CN101907617B - Quick measuring method of aminopyrine mixed in medicine and health-care foods - Google Patents
Quick measuring method of aminopyrine mixed in medicine and health-care foods Download PDFInfo
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Abstract
The invention discloses a quick measuring method of aminopyrine mixed in medicine and health-care foods. The method comprises the following steps of: (1) extracting an aminopyrine ingredient in medicine and health-care foods to obtain an extracting solution; (2) extracting the extracting solution by using a solvent, separating an obtained extracting solution and concentrating to obtain residues; (3) dissolving the residues once again to obtain a test article solution; and (4) adding a detecting agent to the test article solution. The invention has rapidness, convenience, strong specificity, high precision, sensitive reaction and wide application scope and is suitable for detecting whether the aminopyrine is mixed in the medicine and the health-care foods or not on site. A quick aminopyrine detection kit can be prepared according to the invention, which can meet the requirement on the supervision and the inspection of the medicine and the health-care foods in wide rural areas and middle-sized and small cities with lagged inspection technical conditions.
Description
Technical field
The present invention relates to a kind of detection method of aminopyrine composition, specifically is to detect in medicine and the health food, in particular for detecting the method for whether adding the aminopyrine composition in antirheumatic Chinese medicine preparation and the health food.
Background technology
Aminopyrine (Aminophenazone) has another name called pyramidon, dimethylamidoantipyrine, and its chemical name is a 4-dimethylamino-1,5-dimethyl-2-phenyl-3-pyrazolone, and molecular formula is C
13H
17N
3O.
The aminopyrine antipyretic effect is 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 of 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 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 aminopyrine sample that adds.Illegal Chinese medicine preparation and the health food that adds aminopyrine 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 mainly contains following three kinds in check medicine and the health food at present:
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), according to testing sample whether with the reference substance relevant position on this experiment gained phenomenon of spot occurs and judge whether contain target component in the 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 with the corresponding position of aminopyrine reference substance on spot appears, then point out in the sample and may contain aminopyrine.
Method: it is an amount of to get aminopyrine, dissolves the solution that is mixed with 10mg/ml with methenyl choloride, draws 10 μ l, puts on the silica GF254 thin layer plate, and (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 fast measuring.(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) need fixed place, 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)
Moving phase: methyl alcohol-1% acetum (regulating pH to 3.7) 34: 66 with diethylamine
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 costs an arm and a leg, 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 the liquid-phase chromatographic column (column cap install the pre-chromatographic column of same size filler) of octadecyl silane as filling agent, to contain 0.02mol/L ammonium acetate-0.1% acetic acid aqueous solution/acetonitrile (30: 70) is moving phase, 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.
In addition, stipulated three kinds of discrimination methods in the aminopyrine ministerial standard, specific as follows:
Get the about 0.6g of this product, add water 15ml dissolving after, according to following method test:
(1) gets solution 5ml, add 3 in watery hydrochloric acid and ferric trichloride test solution 1ml, promptly show violet; Add dilute sulfuric acid number droplet again, become aubergine.
(2) get solution 5ml, add 5 of silver nitrate test solutions, promptly show violet, gradually separate out the argent of grey black.
(3) get solution 5ml, add rare iron potassuim cyanide test liquid, promptly show mazarine or precipitate.
Above method is used for the fast measuring of medicine and health food aminopyrine composition, all has shortcomings such as sensitivity is not high, specificity is relatively poor.For method (1), when the amount of taking reach clinical minimum pharmaceutical dosage 1/10th the time, the chromogenic reaction phenomenon does not almost observe, and similar reaction can both take place a lot of materials in the Chinese medicine matrix, points out the sensitivity of this method and specificity all lower.The sensitivity of method (2) reaction can meet the demands, but owing to many compositions in the Chinese medicine matrix can generate precipitation with silver ion, brings larger interference for the observation of reacting phenomenon.For method (3), when the amount of taking reach clinical minimum pharmaceutical dosage 1/10th the time, reacting phenomenon does not almost observe.Point out the sensitivity of this method lower.
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 costs an arm and a leg 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 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 short-time test kit.
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.
The rapid assay methods of doping aminopyrine in medicine of the present invention, the health food, form by following steps successively:
(1) the aminopyrine composition in extraction medicine and the health food obtains extract;
(2) with solvent extraction described extract, separating and extracting liquid, concentrate residue;
(3) described residue is dissolved once more, get need testing solution;
(4) in described need testing solution, add detection agent.
Wherein, the aminopyrine composition in water extraction medicine and the health food in the step (1); Use the ethyl acetate extraction extract in the step (2); Residue water dissolving in the step (3); Detection agent in the step (4) is ferric trichloride test solution and iron potassuim cyanide test liquid.
The aminopyrine building stone has extremely strong reductibility, ferric ion can be reduced to ferrous ion, and the ferrous ion that is generated can generate mazarine complex compound Hexacyanoferrate ferropotassium with the Hexacyanoferrate root complexing in the potassium ferricyanide.
At most of medicines or health food in the market, recommend sampling amount as follows:
| Formulation | Sampling amount |
| Capsule | 1～2 intragranular is tolerant |
| Tablet | 2 |
| 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, to separate so that 5～10ml is water-soluble, 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 vibration dissolving, gained solution is 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 is need testing solution.
