CN102023157B - Quick measurement method for pyrazolone substances doped in medicaments and health-care food - Google Patents
Quick measurement method for pyrazolone substances doped in medicaments and health-care food Download PDFInfo
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Abstract
The invention discloses a quick measurement method for pyrazolone substances doped in medicaments and health-care food. The method comprises the following steps of: (1) extracting aminopyrine and similar components thereof in the medicaments and the health-care food to obtain extract; (2) further extracting the extract by using a solvent, and collecting extract and extracted solution serving as sample solution respectively, and (3) adding a developing agent into the sample solution respectively. The detection method is quick, simple and convenient, has strong specificity, high accuracy, sensitive response and wide application range, and is suitable for inspecting whether the medicaments and the health-care food are doped with the aminopyrine and the similar components thereof on site. A quick detection kit for the aminopyrine and the similar components thereof can meet the requirements of medicament development and health-care food supervision and inspection in vast rural areas and middle and small-sized cities with behindhand inspection technology.
Description
Technical field
The present invention relates to the detection method of a kind of pyrazolone chemical constitution aminopyrine and analog thereof, specifically be to detect in medicine and the health food, in particular for detecting the method for whether adding aminopyrine, antipyrine and analgin composition in antirheumatic Chinese medicine preparation and the health food.
Background technology
Pyrazolone chemical constitution aminopyrine and analogue antipyretic effect thereof are stronger, and slowly and lasting, the anti-inflammatory anti rheumatism action is similar to aspirin.By suppressing the synthetic of hypothalamus prostaglandin and discharge, recover the reactivity of heat-regulating centers receptive neuron and play antipyretic effect; By suppressing Cycloxygenase, selectivity suppresses synthesizing of hypothalamus heat-regulating centers prostaglandin, causes the peripheral vascular expansion, perspires and reaches analgesic effect; By suppressing the synthetic of prostaglandin etc. and discharge, improve the threshold of pain and play analgesic activity, belong to the periphery antalgesic.Aminopyrine be because causing bone marrow suppression and can form the nitrosamine carcinogen, thus single superseded with preparation, clinical commonly used be its compound preparation.
The clinical compound preparation that contains aminopyrine and analogue thereof commonly used mostly is prescription medicine at present, needs of patients can be taken under doctor's guidance, national correlation department has carried out strict regulation to production, operation and the use of this similar drug, and the adverse drug reaction that causes for aminopyrine also once had report as nauseating, vomiting, allergic dermatitis etc.But in recent years, illegal situation of adding aminopyrine but is on the rise in some antirheumatic Chinese patent drugs and the health food, and each associated mechanisms has also strengthened the supervision dynamics for this reason, hits the illegal sample that adds aminopyrine.But the Chinese medicine preparation and the health food that illegally add aminopyrine are mainly sold in vast rural area and small and medium-sized cities underdeveloped, because these regional technology ability to supervise weaknesses, lack necessary testing instruments and technology, cause illegally adding the abuse of medicine, bring hidden danger for the people's drug safety.
Illegal method of adding aminopyrine and analogue thereof mainly contains following three kinds in check medicine and the health food:
1, thin-layered chromatography:
Composition to be measured in the sample extracts with methenyl choloride, and the need testing solution of gained and reference substance solution point launch with developping agent on same block of thin layer plate (thin layer plate is made by silica gel usually), and after drying, thin layer plate is examined under uviol lamp and shown.Different material occurs with the form of spot on the different position of chromatographic sheet that (reason is that different materials has different migration velocities, often launch the back spot to the distance between the initial point with chromatogram migration value representation), whether judge whether contain target component in the testing sample this experiment gained phenomenon of spot occurring with the reference substance relevant position according to testing sample.The need testing solution of aminopyrine reference substance solution and sample extraction gained is point sample on same chromatographic sheet, developping agent launches, after drying, chromatographic sheet is examined under uviol lamp and is shown, if the need testing solution thin-layer chromatogram is then pointed out in the sample and may be contained aminopyrine spot occurring with the corresponding position of aminopyrine reference substance.
Method: get aminopyrine and analogue is an amount of, dissolve the solution that is mixed with 10mg/ml with methenyl choloride, draw 10 μ l, put on the silica GF254 thin layer plate, (9: 6: 1: 0.01) be developping agent, the exhibition distance was 15.5cm with methenyl choloride-ether-acetone-ammoniacal liquor.After the expansion, dry, put that (254nm) inspects Rf=0.57 under the uviol lamp.
