CN103954724A - Method for detecting Jingfang granules - Google Patents
Method for detecting Jingfang granules Download PDFInfo
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Abstract
The invention relates to a method for detecting Jingfang granules. The method comprises the steps of character identifying, checking and measuring content, wherein the step of identifying comprises identification of schizonepeta, radix angelicae pubescentis, ligusticum wallichii, fructus aurantii and bupleurum longiradiatum; the step of measuring content refers to a step of measuring content of ephedrine hydrochloride. Aiming at the problem that the condition that fewer raw materials are added or corresponding raw materials are not added by illegal manufacturer or a counterfeit drug bupleurum longiradiatum is mixed cannot be monitored because active ingredients of the granules cannot be correspondingly detected by a set of perfect detection method at present, a scientific, reasonable, practical and feasible component identification and content measurement method is formulated, the clinical effects of the Jingfang granules are guaranteed, quality indexes of several medicinal materials are clear, and application of various medicinal materials in the Jingfang granules is ensured, so that the curative effect of the drug is guaranteed. Moreover, the counterfeit drug bupleurum longiradiatum in radix bupleuri can be effectively detected, and a phenomenon that health of patients is endangered by two toxic ingredients, including bupleurotoxin and acetylbupleurotoxin, contained in bupleurum longiradiatum is avoided.
Description
Technical field
The present invention relates to the detection method of the anti-particle of a kind of chaste tree.
Background technology
Anti-(electuary) particle of chaste tree is second kind of recording of " the Sanitation Ministry medicine standard " Traditional Chinese medicine historical preparation, standard number is WS3-B-0328-90, prescription, for schizonepeta, windproof, notopterygium root, levisticum, radix bupleuri, the root of purple-flowered peucedanum, Ligusticum wallichii, Fructus Aurantii, Poria cocos, balloonflower root, Radix Glycyrrhizae, is pure Chinese medicine and granule.It has inducing sweat and dispelling exogenous evils, the effect of loose wind clearing damp.Be used for the treatment of clinically cold, headache bodily pain, aversion to cold is lossless, nasal obstruction runny nose, cough.To be used for the treatment of in the market cold, headache bodily pain, aversion to cold is lossless, nasal obstruction runny nose, the common drug of cough.But up to the present, also do not have a set of perfect detection method to detect accordingly its effective ingredient, may cause so illegal manufacturer not prepared burden in strict accordance with the dosage of writing out a prescription in the time producing medicine, wantonly reduce the raw material that price is high, cause the curative effect of medicine obviously to decline, affect the safe and effective of medicine, grievous injury patient's interests.On the other hand, in prescription, use medicinal material radix bupleuri, because of its use amount larger, and its output is limited, so its adulterant bigleaf thorowax root is also had a mind to or is not intended to sneak into use, but contains bupleurotoxin and acetylbupleurotoxin in bigleaf thorowax root, these two kinds of compositions are all noxious materials, repeatedly there is the poisoning Adverse drug events of medicine that is mixed with bigleaf thorowax root because taking, so it is necessary to control bigleaf thorowax root.The discriminating control problem of bigleaf thorowax root medicinal material in pharmacopeia also inquired in " Shandong medical industry " the 22 the 5th phase of volume in 2003 " to supplementing of the Chinese Pharmacopoeia version radix bupleuri method of inspection in 2000 " literary composition, but its method has obvious deficiency: place 24 hours, detection time is oversize, is unfavorable for drug production process control and drug quality supervision and check; Because of bupleurotoxin and acetylbupleurotoxin content relatively low, point sample is 2 μ l only, point sample amount is very few, the accuracy of impact inspection; Because of bupleurotoxin and acetylbupleurotoxin content relatively low, under uviol lamp, inspect, observe without chromogenic reagent, observing effect is bad.Main is many, the contained complicateds of the anti-particle prescription flavour of a drug of chaste tree, and other composition can produce to be obscured and disturbs.Other Chinese patent drug that contains radix bupleuri is also the same, and because its prescription flavour of a drug are many, complicated, wherein will control bigleaf thorowax root very difficult, so finding a kind of better way, to control sneaking into of bigleaf thorowax root be the task of top priority.
