pairs with legal system.Test according to thin layer chromatography (appendix VI B), draw above-mentioned need testing solution 10 μ l, control medicinal material solution 3 μ l, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (7: 3) is developing solvent, launches, and takes out, dry, spray, is put under the ultra-violet lamp (365nm) and is inspected in about 7～10 minutes of 105 ℃ of heating with 10% sulfuric acid solution of 5% paradime thylaminobenzaldehyde.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(3) get above-mentioned (2) following need testing solution as need testing solution.Other gets Radix Saposhnikoviae control medicinal material 2g, shines medical material solution in pairs with legal system down according to above-mentioned (2) item.Test according to thin layer chromatography (appendix VI B), draw above-mentioned need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃)-ethyl acetate (1: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
In addition, the present invention also determines the detection method and the controlling index of product active ingredient, and is specific as follows:
Measure according to high performance liquid chromatography (appendix VI D).
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica, are mobile phase with acetonitrile-water (32: 68); Evaporative light scattering detector.Number of theoretical plate calculates with the astragaloside peak should be not less than 4000.
The preparation of reference substance solution: it is an amount of to get the astragaloside reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains astragaloside 0.12mg, promptly.
The preparation of need testing solution: get this product under the content uniformity item, porphyrize is got about 2.5g, the accurate title, decide, and puts in the apparatus,Soxhlet's, adds methanol 100ml, reflux is to extracting liquid colourless (about 64, the time), extracting solution reclaims solvent and is concentrated into driedly, and residue adds water 20ml, slight fever makes dissolving, extracts 4 times with the water-saturated n-butanol jolting, each 40ml, merge n-butyl alcohol liquid, use ammonia solution thorough washing 2 times, each 40ml, merge ammoniacal liquor and use the water-saturated n-butanol jolting to extract 2 times, each 20ml discards ammoniacal liquor, merge n-butyl alcohol liquid, evaporate to dryness, residue add methanol make the dissolving and be transferred in the 10ml measuring bottle, be diluted to scale with methanol, shake up, filter, get subsequent filtrate, promptly.
Algoscopy: accurate respectively reference substance solution 10 μ l, the 20 μ l of drawing, need testing solution 10 μ l inject chromatograph of liquid, measure, and calculate with external standard two-point method logarithmic equation, promptly.
Every bag 5 gram of this product contains the Radix Astragali with astragaloside (C
41H
68O
14) meter, must not be less than 3.5mg.
Through experimental verification, good, the middle precision of this detection method repeatability is good, specificity strong, the log-linear relation is good, and the response rate of sample is better in the scope of 0.35mg/g～2.75mg/g, is fit to the requirement of assay.This shows that method provided by the present invention can be applicable to the quality control that the jade screen wind facies closes preparation, can effectively control the product quality of Related product, guarantees the effectiveness of product.
Description of drawings
Below, describe embodiment of the present invention in conjunction with the accompanying drawings in detail, wherein:
Fig. 1 is that the thin layer chromatography of the Radix Astragali is differentiated figure, 1,2 and 3 YUPINGFENG KELI that are respectively different batches wherein, and 4 is Radix Astragali control medicinal material liquid, 5 is Radix Astragali negative control.
Fig. 2 is that the thin layer chromatography of the Rhizoma Atractylodis Macrocephalae is differentiated figure, 1,2 and 3 YUPINGFENG KELI that are respectively different batches wherein, and 4 is Rhizoma Atractylodis Macrocephalae control medicinal material liquid, 5 is Rhizoma Atractylodis Macrocephalae negative control.
Fig. 3 is the Rhizoma Atractylodis Macrocephalae thin layer chromatography discriminating figure that improves one's methods and obtain, 1,2 and 3 YUPINGFENG KELI that are respectively different batches wherein, and 4 is Rhizoma Atractylodis Macrocephalae control medicinal material liquid, 5 is Rhizoma Atractylodis Macrocephalae negative control.
Fig. 4 is that the thin layer chromatography of Radix Saposhnikoviae is differentiated figure, 1,2 and 3 YUPINGFENG KELI that are respectively different batches wherein, and 4 is Radix Saposhnikoviae control medicinal material liquid, 5 is the Radix Saposhnikoviae negative control.
Fig. 5 A to Fig. 5 C is respectively the chromatogram of astragaloside various sample: reference substance (Fig. 5 A), sample (Fig. 5 B) and negative sample (Fig. 5 C).
The correction graph that Fig. 6 measures for Astragaloside content.
Fig. 7 A to 7C is the chromatogram of astragaloside under different C18 chromatographic columns: Yi Lite ODS-2Hypersil (Fig. 7 A), Thermo ODS-2Hypersil (Fig. 7 B), Agilent ZORBAX SB (Fig. 7 C).