The advantage of thin-layered chromatography is not need to use expensive analytical instrument.This method shortcoming is: (1) chromatographic resolution rate is lower, the Chinese medicine preparation complicated component, disturbing factor is more, easily the erroneous judgement of some compositions is aminopyrine, if some coexistence composition amount is big and chromatogram migration value with aminopyrine approaching then can the jamming target composition detect.(2) development of chromatogram is long with the time of drying, and can not satisfy the requirement of quick mensuration.(3) chromatographic sheet needs drying to deposit, and the temperature and humidity of environment is big to the influence of separating effect.(4) require the experimenter that experience is preferably arranged.(5) fixed place need be arranged, be not suitable for doing mobile big scene and detect.
2, high performance liquid chromatography
High performance liquid chromatography is modern analytical approach commonly used.Under identical chromatographic condition, different materials has different chromatographic retentions.The need testing solution of aminopyrine reference substance solution and sample extraction gained difference sample introduction can judge whether contain aminopyrine in the testing sample according to chromatographic retention under identical chromatographic condition.
Chromatographic condition: chromatographic column: C
18(250mm * 4.6mm, 5 μ m)
Phase flows: methyl alcohol-1% acetum (regulating pH to 3.7 with diethylamine) 34: 66
Flow velocity: 1.0ml/min
Detect wavelength: 260nm
Column temperature: 30 ℃
Sampling volume: 20 μ l
Theoretical cam curve: 11458
Retention time: 13.35min
The advantage of high performance liquid chromatography is chromatographic resolution efficient height, and is highly sensitive.Shortcoming is: (1) instrument is expensive, and time for sample pretreatment is long, chromatographic column vulnerable to pollution, analysis cost height.(2) when the chromatographic retention of chromatographic retention and the aminopyrine of coexistence composition near the time judgement that makes mistake of do easily.(3) instrument requires height to environment for use, needs fixedly put, and is not suitable for doing mobile big scene and detects.
3, high performance liquid chromatography-mass spectrometry method
High performance liquid chromatography-mass spectrometry method is that a kind of analysis cost is higher than high performance liquid chromatography, and operation is than high performance liquid chromatography complex analysis methods more.As separation vessel, mass spectrometer is applicable to analysis complicated component, the sample that background interference is serious as the high performance liquid chromatography-mass spectrometry method of analyzer, can improve the reliability of testing result with high performance liquid chromatograph.
LC-MS condition: use octadecyl silane to be the liquid-phase chromatographic column (column cap installs the pre-chromatographic column of same size filler additional) of filling agent, be the phase that flows to contain 0.02mol/L ammonium acetate-0.1% acetic acid aqueous solution/acetonitrile (30: 70), the detection wavelength is 280nm, sample size 10 μ l, theoretical cam curve is not less than 1000,25 ℃ of column temperatures, mass spectrum assembling electron spray ionisation source (ESI), source voltage 5kV, 275 ℃ of capillary temperatures, capillary voltage 15V, sheath gas velocity 40arb, positive ion detects, and scan mode adopts full scan one-level mass spectrum, full scan second order ms (MS/MS), quality acquisition range 100～1000.
The shortcoming of high performance liquid chromatography-mass spectrometry method is that instrument is higher to the requirement of environment for use, needs fixedly to put, and is not suitable for doing mobile big scene and detects.
The main method that adopts in actual detected at present is high performance liquid chromatography and high performance liquid chromatography-mass spectrometry method.The resolution of these two kinds of methods and sensitivity are all higher, but because required instrument is expensive, experimental implementation complexity, and instrument requiring high reason and being not suitable for rapid screening and the detection of mobile big scene environment for use.
Summary of the invention
The object of the present invention is to provide a kind of defective that overcomes existing detection technique, analysis cost is low, do not need to use valuable analytical instrument, specificity is strong, highly sensitive, be applicable to the method for quickly detecting that whether adds aminopyrine and analog thereof in field test medicine and the health food.
Another object of the present invention is to provide the application of said method at preparation aminopyrine and the quick test kit of analog thereof.
Application in the examination check that another object of the present invention is to provide said method in check medicine, health food, whether to add aminopyrine and analog thereof.