Summary of the invention
Object of the present invention, be to provide the detection method of the anti-particle of a kind of chaste tree, can effectively monitor illegal manufacturer and throw less or do not throw corresponding raw material, monitor sneaking into of adulterant bigleaf thorowax root simultaneously, prevent from taking the generation of rear poisoning Adverse drug events, make this drug safety effective, and ensured the clinical efficacy of Yinchai Granules.
Technical scheme of the present invention is as follows:
The prescription of the anti-particle of this chaste tree: schizonepeta 75g, windproof 75g, notopterygium root 75g, levisticum 75g, radix bupleuri 75g, root of purple-flowered peucedanum 75g, Ligusticum wallichii 75g, Fructus Aurantii 75g, Poria cocos 75g, balloonflower root 75g, Radix Glycyrrhizae 25g.
The detection method of the anti-particle of this chaste tree, comprise proterties, discriminating, inspection, assay project, wherein, discriminating comprises the discriminating of schizonepeta, the discriminating of levisticum, the discriminating of Ligusticum wallichii, the discriminating of Fructus Aurantii, the discriminating of bigleaf thorowax root, the assay that assay is ephedrine hydrochloride, and detection method comprises following:
The discriminating of schizonepeta is: taking schizonepeta as control medicinal material, taking sherwood oil-chloroform-methanol as developping agent, differentiate by thin-layered chromatography;
The discriminating of levisticum is: taking levisticum as control medicinal material, taking sherwood oil-chloroform-methanol as developping agent, differentiate by thin-layered chromatography;
The discriminating of Ligusticum wallichii is: taking Ligusticum wallichii as control medicinal material, taking sherwood oil-chloroform-methanol as developping agent, differentiate by thin-layered chromatography;
The discriminating of Fructus Aurantii is: taking Fructus Aurantii as control medicinal material, place the subnatant spending the night as developping agent taking chloroform-methanol-water, differentiate by thin-layered chromatography;
The discriminating of bigleaf thorowax root is: taking bupleurotoxin, acetylbupleurotoxin as reference substance, taking normal hexane-ethyl acetate as developping agent, differentiate by thin-layered chromatography.
The assay of ephedrine hydrochloride: be taking ephedrine hydrochloride as reference substance, with high performance liquid chromatography row assay.
Detection method comprises following:
(1) discriminating of schizonepeta
Get this product 10g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as need testing solution, separately get schizonepeta control medicinal material 1g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as shining medicinal material solution, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=9～11:2～4:1.5～2.5 are as developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color,
(2) discriminating of levisticum
Get this product 10g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get levisticum control medicinal material 1g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=18～22:4～6:1.5～2.5 are as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of Ligusticum wallichii
Get this product 10g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution, separately get Ligusticum wallichii control medicinal material 1g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=4～6:1.5～2.5:0.7～1.3 are as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of Fructus Aurantii
Get this product 10g, add acetone 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get ephedrine hydrochloride reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, select chloroform: methyl alcohol: the mixed liquor of water=11～15:6～8:1.5～2.5, the subnatant spending the night 10 DEG C of following placements is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(5) discriminating of bigleaf thorowax root
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make the reference substance solution of every 1ml containing bupleurotoxin 1mg and acetylbupleurotoxin 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=6～10:0.5～1.5 are as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the not spot of aobvious same color,
(6) assay of ephedrine hydrochloride
With octadecylsilane chemically bonded silica be filling agent, acetonitrile: 0.2% phosphoric acid=17.5:82.5 is mobile phase, 35 DEG C of column temperatures, detection wavelength is 283nm, flow velocity 1.0ml/min, number of theoretical plate calculates and should be not less than 5000 by ephedrine hydrochloride peak, take and use phosphorus pentoxide to be dried the ephedrine hydrochloride reference substance 0.00503g of 24 hours in 50ml measuring bottle, adding formamide dissolves and is diluted to scale, shake up, draw this reference substance solution 5ml in 10ml measuring bottle, adding formamide dissolves and is diluted to scale, obtain the ephedrine hydrochloride reference substance solution of every 1ml containing 50.30 μ g, get this product 1.0g, add formamide 50ml, weighed weight, ultrasonic processing 15 minutes, let cool, weighed weight again, supply the weight of less loss with formamide, shake up, with 0.45 μ m miillpore filter filtration, get subsequent filtrate, obtain need testing solution, accurate reference substance solution and the each 10ul of need testing solution of drawing, injection liquid chromatography, measure peak area, calculate by external standard method, obtain.