The specific embodiment
Followingly the present invention is described with reference to specific embodiment.It will be appreciated by those skilled in the art that these embodiment only are used to illustrate the present invention, the scope that it does not limit the present invention in any way.
Embodiment 1The preparation method of YUPINGFENG KELI preparation
Present embodiment is the preparation method of YUPINGFENG KELI preparation provided by the present invention, and is specific as follows: get 3: 1: 1 by weight prescriptions of the Radix Astragali, the Rhizoma Atractylodis Macrocephalae (stir-fry), Radix Saposhnikoviae, Radix Saposhnikoviae is given as one thinks fit cataclasm, extract volatile oil, the aqueous solution after distillation device is in addition collected; The medicinal residues and the Radix Astragali, Rhizoma Atractylodis Macrocephalae extracting in water twice, 1.5 hours each time, 1 hour for the second time; collecting decoction filters, and filtrate is concentrated in right amount; adding ethanol is 70% to containing the alcohol amount, stirs, and leaves standstill; filter, decompression filtrate recycling ethanol, the aqueous solution that adds after the above-mentioned distillation stirs evenly; leave standstill, get supernatant, filter; filtrate is concentrated into relative density 1.30～1.33 (70 ℃); an amount of with mannitol, dextrin and correctives, trough type mixing machine mixes, and oscillating granulator waves granulation; dry; put cold, choosing grain, spray adds above-mentioned Radix Saposhnikoviae volatile oil; mixing, promptly.
Embodiment 2The preparation method of YUPINGFENG KELI preparation
Present embodiment is the preparation method of YUPINGFENG KELI preparation provided by the present invention, and is specific as follows:
Get 3: 1: 1 by weight prescriptions of the Radix Astragali, the Rhizoma Atractylodis Macrocephalae (stir-fry), Radix Saposhnikoviae, Radix Saposhnikoviae is given as one thinks fit cataclasm, extract volatile oil, the aqueous solution after distillation device is in addition collected; The medicinal residues and the Radix Astragali, Rhizoma Atractylodis Macrocephalae extracting in water twice, 1.5 hours each time, 1 hour for the second time; collecting decoction filters, and filtrate is concentrated in right amount; adding ethanol is 70% to containing the alcohol amount, stirs, and leaves standstill; filter, decompression filtrate recycling ethanol, the aqueous solution that adds after the above-mentioned distillation stirs evenly; leave standstill; get supernatant, filter, filtrate is concentrated into relative density 1.30～1.33 (70 ℃); an amount of with mannitol, dextrin, correctives; wet mixing pelletizer is granulated, and drying is put cold; the choosing grain; spray adds above-mentioned Radix Saposhnikoviae volatile oil, mixing, promptly.
Embodiment 3The preparation method of YUPINGFENG KELI preparation
Present embodiment is the preparation method of YUPINGFENG KELI preparation provided by the present invention, and is specific as follows: get 3: 1: 1 by weight prescriptions of the Radix Astragali, the Rhizoma Atractylodis Macrocephalae (stir-fry), Radix Saposhnikoviae, Radix Saposhnikoviae is given as one thinks fit cataclasm, extract volatile oil, the aqueous solution after distillation device is in addition collected; The medicinal residues and the Radix Astragali, Rhizoma Atractylodis Macrocephalae extracting in water twice, 1.5 hours each time, 1 hour for the second time; collecting decoction filters, and filtrate is concentrated in right amount; adding ethanol is 70% to containing the alcohol amount, stirs, and leaves standstill; filter, decompression filtrate recycling ethanol, the aqueous solution that adds after the above-mentioned distillation stirs evenly; leave standstill; get supernatant, filter, filtrate is concentrated into relative density 1.30～1.33 (70 ℃); an amount of with mannitol, dextrin, correctives; boiling granulating machine spray granulation, drying is put cold; the choosing grain; spray adds above-mentioned Radix Saposhnikoviae volatile oil, mixing, promptly.
Correctives is selected from one or more in sucrose, aspartame, steviosin, cyclamate and the edible essence among the above embodiment 1,2 and 3.
Prepared finished product is every bag 5 gram among the above embodiment 1,2 and 3, and every bag contains the Radix Astragali and must not calculate by astragaloside and be less than 3.5mg.
Embodiment 4The thin layer chromatography discrimination method of each component composition of YUPINGFENG KELI preparation
Present embodiment is the thin layer chromatography discrimination method of each component composition of YUPINGFENG KELI preparation provided by the present invention.