The rapid assay methods of doping aminopyrine and analog thereof in medicine of the present invention, the health food, formed by following steps successively:
(1) aminopyrine and the analog composition thereof in extraction medicine and the health food obtains extract;
(2) further use the described extract of solvent extraction, collect respectively extract and the extraction after solution, as need testing solution;
(3) in described need testing solution, add developer respectively.
Wherein, aminopyrine and the analog composition thereof in water extraction medicine and the health food in the step (1); Use the ethyl acetate extraction extract in the step (2); The extract of collecting in the step (2) is further water dissolving after concentrating, as need testing solution; Developer in the step (3) is ferric ammonium sulfate.
Aminopyrine and analog antipyrine thereof, analgin can and then generate coloured product by the ferric ammonium sulfate oxidation at normal temperatures.
At most of medicines or health food in the market, recommend sampling amount as follows:
| Formulation | Sampling amount |
| Capsule | 1 intragranular is tolerant |
| Tablet | 2 |
[0036]?
| Honeyed bolus | 1/2 ball |
| Granule | 1/2 bag |
| Oral liquid | 1/2 |
Concrete technical scheme is as follows:
For solid sample, should or shred its porphyrize, with the water-soluble solution of 5～10ml, jolting is extracted fully it, leaves standstill a moment, removes by filter insolubles, collects filtrate.Filtrate is used the equal-volume ethyl acetate extraction, leaves standstill a moment after the jolting, shift the ethyl acetate layer extract, concentrate residue, in residue, add 3～5ml water, the residue water layer solution after the vibration dissolving, gained solution and extraction is respectively as need testing solution.
For fluid sample, should measure an amount of sample solution, place separating funnel, add the equal-volume ethyl acetate extraction, shift the ethyl acetate layer extract, concentrate residue, in residue, add 3～5ml water, the vibration dissolving, gained solution and original solution are respectively as need testing solution.
Wherein, the purpose that solid sample is dissolved in water is that the water soluble ingredient in aminopyrine and analogue and the sample is extracted from matrix.
The purpose of ethyl acetate extraction is the pigment of removing on the basis that keeps aminopyrine and analogue thereof in the Chinese medicine preparation, observes the interference that brings to experimental result thereby remove the sample intrinsic colour; Acetic acid ethyl acetate extract concentrated and be in order to make aminopyrine and analogue thereof from ethyl acetate, disperse to come out with the purpose that water redissolves, and need testing solution and water-soluble developer are dissolved each other, be convenient to develop the color.
Drip the ferric sulphate ammonium salt solution in water redissolution solution after concentrating to the ethyl acetate layer extract respectively and the residue water layer solution after the extraction, observe chromogenic reaction.
Contain the sample of aminopyrine and antipyrine after splashing into the ferric sulphate ammonium salt solution, chromogenic reaction takes place in the former, and chromogenic reaction does not take place the latter; Contain the sample of analgin after splashing into the ferric sulphate ammonium salt solution, chromogenic reaction does not take place in the former, and chromogenic reaction takes place the latter.
In the judgement of positive findings, if contain aminopyrine in the sample, then solution becomes purple or bluish violet; If contain antipyrine in the sample, then solution becomes buff or dark brown; If contain analgin in the sample, then solution becomes yellow green.The negative control sample is colourless or faint yellow.
When dripping the ferric ammonium sulfate developer, when adding 1 ferric sulphate ammonium salt solution, can produce the color reaction of moment, disappear subsequently, when the amount of splashing into that increases developer gradually to 1ml, color does not disappear.
Among the present invention, the concentration of developer ferric sulphate ammonium salt solution can be adjusted within the specific limits according to actual conditions.When the concentration of ferric sulphate ammonium salt solution increased, the amount of splashing into reduced, and chromogenic reaction speed is fast, but along with the increase of concentration, the color of developer itself also can be deepened, thereby interference is to the judgement of phenomenon.Therefore the concentration of developer ferric sulphate ammonium salt solution of the present invention is 1%～3%, and is preferred 1.5%～2.5%, more preferably 2%.
According to the present invention, can make the reagent for quickly examining box of aminopyrine and analog antipyrine thereof, analgin.
According to the present invention, can be applied in the examination check that whether medicine, health food mix aminopyrine and analog antipyrine thereof, analgin.
Compare with prior art, the present invention has following advantage:
Fast, easy.The whole operation process comprised flooding 3 minutes, filtered 2 minutes, and ethyl acetate extraction 3 minutes, extract dries up 2 minutes, and residue redissolved 2 minutes, added developer then, and the whole operation process was finished at 12 minutes.Simple and efficient than liquid chromatography, LC-MS method.