Every bag of this product in ephedrine hydrochloride (C27H32O14), must not be less than 7.5mg containing Fructus Aurantii.
Detection method is as follows more specifically:
(1) discriminating of schizonepeta
Get this product 10g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as need testing solution, separately get schizonepeta control medicinal material 1g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as shining medicinal material solution, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=10:3:2 is as developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color,
(2) discriminating of levisticum
Get this product 10g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get levisticum control medicinal material 1g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=20:5:2 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of Ligusticum wallichii
Get this product 10g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution, separately get Ligusticum wallichii control medicinal material 1g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=5:2:1 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of Fructus Aurantii
Get this product 10g, add acetone 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get ephedrine hydrochloride reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, select chloroform: methyl alcohol: water=13: the mixed liquor of 7: 2, the subnatant spending the night 10 DEG C of following placements is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(5) discriminating of bigleaf thorowax root
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make the reference substance solution of every 1ml containing bupleurotoxin 1mg and acetylbupleurotoxin 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=8:1 as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the not spot of aobvious same color,
(6) assay of ephedrine hydrochloride
With octadecylsilane chemically bonded silica be filling agent, acetonitrile: 0.2% phosphoric acid=17.5:82.5 is mobile phase, 35 DEG C of column temperatures, detection wavelength is 283nm, flow velocity 1.0ml/min, number of theoretical plate calculates and should be not less than 5000 by ephedrine hydrochloride peak, take and use phosphorus pentoxide to be dried the ephedrine hydrochloride reference substance 0.00503g of 24 hours in 50ml measuring bottle, adding formamide dissolves and is diluted to scale, shake up, draw this reference substance solution 5ml in 10ml measuring bottle, adding formamide dissolves and is diluted to scale, obtain the ephedrine hydrochloride reference substance solution of every 1ml containing 50.30 μ g, get this product 1.0g, add formamide 50ml, weighed weight, ultrasonic processing 15 minutes, let cool, weighed weight again, supply the weight of less loss with formamide, shake up, with 0.45 μ m miillpore filter filtration, get subsequent filtrate, obtain need testing solution, accurate reference substance solution and the each 10ul of need testing solution of drawing, injection liquid chromatography, measure peak area, calculate by external standard method, obtain the content of this product.
Every bag of this product in ephedrine hydrochloride (C27H32O14), must not be less than 7.5mg containing Fructus Aurantii.
Proterties: this product is brown particle; Gas perfume (or spice), sweet, the micro-hardship of taste.
Check: should meet every regulation relevant under granule item (annex I C of " Chinese Pharmacopoeia " version in 2010).
The ratio of developping agent of the present invention and the ratio of mobile phase are all in volume ratio.
Technique effect of the present invention:
The present invention is by the discriminating to the schizonepeta in the anti-particle of chaste tree, the discriminating of levisticum, the discriminating of Ligusticum wallichii, the discriminating of Fructus Aurantii, the discriminating of bigleaf thorowax root, the assay of ephedrine hydrochloride, make the Main Ingredients and Appearances such as schizonepeta, levisticum, Ligusticum wallichii, Fructus Aurantii in prescription all obtain effective monitoring, on the other hand, the adulterant bigleaf thorowax root of radix bupleuri is also effectively detected, and has avoided these two kinds of toxic substances harm patients' of the bupleurotoxin that contains in bigleaf thorowax root and acetylbupleurotoxin health.The present invention can monitor the quality of the anti-particle of chaste tree better and more comprehensively; and can effectively control the anti-particle of illegal manufacturers produce chaste tree of poor quality, thus ensure the curative effect of medicine, ensure the safety of medicine; protected patient's interests, this method is scientific and reasonable, practical.