(1) thin layer chromatography of the Radix Astragali is differentiated
This method refinement Radix Astragali control medicinal material amount of water and decocting time.Empirical tests with check, this method basic feasible solution, negative control is noiseless.The thin layer chromatography discriminating figure of the Radix Astragali sees Fig. 1.
The need testing solution preparation: get this product 5g, add water 20ml and make dissolving, filter, filter washs with 5ml moisture, and filtrate and washing liquid merge, and (25ml 15ml), merges chloroform extraction liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving to extract 2 times with the chloroform jolting.
The preparation of Radix Astragali control medicinal material solution: (middle inspection provides, and lot number is: 120974-200407) 6g decocts with water secondary (250ml to get Radix Astragali control medicinal material, 150ml), decocted collecting decoction 30 minutes at every turn, filter, filtrate is concentrated into about 5ml, adds 3 times of amounts of ethanol, leave standstill and make precipitation, filter the filtrate evaporate to dryness, residue adds water 10ml dissolving, rise from " filter, filter washs with 5ml moisture ... ", shine medical material solution in pairs with legal system.
Radix Astragali negative control solution preparation: get Radix Astragali negative sample (not containing the Radix Astragali, all the other prescriptions and the same finished product of preparation method) 5g, prepare with the need testing solution preparation method.
Lamellae: self-control silica gel g thin-layer plate
Point sample amount: need testing solution, each 8 μ l of negative controls, Radix Astragali control medicinal material liquid 4 μ l
Point sample mode: point-like
Developing solvent: petroleum ether (60～90 ℃)-ethyl acetate (2: 1)
Exhibition distance: 8.7cm
Colour developing and inspecting: spray is inspected (T=27 ℃ of RH=76%) with the mixed liquor of 1% potassium ferricyanide-2% ferric chloride test solution (1: 1) under the daylight.
(2) thin layer chromatography of the Rhizoma Atractylodis Macrocephalae is differentiated
This method refinement Rhizoma Atractylodis Macrocephalae control medicinal material add the water yield and decocting time.Empirical tests, negative control is noiseless, the method basic feasible solution.The thin layer chromatography discriminating figure of the Rhizoma Atractylodis Macrocephalae sees Fig. 2.
The need testing solution preparation: get this product 5g, add water 20ml and make dissolving, filter, filter washs with 5ml moisture, washing liquid and filtrate merge, with petroleum ether (30～60 ℃) extract 2 times (25ml, 20ml), merge petroleum ether extract, evaporate to dryness adds methanol 0.5ml and makes dissolving.
The preparation of Rhizoma Atractylodis Macrocephalae control medicinal material solution: (middle inspection provides to get Rhizoma Atractylodis Macrocephalae control medicinal material, lot number is: 120925-200407) 2g, and add water 250ml and decocted 30 minutes, filter, filtrate is concentrated into about 5ml, add 3 times of amount precipitations of ethanol, leave standstill, filter, the filtrate evaporate to dryness, residue adds 10ml water makes dissolving, shines medical material solution from " filter, filter washs with 5ml moisture ... " in pairs with legal system.
Rhizoma Atractylodis Macrocephalae negative control solution preparation: get Rhizoma Atractylodis Macrocephalae negative sample (not containing the Rhizoma Atractylodis Macrocephalae, all the other prescriptions and the same finished product of preparation method) 5g, make Rhizoma Atractylodis Macrocephalae negative control solution by the preparation method of need testing solution.
Lamellae: self-control silica gel g thin-layer plate
Point sample amount: need testing solution, each 12 μ l of negative control, Rhizoma Atractylodis Macrocephalae control medicinal material liquid 3 μ l
Point sample mode: point-like
Developing solvent: cyclohexane extraction-ethyl acetate (7: 3)
Exhibition distance: 8.8cm
Colour developing and inspecting: dry, spray is with 10% sulfuric acid solution of 5% paradime thylaminobenzaldehyde, in about 10 minutes of 130 ℃ of bakings, put under the ultra-violet lamp (365nm) and inspect (T=27 ℃, RH=76%).
This discriminating project is verified and checked, said method is improved to: get this product 5g, add water 20ml and make dissolving, with petroleum ether (30～60 ℃) jolting extract 2 times (25ml, 20ml), centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving.Other gets Rhizoma Atractylodis Macrocephalae control medicinal material 2g, adds water 250ml, decocts 30 minutes, filters, filtrate is concentrated into about 10ml, adds ethanol 30ml jolting, leaves standstill, and filters, filtrate is steamed to there not being the alcohol flavor, rises from " petroleum ether (30～60 ℃) jolting is extracted 2 times ... ", shines medical material solution in pairs with legal system.This speckle that obtains of improving one's methods makes moderate progress, and (wherein the point sample amount is need testing solution, each 10 μ l of negative control, and Rhizoma Atractylodis Macrocephalae control medicinal material liquid 3 μ l inspect T=24 ℃, RH=70%) to the results are shown in Figure 3.