Specificity is strong, accuracy rate is high.According to the method validation result, the auxiliary material commonly used of formulations such as tablet, capsule, pill, granule, oral liquid is all noiseless to detecting of aminopyrine and analog thereof.
Be quick on the draw rapidly.The minimum detectability of the present invention's material aminopyrine to be checked, antipyrine and analgin all is lower than clinical minimum effective dose, and after adding developer chromogenic reaction takes place immediately.Therefore with whether add aminopyrine and analogue antipyrine thereof in this method inspection medicine, the health food, analgin has enough sensitivity.
Applied widely.This method can be used for solid pharmaceutical preparation and liquid preparation, no matter is that Chinese medicine preparation or health food all can use this method.
The quick screening method that adds aminopyrine and analogue thereof in Chinese patent drug provided by the invention and the health food without authorization can help timely rapid screening to go out illegal interpolation medicine and health food, be convenient to mobile big execute-in-place, and effectively prevent from illegally adding the abuse of medicine, reliable guarantee is provided for the masses' drug safety.
Embodiment
Following examples will help those of ordinary skill in the art further to understand the present invention, but not limit the present invention in any form.
Among the following embodiment, the compound method of ferric sulphate ammonium salt solution is as follows: for example, 2% ferric sulphate ammonium salt solution is to take by weighing ferric ammonium sulfate 2.0g, adds to obtain after water 100ml dissolves.The preparation Using such method of the ferric sulphate ammonium salt solution of other concentration adjusts the consumption of ferric ammonium sulfate and obtains.
Embodiment 1
Gastrodia capsule (capsule indicates 2/time of doses)
It is tolerant to get 1 intragranular, adds aminopyrine 0.01g (be equivalent to clinical minimum effective dose 1/10th), places the 10ml sample hose, add 5ml water, vibration makes it abundant dissolving, filters, collect filtrate, in filtrate, add 5ml ethyl acetate, jolting 2min, leave standstill, get the ethyl acetate layer extract, shift extract and dry up with hair dryer, in residue, add 4ml water, jolting makes dissolving, gets need testing solution.Add 2% ferric sulphate ammonium salt solution in this solution, solution produces the purple of moment, finally becomes bluish violet.Add 2% ferric sulphate ammonium salt solution 1ml, solution nondiscolouring in the water layer solution after the extraction.
The negative control specimen test: 1 intragranular of getting same sample is tolerant, places the 10ml sample hose, is dissolved in water, and after this operates the samely, filters, extraction the preparation need testing solution.In need testing solution, add 2% ferric sulphate ammonium salt solution 1ml, the equal nondiscolouring of solution respectively.
Embodiment 2
Yaotongning capsules (capsule indicates 2/time of doses)
It is tolerant to get 1 intragranular, adds aminopyrine 0.01g (be equivalent to clinical minimum effective dose 1/10th), places the 10ml sample hose, add 5ml water, vibration makes it abundant dissolving, filters, collect filtrate, in filtrate, add 5ml ethyl acetate, jolting 2min, leave standstill, get the ethyl acetate layer extract, shift extract and dry up with hair dryer, in residue, add 4ml water, jolting makes dissolving, gets need testing solution.Add 1.8% ferric sulphate ammonium salt solution in this solution, solution produces the purple of moment, finally becomes bluish violet.Add 1.8% ferric sulphate ammonium salt solution 1ml, solution nondiscolouring in the water layer solution after the extraction.
The negative control specimen test: 1 intragranular of getting same sample is tolerant, places the 10ml sample hose, is dissolved in water, and after this operates the samely, filters, extraction the preparation need testing solution.In need testing solution, add 1.8% ferric sulphate ammonium salt solution 1ml, the equal nondiscolouring of solution respectively.
Embodiment 3
FENGSHI GUANJIEYAN PIAN (yellow coating tablet, sheet heart grey indicate 4 slices/time of doses)
2 of sample thiefs are removed dressing, grind in mortar, add aminopyrine 0.01g (be equivalent to clinical minimum effective dose 1/10th), place the 10ml sample hose, add 5ml water, vibration makes it abundant dissolving, filters, and collects filtrate, add 5ml ethyl acetate in filtrate, jolting 2min leaves standstill, get the ethyl acetate layer extract, shift extract and dry up with hair dryer, in residue, add 4ml water, jolting makes dissolving, gets need testing solution.Add 1.5% ferric sulphate ammonium salt solution in this solution, solution produces the purple of moment, finally becomes bluish violet.Add 1.5% ferric sulphate ammonium salt solution 1ml, solution nondiscolouring in the water layer solution after the extraction.