The present invention is studied assay, and specific experiment data is as follows:
The investigation of content assaying method
1, instrument and reagent:
1.1HP1100 high performance liquid chromatograph, is configured to G1311A quaternary pump, G1313A automatic sampler, G1316A column oven, G1314A UV-detector, HP chem workstation.
1.2 chromatographic columns: BDS-C18 post Kromasil (250mm × 4.6mm).
1.3 ephedrine hydrochloride reference substances (research institute provides by Products in China, and lot number is 0722-201008), methyl alcohol (chromatographically pure), phosphoric acid (analyzing pure), water are self-control redistilled water.
2, chromatographic condition and system suitability: with octadecylsilane chemically bonded silica be filling agent; Acetonitrile-0.2% phosphoric acid (17.5:82.5) is mobile phase; 35 DEG C of column temperatures, detection wavelength is 283nm; Flow velocity 1.0ml/min; Number of theoretical plate calculates and should be not less than 5000 by ephedrine hydrochloride peak.
3, the preparation of reference substance solution: precision takes through the phosphorus pentoxide ephedrine hydrochloride reference substance 0.00503g of dry 24 hours in 50ml measuring bottle, adding formamide dissolves and is diluted to scale, shake up, accurate this reference substance solution 5ml that draws, in 10ml measuring bottle, obtains the ephedrine hydrochloride reference substance solution of every 1ml containing 50.30 μ g.
4, the preparation of need testing solution: get this product 1.0g, accurately weighed, precision adds formamide 50ml, weighed weight, ultrasonic processing 15 minutes, lets cool, more weighed weight, supplies the weight of less loss with formamide, shake up, with 0.45 μ m miillpore filter filtration, get subsequent filtrate, to obtain final product.
5, determination method: accurate reference substance solution and the each 10ul of need testing solution of drawing respectively, injection liquid chromatography, measures peak area, calculates by external standard method, to obtain final product.
6, methodological study
6.1, the selection of chromatographic condition and system suitability
With octadecylsilane chemically bonded silica be filling agent; Acetonitrile-0.2% phosphoric acid (17.5:82.5) is mobile phase; Column temperature is 35 DEG C; Flow velocity is 1.0ml/min; Selective determination wavelength is 283nm, detects by UV-detector.With this understanding, ephedrine hydrochloride and other components all can reach baseline separation, and experiment shows: in test sample, have the peak consistent with ephedrine hydrochloride reference substance retention time, negative control is noiseless.
The investigation of 6.2 ranges of linearity:
Precision takes through the phosphorus pentoxide ephedrine hydrochloride reference substance 0.00503g of dry 24 hours in 50ml measuring bottle, adds formamide and dissolves and be diluted to scale, shakes up.Accurate this reference substance solution 1,3,5,7, the 9ml of drawing, in 5 10ml measuring bottles, is diluted to scale with methyl alcohol, and the accurate 10 μ l that draw inject high performance liquid chromatographs respectively, measure, taking concentration as horizontal ordinate, peak area is that ordinate returns processing, obtains regression equation:
A＝32.9204098C-1.9912226(n＝5),γ＝1.00000
Result shows that ephedrine hydrochloride is good linear relationship between sample size 0.1006 μ g-0.9054 μ g, the results are shown in Table 1.
Table 1 ephedrine hydrochloride typical curve test findings
The investigation of 6.3 precision:
Ephedrine hydrochloride reference substance solution (concentration is 50.03 μ g/ml) is repeated to sample introduction five times, measure peak area, ephedrine hydrochloride peak area mean value=1654.4886, RSD=0.24%.Result shows: precision is good, the results are shown in Table 2.
Table 2 precision is investigated result
6.4 replica test
Precision takes (050601) 5 part, same lot number sample, by need testing solution preparation method preparation, measures its content in accordance with the law, and mean value is 11.557mg/ bag, RSD=0.62%.The results are shown in Table 3, test shows: the repeatability of assay method is good.