(3) thin layer chromatography of Radix Saposhnikoviae is differentiated
This method refinement Radix Saposhnikoviae control medicinal material amount of water and decocting time.Through checking, negative control is noiseless, the method basic feasible solution.The thin layer chromatography discriminating figure of Radix Saposhnikoviae sees Fig. 4.
Need testing solution preparation: the need testing solution preparation during concrete grammar is differentiated with the thin layer chromatography of above-mentioned (2) Rhizoma Atractylodis Macrocephalae.
The preparation of Radix Saposhnikoviae control medicinal material solution: (middle inspection provides, and lot number is: 947-9302) 2g, the preparation method preparation of pressing need testing solution to get the Radix Saposhnikoviae control medicinal material.
Radix Saposhnikoviae negative control solution preparation: get Radix Saposhnikoviae negative sample (not containing Radix Saposhnikoviae, all the other prescriptions and the same finished product of preparation method) 5g, make the Radix Saposhnikoviae negative control solution by the preparation method of need testing solution.
Lamellae: self-control silica gel g thin-layer plate
Point sample amount: need testing solution, each 10 μ l of negative control, Radix Saposhnikoviae control medicinal material liquid 3 μ l
Point sample mode: point-like
Developing solvent: petroleum ether (60～90 ℃)-ethyl acetate (1: 1)
Exhibition distance: 8.8cm
Colour developing and inspecting: dry, put under the ultra-violet lamp (365nm) and inspect (T=27 ℃, RH=76%)
Embodiment 5The content assaying method of YUPINGFENG KELI preparation main component astragaloside
The present invention adopts the content of high effective liquid chromatography for measuring astragaloside.According to ten batches determination data, limit must not be less than the 0.12mg revision by every 1g of primary standard (thin layer chromatography scanning) must not be less than 3.5mg (high performance liquid chromatography) for every bag.Empirical tests with check, this method is feasible.
(1) instrument and reagent
Instrument: high performance liquid chromatograph: Agilent 1100 series; Detector: Allteach ELSD 2000ES; Chemstation 10.02 chromatographic work stations.Chromatographic column (1) Thermo ODS-2Hypersil (150mm * 4.6mm, 5 μ m), (2) Yi Lite ODS-2Hypersil (150mm * 4.6mm, 5 μ m), (3) Agilent ZORBAX SB (150mm * 4.6mm, 5 μ m) and Millipore demineralizer: milli-Q
Reagent: acetonitrile is a chromatographically pure; Water is the Millipore deionized water; N-butyl alcohol, methanol are analytical pure.
Sample: lot number 060204; Radix Astragali negative control: by the preparation of YUPINGFENG KELI prescription;
Reference substance: astragaloside (lot number: 110781-200512, Nat'l Pharmaceutical ﹠ Biological Products Control Institute)
(2) methodology checking:
1) accuracy test
Get 6 parts of the YUPINGFENG KELI (content is 0.7369mg/g) of known content (lot number 060204), every part of about 1.25g, the accurate title, decide, astragaloside reference substance solution (0.1247mg/ml) 8ml is got in every group of interpolation respectively successively, make for test agent solution in accordance with the law, press chromatographic condition and measure, calculate recovery rate the results are shown in Table 1.
Table 1 recovery test result (n=6)
In table 1, the response rate=(institute's measured value-sample size)/addition * 100%
Experimental result shows: the response rate of this method is good, is fit to the requirement of assay.
2) precision test
1. replica test is got with 6 parts of batch samples, every part of about 2.5g, and accurate the title, decide, and prepares sample solution by " for the preparation of test agent solution " method, measures in accordance with the law, the results are shown in Table 2.
Table 2 replica test result (n=6)
Experimental result shows: the repeatability of this method is good, is fit to the requirement of assay.
2. precision is chosen same sample (lot number 060107) in the middle of, is prepared respectively for test agent solution by three bit test persons in accordance with the law, according to method operation under the assay item, measures the content of astragaloside with same equipment, the results are shown in Table 3.
Table 3 different operating personnel's measurement result relatively
Experimental result shows: the middle precision of this method is good.
3) specificity
The preparation method that supplies test agent solution is with above-mentioned replica test.
Radix Astragali negative sample is got in the preparation of Radix Astragali negative control sample solution, makes with method.