Negative control specimen test: get 2 of same sample, remove dressing, in mortar, grind, place the 10ml sample hose, be dissolved in water, after this operate the samely, filter, extraction, the preparation need testing solution.In need testing solution, add 1.5% ferric sulphate ammonium salt solution 1ml, the equal nondiscolouring of solution respectively.
Embodiment 4
FENGSHI GUANJIEYAN PIAN (tablet indicates 4 slices/time of doses)
2 of sample thiefs grind in mortar, add aminopyrine 0.01g (be equivalent to clinical minimum effective dose 1/10th), place the 10ml sample hose, add 5ml water, vibration makes it abundant dissolving, filter, collect filtrate, in filtrate, add 5ml ethyl acetate, jolting 2min leaves standstill, and gets the ethyl acetate layer extract, shifting extract dries up with hair dryer, add 4ml water in residue, jolting makes dissolving, gets need testing solution.Add 1% ferric sulphate ammonium salt solution in this solution, solution produces the purple of moment, finally becomes bluish violet.Add 1% ferric sulphate ammonium salt solution 1ml, solution nondiscolouring in the water layer solution after the extraction.
Negative control specimen test: get 2 of same sample, in mortar, grind, place the 10ml sample hose, be dissolved in water, after this operate the samely, filter, extraction, the preparation need testing solution.In need testing solution, add 1% ferric sulphate ammonium salt solution 1ml, the equal nondiscolouring of solution respectively.
Embodiment 5
Musk rheumatic capsule (capsule indicates 2/time of doses)
It is tolerant to get 1 intragranular, adds analgin 0.05g (be equivalent to clinical minimum effective dose 1/10th), places the 10ml sample hose, add 5ml water, vibration makes it abundant dissolving, filters, collect filtrate, in filtrate, add 5ml ethyl acetate, jolting 2min, leave standstill, get the ethyl acetate layer extract, shift extract and dry up with hair dryer, in residue, add 4ml water, jolting makes dissolving, gets need testing solution.Add 2.2% ferric sulphate ammonium salt solution 1ml in this solution, the solution nondiscolouring adds 2.2% ferric sulphate ammonium salt solution in the water layer solution after the extraction, and solution produces the blue-green of moment, finally becomes yellow green.
The negative control specimen test: it is tolerant to get same sample 1 intragranular, places the 10ml sample hose, is dissolved in water, and after this operates the samely, filters, extraction the preparation need testing solution.In need testing solution, add 2.2% ferric sulphate ammonium salt solution 1ml, the equal nondiscolouring of solution respectively.
Embodiment 6
Musk rheumatic capsule (capsule indicates 2/time of doses)
It is tolerant to get 1 intragranular, adds antipyrine 0.01g, places the 10ml sample hose, add 5ml water, vibration makes it abundant dissolving, filters, collect filtrate, in filtrate, add 5ml ethyl acetate, jolting 2min, leave standstill, get the ethyl acetate layer extract, shift extract and dry up with hair dryer, in residue, add 4ml water, jolting makes dissolving, gets need testing solution.Add 2.5% ferric sulphate ammonium salt solution in this solution, solution produces the yellow of moment, finally becomes dark brown.Add 2.5% ferric sulphate ammonium salt solution 1ml, solution nondiscolouring in the water layer solution after the extraction.
The negative control specimen test: it is tolerant to get same sample 1 intragranular, places the 10ml sample hose, is dissolved in water, and after this operates the samely, filters, extraction the preparation need testing solution.In need testing solution, add 2.5% ferric sulphate ammonium salt solution 1ml, the equal nondiscolouring of solution respectively.
Embodiment 7
Bone spur pain-eliminating capsule (capsule indicates 2/time of doses)
It is tolerant to get 1 intragranular, adds analgin 0.05g (be equivalent to clinical minimum effective dose 1/10th), places the 10ml sample hose, add 5ml water, vibration makes it abundant dissolving, filters, collect filtrate, in filtrate, add 5ml ethyl acetate, jolting 2min, leave standstill, get the ethyl acetate layer extract, shift extract and dry up with hair dryer, in residue, add 4ml water, jolting makes dissolving, gets need testing solution.Add 2.8% ferric sulphate ammonium salt solution 1ml in this solution, the solution nondiscolouring adds 2.8% ferric sulphate ammonium salt solution in the water layer solution after the extraction, and solution produces the blue-green of moment, finally becomes yellow green.