Table 3: sample replica test
6.5 application of sample recovery experiments
Precision takes the about 0.50g of sample that lot number is 050601 (known content is 2.30mg/g) respectively, put in the measuring bottle of 6 50ml, add respectively again ephedrine hydrochloride reference substance solution (concentration is 1.12mg/ml) 1.0ml, by above-mentioned need testing solution preparation method and chromatographic condition, preparing application of sample reclaims need testing solution and injects high performance liquid chromatograph, measure content, with following formula calculate recovery rate, the results are shown in Table 4, test findings shows: the recovery is between 96.64%～102.3%, and application of sample reclaims good.
Table 4 ephedrine hydrochloride application of sample recovery test result
6.6 stability tests: the sample that is (050601) by lot number is prepared need testing solution by need testing solution preparation method, and respectively at 0 hour, 1 hour, 2 hours, 4 hours, 8 hours, the accurate 10 μ l that draw inject high performance liquid chromatograph, measure peak area integrated value, the results are shown in Table 5, result shows: under this experiment condition, Determination of ephedrine hydrochloride is stable in 8 hours.
The stability test of table 5 ephedrine hydrochloride
Therefore: every bag of the 3 batches of anti-particle Determination of ephedrine hydrochloride of chaste tree is between 4.606mg-4.899mg, more stable.
Through above experiment, prove method reasonable of the present invention.
Embodiment
Embodiment 1:
The windproof 75g notopterygium root of [prescription] schizonepeta 75g 75g levisticum 75g radix bupleuri 75g root of purple-flowered peucedanum 75g Ligusticum wallichii 75g Fructus Aurantii 75g Poria cocos 75g balloonflower root 75g Radix Glycyrrhizae 25g
Simply, schizonepeta, windproof, notopterygium root, levisticum, the root of purple-flowered peucedanum, Ligusticum wallichii and Fructus Aurantii are extracted respectively volatile oil to [method for making] above ten, and the another device of aqueous solution after Ligusticum wallichii, Fructus Aurantii distillation is collected; The dregs of a decoction of Ligusticum wallichii, Fructus Aurantii and Poria cocos, according to the percolation under liquid extract and extract item, be made into 25% ethanolic solution by above-mentioned aqueous solution and make solvent, carries out diacolation; The three taste boiling secondaries such as the dregs of a decoction of schizonepeta, windproof, notopterygium root, levisticum and the root of purple-flowered peucedanum and all the other radix bupleuri, balloonflower root, Radix Glycyrrhizae, each 1.5 hours, collecting decoction, filtered, and filtrate is condensed into thick paste; Merge filter liquid and thick paste, mix, leave standstill, filter, at the temperature of 80～85 DEG C, it is 1.30 clear cream that filtrate is condensed into relative density, and 1 part of qinghuo reagent, with 6 parts of sucrose, mixes granulation, dry, adds the volatile oil such as above-mentioned schizonepeta, mixes, and to obtain final product.
[proterties] this product is brown particle; Gas perfume (or spice), sweet, the micro-hardship of taste.
The discriminating of [discriminating] (1) schizonepeta
Get this product 10g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as need testing solution, separately get schizonepeta control medicinal material 1g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as shining medicinal material solution, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=9:2:1.5 is as developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color,
(2) discriminating of levisticum
Get this product 10g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get levisticum control medicinal material 1g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=18:4:1.5 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of Ligusticum wallichii
Get this product 10g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution, separately get Ligusticum wallichii control medicinal material 1g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=4:1.5:0.7 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of Fructus Aurantii
Get this product 10g, add acetone 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get ephedrine hydrochloride reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, select chloroform: the mixed liquor of methyl alcohol: water=11:6:1.5, the subnatant spending the night 10 DEG C of following placements is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(5) discriminating of bigleaf thorowax root
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make the reference substance solution of every 1ml containing bupleurotoxin 1mg and acetylbupleurotoxin 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=6:0.5 as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the not spot of aobvious same color,
[inspection] should meet every regulation relevant under granule item (annex I C of " Chinese Pharmacopoeia " version in 2010).
[assay] is according to high effective liquid chromatography for measuring.