The preparation of reference substance solution: it is an amount of to get the astragaloside reference substance, and accurate the title decides, and adds methanol and makes the solution that contains astragaloside 0.12mg among every 1ml, promptly.
The result shows: astragaloside reference substance retention time is 11.542, and astragaloside peak retention time is 11.644 in the YUPINGFENG KELI test sample, and the negative sample that does not contain the Radix Astragali does not have chromatographic peak at corresponding retention time place, and is noiseless, meets the requirements.The results are shown in Figure 5A to Fig. 5 C.
4) linear relationship
Get astragaloside reference substance (concentration is 0.1247mg/ml), accurate respectively 2,10,20,30, the 35 μ l of absorption inject chromatograph of liquid, the record peak area, and the logarithm of getting peak area and concentration value carries out linear regression.The results are shown in Table 4 and Fig. 6.
Table 4 astragaloside calibration trace result of calculation
The result shows: the astragaloside that this method is measured log-linear relation in 0.25～5.0 μ g scope is good.
5) scope
Compound concentration is the reference substance solution of 0.1247mg/ml respectively, and is standby.
The preparation of low strength range solution: the about 0.23g of sample thief (lot number 060204), the accurate title, decide, the reference substance solution 1.4ml that adds 0.1247mg/ml, preparation method operation with need testing solution, promptly get the low strength range need testing solution, 6 parts of operation repetitives are distinguished sample introduction in accordance with the law, calculate recovery rate the results are shown in Table 6.
The preparation of high concentration range solution: the about 1.66g of sample thief (lot number 060204), the accurate title, decide, the reference substance solution 10ml that adds 0.1247mg/ml, preparation method operation with need testing solution, promptly get the high concentration range need testing solution, 6 parts of operation repetitives are distinguished sample introduction in accordance with the law, calculate recovery rate the results are shown in Table 5 and table 6.
Table 5 hangs down the scope result of the test
The high scope result of the test of table 6
The result shows: in the concentration range of 0.35mg/g～2.75mg/g, the response rate of sample is better, meets the requirement of assay.
6) ruggedness is investigated
The selection of A, chromatographic condition: adopt the content assaying method of astragaloside under (" 2005 editions one one of Chinese pharmacopoeia) Radix Astragali item, the result shows: being filler with the octadecylsilane chemically bonded silica, is mobile phase with acetonitrile-water (32: 68); Evaporative light scattering detector: 103 ℃ of drift tube temperatures, carrier gas flux: 2.8L/min; Column temperature: 35 ℃, be separation condition, the sample baseline is steady, and separating degree is good and negative noiseless, sees Fig. 5 A to 5C.So select the analytical method of above chromatographic condition as astragaloside in the YUPINGFENG KELI.
B, extracting method are investigated:
1. methanol ultrasonic-washing of saturated n-butanol extraction-ammonia solution
Get this product under the content uniformity item, porphyrize is got about 10g, and accurate the title decides, put in the conical flask, add methanol 150ml, and supersound process 40 minutes (220W, 50HKz), extracting solution reclaims solvent and is concentrated into driedly, and residue adds water 20ml, and slight fever makes dissolving, extracts 4 times with the water-saturated n-butanol jolting, each 40ml merges n-butyl alcohol liquid, uses ammonia solution thorough washing 2 times, each 40ml, discard ammoniacal liquor, n-butyl alcohol liquid evaporate to dryness, residue is with dissolve with methanol and be transferred in the 10ml measuring bottle, add methanol to scale, shake up, promptly.
2. methanol Soxhlet extraction-saturated n-butanol extraction-ammonia solution washing method
Get this product under the content uniformity item, porphyrize is got about 10g, and accurate the title decides, put in the apparatus,Soxhlet's, add methanol 100ml, reflux 2 hours, extracting solution reclaims solvent and is concentrated into dried, residue adds water 20ml, and slight fever makes dissolving, extracts 4 times with the water-saturated n-butanol jolting, each 40ml, merge n-butyl alcohol liquid, use ammonia solution thorough washing 2 times, each 40ml, discard ammoniacal liquor, n-butyl alcohol liquid evaporate to dryness, residue is with dissolve with methanol and be transferred in the 10ml measuring bottle, add methanol to scale, shake up, promptly.
3. saturated n-butyl alcohol reflux, extract,-ammonia solution washing method
Get this product under the content uniformity item, porphyrize is got about 10g, the accurate title, decide, and puts in the conical flask, adds water-saturated n-butanol 100ml, reflux 6 hours, extracting solution ammonia solution thorough washing 2 times, each 40ml, discard ammoniacal liquor, n-butyl alcohol liquid evaporate to dryness, residue is with dissolve with methanol and be transferred in the 10ml measuring bottle, adds methanol to scale, shake up, promptly.