The negative control specimen test: it is tolerant to get same sample 1 intragranular, places the 10ml sample hose, is dissolved in water, and after this operates the samely, filters, extraction the preparation need testing solution.In need testing solution, add 2.8% ferric sulphate ammonium salt solution 1ml, the equal nondiscolouring of solution respectively.
Embodiment 8
Bone spur pain-eliminating capsule (capsule indicates 2/time of doses)
It is tolerant to get 1 intragranular, adds antipyrine 0.01g, places the 10ml sample hose, add 5ml water, vibration makes it abundant dissolving, filters, collect filtrate, in filtrate, add 5ml ethyl acetate, jolting 2min, leave standstill, get the ethyl acetate layer extract, shift extract and dry up with hair dryer, in residue, add 4ml water, jolting makes dissolving, gets need testing solution.Add 3% ferric sulphate ammonium salt solution in this solution, solution produces the yellow of moment, finally becomes dark brown.Add 3% ferric sulphate ammonium salt solution 1ml, solution nondiscolouring in the water layer solution after the extraction.
The negative control specimen test: it is tolerant to get same sample 1 intragranular, places the 10ml sample hose, is dissolved in water, and after this operates the samely, filters, extraction the preparation need testing solution.In need testing solution, add 3% ferric sulphate ammonium salt solution 1ml, the equal nondiscolouring of solution respectively.
Claims (5)
1. mix in a medicine, the health food rapid assay methods of aminopyrine, antipyrine or analgin, formed by following steps successively:
(1) water extracts aminopyrine, antipyrine or the analgin composition in medicine and the health food, obtains extract;
(2) further use the described extract of ethyl acetate extraction, collect the water layer solution after acetic acid ethyl acetate extract and the extraction respectively, acetic acid ethyl acetate extract is dissolved through concentrating the further water in back, with water layer solution after the described extraction respectively as need testing solution; (3) water after concentrating to acetic acid ethyl acetate extract respectively redissolves and adds the developer ferric ammonium sulfate in the residue water layer solution after solution and the extraction, and the concentration of described ferric sulphate ammonium salt solution is 1%-3%, observes chromogenic reaction;
Contain the sample of aminopyrine or antipyrine after splashing into the ferric sulphate ammonium salt solution, chromogenic reaction takes place in the former, and chromogenic reaction does not take place the latter; Contain the sample of analgin after splashing into the ferric sulphate ammonium salt solution, chromogenic reaction does not take place in the former, and chromogenic reaction takes place the latter;
If contain aminopyrine in the sample, then solution becomes purple or bluish violet; If contain antipyrine in the sample, then solution becomes buff or dark brown; If contain analgin in the sample, then solution becomes yellow green.
2. assay method as claimed in claim 1, it is characterized in that: for solid medicine or health food, in described step (1) and (2), be that 1 intragranular of capsule is tolerant, 2 in tablet, honeyed bolus 1/2 ball or granule 1/2 wrap porphyrize or shred, with the water-soluble solution of 5～10ml, jolting is extracted fully it, leaves standstill a moment, remove by filter insolubles, collect filtrate, be extract, filtrate is used the equal-volume ethyl acetate extraction, leave standstill a moment after the jolting, shift the ethyl acetate layer extract, concentrate residue, in residue, add 3～5ml water, the vibration dissolving, the residue water layer solution after gained solution and the extraction is respectively as need testing solution.
3. assay method as claimed in claim 1 is characterized in that:
For fluid sample, in step (1) and (2), be that 1/2 of oral liquid is placed separating funnel, add the equal-volume ethyl acetate extraction, shift the ethyl acetate layer extract, concentrate residue, in residue, add 3～5ml water, the vibration dissolving, gained solution and original solution are respectively as need testing solution.
4. the application of the described assay method of claim 1 in preparation aminopyrine, antipyrine or analgin reagent for quickly examining box.
5. whether the described assay method of claim 1 mixes application in the examination check of aminopyrine, antipyrine or analgin at medicine and health food.
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