With octadecylsilane chemically bonded silica be filling agent, acetonitrile: 0.2% phosphoric acid=17.5:82.5 is mobile phase, 35 DEG C of column temperatures, detection wavelength is 283nm, flow velocity 1.0ml/min, number of theoretical plate calculates and should be not less than 5000 by ephedrine hydrochloride peak, take ephedrine hydrochloride reference substance 0.00503g in 50ml measuring bottle, adding formamide dissolves and is diluted to scale, shake up, draw this reference substance solution 5ml in 10ml measuring bottle, adding formamide dissolves and is diluted to scale, obtain the ephedrine hydrochloride reference substance solution of every 1ml containing 50.30 μ g, get this product 1.0g, add formamide 50ml, weighed weight, ultrasonic processing 15 minutes, let cool, weighed weight again, supply the weight of less loss with formamide, shake up, filter with miillpore filter, get subsequent filtrate, obtain need testing solution, accurate reference substance solution and the each 10ul of need testing solution of drawing, injection liquid chromatography, measure peak area, calculate by external standard method, obtain the content of this product.
Every bag of this product in ephedrine hydrochloride (C27H32O14) 7.9mg, is no less than 7.5mg containing Fructus Aurantii.
Embodiment 2:
In the present embodiment, except discrimination method difference, all the other detection methods are all identical with embodiment 1, and concrete discrimination method is as follows:
(1) discriminating of schizonepeta
Get this product 10g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as need testing solution, separately get schizonepeta control medicinal material 1g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as shining medicinal material solution, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=10:3:2 is as developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color,
(2) discriminating of levisticum
Get this product 10g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get levisticum control medicinal material 1g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=20:5:2 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of Ligusticum wallichii
Get this product 10g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution, separately get Ligusticum wallichii control medicinal material 1g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=5:2:1 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of Fructus Aurantii
Get this product 10g, add acetone 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get ephedrine hydrochloride reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, select chloroform: methyl alcohol: water=13: the mixed liquor of 7: 2, the subnatant spending the night 10 DEG C of following placements is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(5) discriminating of bigleaf thorowax root
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make the reference substance solution of every 1ml containing bupleurotoxin 1mg and acetylbupleurotoxin 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=8:1 as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the not spot of aobvious same color,
Embodiment 3:
In the present embodiment, except discrimination method difference, all the other detection methods are all identical with embodiment 1, and concrete discrimination method is as follows:
(1) discriminating of schizonepeta
Get this product 10g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as need testing solution, separately get schizonepeta control medicinal material 1g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as shining medicinal material solution, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=11:4:2.5 is as developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color,
(2) discriminating of levisticum
Get this product 10g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get levisticum control medicinal material 1g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=22:6:2.5 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of Ligusticum wallichii
Get this product 10g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution, separately get Ligusticum wallichii control medicinal material 1g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=6:2.5:1.3 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of Fructus Aurantii
Get this product 10g, add acetone 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get ephedrine hydrochloride reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, select chloroform: the mixed liquor of methyl alcohol: water=15:8:2.5, the subnatant spending the night 10 DEG C of following placements is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(5) discriminating of bigleaf thorowax root
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make the reference substance solution of every 1ml containing bupleurotoxin 1mg and acetylbupleurotoxin 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=10:1.5 as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the not spot of aobvious same color.