Algoscopy: accurate respectively reference substance solution 10ul, the 20ul of drawing, with need testing solution 5ul, inject chromatograph of liquid, measure, promptly.
Table 7 Different Extraction Method result of the test
Experimental result shows: 1. methanol ultrasonic-extraction efficiency of saturated n-butanol extraction-ammonia solution washing method and 3. saturated n-butyl alcohol reflux, extract,-ammonia solution washing method is far below 2. methanol Soxhlet extraction-saturated n-butanol extraction-ammonia solution washing method, so the need testing solution preparation method of having selected 2. methanol Soxhlet extraction-saturated n-butanol extraction-ammonia solution washing method to measure as Astragaloside content in the YUPINGFENG KELI.
The comparison of C, different extraction times
Compared at sampling amount 2.5g, the methanol Soxhlet is extracted three differentiations over time, result's (seeing Table 8) shows: consider the instrumental error of the sum of errors evaporative light scattering detector that extracts operating process, think to extract and extracted substantially fully in 5 hours, consider to have between the different samples difference to a certain degree, so will be made as extraction time 6 hours, the results are shown in Table 8.
The comparison of the different methanol eddy of table 8 extraction time
D, different chromatographic column are relatively
Choose the C18 chromatographic column (150mm * 4.6mm, 5 μ m) of three kinds of different models respectively and measure same sample (lot number 060107) solution, the results are shown in Table 9 and Fig. 7 A to 7C.
The different chromatographic columns of table 9 relatively
The result shows: the chromatographic column influence of different model is less, meets the requirement of assay.
E, stability
Get lot number and be 060204 the about 2.5g of sample, accurately claim surely, prepare need testing solution in accordance with the law, the sample introduction successively at 0,5,8,10,13,16 hour respectively, the comparison peak area value the results are shown in Table 10.
Table 10 stability of solution measurement result
7) sample determination
Get 10 batches of YUPINGFENG KELI, divide the another name sample each 2.5g, the accurate title, decide, and prepares need testing solution in accordance with the law, and sample introduction the results are shown in Table 11 respectively.
The Astragaloside content measurement result of table 1110 batch YUPINGFENG KELI
10 batch samples of surveying, the content of astragaloside is between 3.70～7.05mg/ bag.Consider the influence that Radix Astragali changes of contents is big and production process is brought of separate sources in the YUPINGFENG KELI, the content of drafting astragaloside in every bag of YUPINGFENG KELI (5 gram) must not be less than 3.5mg.
Claims (11)
1. jade screen air port formulation, said preparation is preferably granule, is made by the Radix Astragali, the Rhizoma Atractylodis Macrocephalae and Radix Saposhnikoviae, and the parts by weight proportioning of above-mentioned three kinds of raw medicinal materials is 3: 1: 1, and the content of astragaloside is more than the 0.7mg/g in the said preparation.
2. prepare the method for the described jade screen of claim 1 air port formulation, it is characterized in that this method may further comprise the steps: get the Radix Saposhnikoviae medicinal residues that extract behind the volatile oil, with the Radix Astragali, Rhizoma Atractylodis Macrocephalae extracting in water twice, the gained decocting liquid is concentrated in right amount, adds ethanol and makes that to contain alcohol amount be 70%, stir, leave standstill; Filter, decompression filtrate recycling ethanol adds the water distillate when extracting Radix Saposhnikoviae volatile oil, stir evenly, leave standstill, get supernatant and filter, filtrate is concentrated into relative density 1.30～1.33 (70 ℃), and is an amount of with mannitol, dextrin and correctives, makes granule, dry, put cold, choosing grain, spray adds Radix Saposhnikoviae volatile oil, mixing, promptly; Preferably, wherein said correctives is selected from one or more in sucrose, aspartame, steviosin, cyclamate and the edible essence.
3. the detection method of the described jade screen of claim 1 air port formulation, this method adopt thin layer chromatography to differentiate respectively the Radix Astragali, the Rhizoma Atractylodis Macrocephalae and Radix Saposhnikoviae in the preparation to it is characterized in that this method comprises the step of following preparation control sample:
(1) control sample of the preparation Radix Astragali: get the preferred 6g of Radix Astragali control medicinal material 3～10g, decoct with water secondary (each 100～500ml, preferred 250ml for the first time, 150ml for the second time), each 30 minutes, collecting decoction, filter, filtrate is concentrated into about 5ml, adds 3 times of amounts of ethanol and makes precipitation, leaves standstill, filter, filtrate evaporate to dryness, residue add water 10ml dissolving, filter, filter washs with 5ml moisture, filtrate and washing liquid merge, and extract secondary (each 5～50ml, preferred 25ml for the first time with the chloroform jolting, 15ml for the second time), merge chloroform extraction liquid, evaporate to dryness, residue add methanol 1ml makes dissolving;
(2) control sample of the preparation Rhizoma Atractylodis Macrocephalae: get the preferred 2g of Rhizoma Atractylodis Macrocephalae control medicinal material 1～5g, add water 250ml, decocted 30 minutes, filter, filtrate is concentrated into about 10ml, adds ethanol 30ml jolting, leave standstill, filter, filtrate is steamed to there not being the alcohol flavor, extract secondary (each 10～50ml, preferred 25ml for the first time, 20ml for the second time) with petroleum ether (30～60 ℃) jolting, centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving; And/or
(3) control sample of preparation Radix Saposhnikoviae: get the preferred 2g of Radix Saposhnikoviae control medicinal material 1～5g, add water 250ml, decocted 30 minutes, filter, filtrate is concentrated into about 10ml, adds ethanol 30ml jolting, leave standstill, filter, filtrate is steamed to there not being the alcohol flavor, extract secondary (each 10～50ml, preferred 25ml for the first time, 20ml for the second time) with petroleum ether (30～60 ℃) jolting, centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving.
4. detection method according to claim 3 is characterized in that, said method comprising the steps of:
(1) thin layer chromatography of the discriminating Radix Astragali: get preparation 5g, add water 20ml and make dissolving, filter, filter washs with 5ml moisture, and filtrate and washing liquid merge, extract secondary (25ml for the first time with the chloroform jolting, 15ml for the second time), merge chloroform extraction liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as Radix Astragali need testing solution; Get Radix Astragali control medicinal material 6g, decoct with water secondary (250ml, 150ml for the second time for the first time), each 30 minutes, collecting decoction filters, and filtrate is concentrated into about 5ml, add 3 times of amounts of ethanol and make precipitation, leave standstill, filter the filtrate evaporate to dryness, residue adds water 10ml dissolving, filter, filter washs with 5ml moisture, and filtrate and washing liquid merge, extract secondary (25ml for the first time with the chloroform jolting, 15ml for the second time), merge chloroform extraction liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as Radix Astragali control medicinal material solution; Draw described Radix Astragali need testing solution 8 μ l, Radix Astragali control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃)-ethyl acetate (2: 1) is developing solvent, launch, take out, dry, spray is inspected under the daylight with the mixed solution of 1% potassium ferricyanide-2% ferric chloride test solution (1: 1);
(2) thin layer chromatography of the discriminating Rhizoma Atractylodis Macrocephalae: get preparation 5g, add water 20ml and make dissolving, filter, filter washs with 5ml moisture, washing liquid and filtrate merge, extract secondary (25ml, 20ml for the second time for the first time) with petroleum ether (30～60 ℃) jolting, centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving, as Rhizoma Atractylodis Macrocephalae need testing solution; Get Rhizoma Atractylodis Macrocephalae control medicinal material 2g, add water 250ml, decocted 30 minutes, filter, filtrate is concentrated into about 10ml, adds ethanol 30ml jolting, leave standstill, filter, filtrate is steamed to there not being the alcohol flavor, extract secondary (25ml, 20ml for the second time for the first time) with petroleum ether (30～60 ℃) jolting, centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving, makes Rhizoma Atractylodis Macrocephalae control medicinal material solution; Draw described Rhizoma Atractylodis Macrocephalae need testing solution 10 μ l, Rhizoma Atractylodis Macrocephalae control medicinal material solution 3 μ l, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (7: 3) is developing solvent, launch, take out, dry, spray is with 10% sulfuric acid solution of 5% paradime thylaminobenzaldehyde, in about 7～10 minutes of 105 ℃ of heating, put under the ultra-violet lamp 365nm and inspect; And/or
(3) thin layer chromatography of discriminating Radix Saposhnikoviae: get preparation 5g, add water 20ml and make dissolving, filter, filter washs with 5ml moisture, washing liquid and filtrate merge, extract secondary (25ml, 20ml for the second time for the first time) with petroleum ether (30～60 ℃) jolting, centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving, as the Radix Saposhnikoviae need testing solution; Get Radix Saposhnikoviae control medicinal material 2g, add water 250ml, decocted 30 minutes, filter, filtrate is concentrated into about 10ml, adds ethanol 30ml jolting, leave standstill, filter, filtrate is steamed to there not being the alcohol flavor, extract secondary (25ml, 20ml for the second time for the first time) with petroleum ether (30～60 ℃) jolting, centrifugal, merge petroleum ether extract, volatilize, residue adds methanol 0.5ml makes dissolving, makes Radix Saposhnikoviae control medicinal material solution; Drawing described Radix Saposhnikoviae need testing solution 10 μ l, Radix Saposhnikoviae control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, is developing solvent with petroleum ether (60～90 ℃)-ethyl acetate (1: 1), launches, and takes out, and dries, and puts under the ultra-violet lamp 365nm and inspects.