Claims (4)
1. the detection method of the anti-particle of chaste tree, comprise proterties, discriminating, inspection, assay project, it is characterized in that: described discriminating comprises the discriminating of schizonepeta, the discriminating of levisticum, the discriminating of Ligusticum wallichii, the discriminating of Fructus Aurantii, the discriminating of bigleaf thorowax root, assay is the assay of ephedrine hydrochloride, and detection method comprises following:
(1) discriminating of schizonepeta
Get this product 10g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as need testing solution, separately get schizonepeta control medicinal material 1g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as shining medicinal material solution, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=9～11:2～4:1.5～2.5 are as developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color,
(2) discriminating of levisticum
Get this product 10g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get levisticum control medicinal material 1g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=18～22:4～6:1.5～2.5 are as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of Ligusticum wallichii
Get this product 10g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution, separately get Ligusticum wallichii control medicinal material 1g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=4～6:1.5～2.5:0.7～1.3 are as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of Fructus Aurantii
Get this product 10g, add acetone 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get ephedrine hydrochloride reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, select chloroform: methyl alcohol: the mixed liquor of water=11～15:6～8:1.5～2.5, the subnatant spending the night 10 DEG C of following placements is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(5) discriminating of bigleaf thorowax root
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make the reference substance solution of every 1ml containing bupleurotoxin 1mg and acetylbupleurotoxin 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=6～10:0.5～1.5 are as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the not spot of aobvious same color,
(6) assay of ephedrine hydrochloride
With octadecylsilane chemically bonded silica be filling agent, acetonitrile: 0.2% phosphoric acid=17.5:82.5 is mobile phase, 35 DEG C of column temperatures, detection wavelength is 283nm, flow velocity 1.0ml/min, number of theoretical plate calculates and should be not less than 5000 by ephedrine hydrochloride peak, take ephedrine hydrochloride reference substance 0.00503g in 50ml measuring bottle, adding formamide dissolves and is diluted to scale, shake up, draw this reference substance solution 5ml in 10ml measuring bottle, adding formamide dissolves and is diluted to scale, obtain the ephedrine hydrochloride reference substance solution of every 1ml containing 50.30 μ g, get this product 1.0g, add formamide 50ml, weighed weight, ultrasonic processing 15 minutes, let cool, weighed weight again, supply the weight of less loss with formamide, shake up, filter with miillpore filter, get subsequent filtrate, obtain need testing solution, accurate reference substance solution and the each 10ul of need testing solution of drawing, injection liquid chromatography, measure peak area, calculate by external standard method, obtain.
2. the detection method of the anti-particle of chaste tree according to claim 1, is characterized in that: discrimination method is as follows more specifically:
(1) discriminating of schizonepeta
Get this product 10g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as need testing solution, separately get schizonepeta control medicinal material 1g, 50ml adds diethyl ether, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, as shining medicinal material solution, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=10:3:2 is as developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color,
(2) discriminating of levisticum
Get this product 10g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get levisticum control medicinal material 1g, add 60～90 DEG C of sherwood oil 40ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate volatilizes, residue adds methyl alcohol 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=20:5:2 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(3) discriminating of Ligusticum wallichii
Get this product 10g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, as need testing solution, separately get Ligusticum wallichii control medicinal material 1g, add methyl alcohol 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds ethyl acetate 1ml to be made to dissolve, medicinal material solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking sherwood oil: chloroform: methyl alcohol=5:2:1 is as developping agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
(4) discriminating of Fructus Aurantii
Get this product 10g, add acetone 30ml, ultrasonic processing 20 minutes, filter, filtrate is put evaporate to dryness in water-bath, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution, separately get ephedrine hydrochloride reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, select chloroform: methyl alcohol: water=13: the mixed liquor of 7: 2, the subnatant spending the night 10 DEG C of following placements is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color,
(5) discriminating of bigleaf thorowax root
Get this product 10g, add 60～90 DEG C of sherwood oil 30ml, soak 10 minutes, ultrasonic processing 15 minutes, filter, filtrate is waved to 1ml, as need testing solution, separately get bupleurotoxin, acetylbupleurotoxin reference substance, add methyl alcohol and make the reference substance solution of every 1ml containing bupleurotoxin 1mg and acetylbupleurotoxin 1mg, product solution in contrast, test according to thin-layered chromatography, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, taking normal hexane: ethyl acetate=8:1 as developping agent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, be heated to spot colour developing at 105 DEG C clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the not spot of aobvious same color.
3. the detection method of the anti-particle of chaste tree according to claim 1, is characterized in that: the ephedrine hydrochloride reference substance in step (6) uses phosphorus pentoxide to be dried 24 hours.
4. the detection method of the anti-particle of chaste tree according to claim 1, is characterized in that: the miillpore filter aperture in step (6) is 0.45 μ m.
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