5. the detection method of the described jade screen of claim 1 air port formulation is characterized in that, this method adopts the content of astragaloside in the high effective liquid chromatography for measuring preparation.
6. method according to claim 5 is characterized in that, the need testing solution preparation at first adopts the methanol Soxhlet to extract in the described method, and next adopts saturated n-butanol extraction, adopts ammoniacal liquor to wash at last.
7. according to claim 5 or 6 described methods, it is characterized in that described need testing solution prepares by following steps:
Get the preparation porphyrize, get the preferred 2.5g of about 1～10g, the accurate title, decide, and puts in the apparatus,Soxhlet's, add the preferred 100ml of methanol 10～300ml, reflux is to extracting liquid colourless, and extracting solution reclaims solvent and is concentrated into driedly, and residue adds water 20ml, slight fever makes dissolving, extract 4 times with the water-saturated n-butanol jolting, the preferred 40ml of each 10～100ml merges n-butyl alcohol liquid, with ammoniacal liquor thorough washing 2 times, the preferred 40ml of each 10～100ml merges ammoniacal liquor and extracts the preferred 20ml of each 5～50ml 2 times with the water-saturated n-butanol jolting, discard ammoniacal liquor, merge n-butyl alcohol liquid, evaporate to dryness, residue add methanol to be made dissolving and is transferred in the 10ml measuring bottle, be diluted to scale with methanol, shake up, filter, get subsequent filtrate.
8. method according to claim 7 is characterized in that, described methanol Soxhlet extraction time is more than 3 hours, is preferably 6 hours.
9. according to each described method in the claim 5 to 8, it is characterized in that the chromatographic condition in the described method is: filler is an octadecylsilane chemically bonded silica; Mobile phase is acetonitrile-water (20～50: 50～80, preferred 32: 68); Detector is an evaporative light scattering detector; Drift tube temperature is 103 ℃; Carrier gas flux is 2.8L/min; And/or column temperature is 35 ℃.
10. according to each described method in the claim 5 to 9, it is characterized in that the Astragaloside content scope that described method is measured is that every gram granule contains astragaloside 0.35mg～2.75mg.
11. each described method application aspect the quality control in jade screen air port formulation is produced in the claim 1 to 10, described oral formulations is preferably granular preparation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105044260A (en) * | 2015-06-30 | 2015-11-11 | 广州市香雪制药股份有限公司 | Yupingfeng preparation fingerprint construction method and detection method |
| CN109655572A (en) * | 2019-02-28 | 2019-04-19 | 广东省第二中医院（广东省中医药工程技术研究院） | A kind of thin layer chromatography of quick identification Yupingfeng Granules ingredient |
| CN111504943A (en) * | 2020-05-09 | 2020-08-07 | 广东省第二中医院（广东省中医药工程技术研究院） | Construction method and detection method of near-infrared quantitative model of Yupingfeng preparation |
| CN111521701A (en) * | 2020-04-30 | 2020-08-11 | 广东省第二中医院（广东省中医药工程技术研究院） | Near-infrared correction model construction method and detection method in Yupingfeng preparation extraction |
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2009
- 2009-08-04 CN CN2009101615835A patent/CN101987115A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105044260A (en) * | 2015-06-30 | 2015-11-11 | 广州市香雪制药股份有限公司 | Yupingfeng preparation fingerprint construction method and detection method |
| CN105044260B (en) * | 2015-06-30 | 2016-08-24 | 广州市香雪制药股份有限公司 | The construction method of Yupingfeng preparation finger and detection method |
| CN109655572A (en) * | 2019-02-28 | 2019-04-19 | 广东省第二中医院（广东省中医药工程技术研究院） | A kind of thin layer chromatography of quick identification Yupingfeng Granules ingredient |
| CN111521701A (en) * | 2020-04-30 | 2020-08-11 | 广东省第二中医院（广东省中医药工程技术研究院） | Near-infrared correction model construction method and detection method in Yupingfeng preparation extraction |
| CN111504943A (en) * | 2020-05-09 | 2020-08-07 | 广东省第二中医院（广东省中医药工程技术研究院） | Construction method and detection method of near-infrared quantitative model of Yupingfeng preparation |
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Open date: 20110330 |