Wherein, the purpose that solid sample is dissolved in water is that the water soluble ingredient in aminopyrine and the sample is extracted from matrix.The purpose of ethyl acetate extraction is the pigment of removing on the basis that keeps aminopyrine in the Chinese medicine preparation, observes the interference that brings to experimental result to remove the sample intrinsic colour.Acetic acid ethyl acetate extract concentrated and be in order to remove extractant ethyl acetate, to make aminopyrine from ethyl acetate, disperse to come out, and make water-soluble developer and need testing solution miscible, be convenient to develop the color with the purpose that water redissolves.
In the gained need testing solution, drip each 2～5 of ferric trichloride test solution and iron potassuim cyanide test liquids successively, observe chromogenic reaction.
Drip the ferric trichloride test solution and be for sufficient ferric ion is provided, thereby generate ferrous ion,, improve the sensitivity of reaction for next step complexing chromogenic reaction provides sufficient material base with the aminopyrine reaction of strong reducing property.
Fe
3+e→Fe
2+
The purpose that drips the potassium ferricyanide provides the Hexacyanoferrate radical ion, generates the mazarine complex compound with the ferrous ion complexing.
Fe
2++[Fe(CN)
6]
3-→Fe[Fe(CN)
6]
-
In result's judgement,, can generate the mazarine complex compound immediately if contain aminopyrine in the testing sample.Negative control then becomes green suspension.
According to the present invention, can make aminopyrine reagent for quickly examining box.
According to the present invention, can be applied in the examination check that whether medicine, health food mix aminopyrine.
Compare with prior art, the present invention has following advantage:
Fast, easy.The whole operation process comprise flooding 3 minutes, filtered 2 minutes, ethyl acetate extraction 3 minutes, extract dries up 2 minutes, residue redissolve 2 minutes, add developer then, the whole operation process was finished at 12 minutes.Simple and efficient than liquid chromatography, LC-MS method, and need not reference substance.
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.
Be quick on the draw rapidly.The clinical using dosage of aminopyrine is 0.1～0.15g, and the minimum detectability of the present invention's material aminopyrine to be checked has reached 1/10th of clinical minimum effective dose, and after adding developer chromogenic reaction takes place immediately.Therefore check that with this method whether adding aminopyrine in medicine, the health food has enough sensitivity.
Applied widely.This method can be used for solid pharmaceutical preparation and liquid preparation, and no matter is that Chinese medicine preparation or health food all can use this method.
Method provided by the invention is improved the method for aminopyrine ministerial standard, the rare iron potassuim cyanide test liquid in the former method is changed into add ferric trichloride test solution and iron potassuim cyanide test liquid respectively, has improved the sensitivity of reaction.
The quick screening method that adds aminopyrine in medicine provided by the invention and the health food without authorization can help timely rapid screening to go out illegal interpolation medicine, be convenient to mobile big execute-in-place, can effectively prevent from illegally to add 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.
In following examples, the compound method of various test solutions is as follows:
Ferric trichloride test solution: get ferric trichloride 9g, be dissolved in water into 100ml, promptly.
Iron potassuim cyanide test liquid: get potassium ferricyanide 1g, add water 10ml and make dissolving, promptly.
Embodiment 1
Gastrodia capsule (Jilin Jichun Pharmaceutical Co., Ltd., capsule indicate 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, in residue, add 5ml water with hair dryer, jolting makes dissolving, gets need testing solution.Drip 2 of ferric trichloride test solutions in this solution, 2 of iron potassuim cyanide test liquids generate the mazarine complex compound immediately.
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 this solution, drip 2 of ferric trichloride test solutions, 2 of iron potassuim cyanide test liquids, solution becomes green suspension.
Embodiment 2
FENGSHI GUANJIEYAN PIAN (yellow dressing indicates 4 slices/time of doses for Shenyang Dong Xin pharmaceutcal corporation, Ltd, tablet)
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, in residue, add 5ml water with hair dryer, jolting makes dissolving, gets need testing solution.Drip 2 of ferric trichloride test solutions in this solution, 2 of iron potassuim cyanide test liquids generate the mazarine complex compound immediately.
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 this solution, drip 2 of ferric trichloride test solutions, 2 of iron potassuim cyanide test liquids, solution becomes green suspension.
Embodiment 3
FUFANG FENGSHINING PIAN (Guangdong LuoFoshan Medicine Co., Ltd, tablet indicate 2 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 5ml water in residue, jolting makes dissolving, gets need testing solution.Drip 2 of ferric trichloride test solutions in this solution, 2 of iron potassuim cyanide test liquids generate the mazarine complex compound immediately.
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 this solution, drip 2 of ferric trichloride test solutions, 2 of iron potassuim cyanide test liquids, solution becomes green suspension.
Embodiment 4
Bone spur pain-eliminating capsule (Zhongshan City Zhongzhi Pharmaceutical Co., Ltd, capsule indicate 4/time of doses)
It is tolerant to get 2 intragranulars, 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, in residue, add 5ml water with hair dryer, jolting makes dissolving, gets need testing solution.Drip 2 of ferric trichloride test solutions in this solution, 2 of iron potassuim cyanide test liquids generate the mazarine complex compound immediately.
The negative control specimen test: it is tolerant to get same sample 2 intragranulars, places the 10ml sample hose, is dissolved in water, and after this operates the samely, filters, extraction the preparation need testing solution.In this solution, drip 2 of ferric trichloride test solutions, 2 of iron potassuim cyanide test liquids, solution becomes green suspension.
Embodiment 5
WANTONG JINGU PIAN (Tonghua Wan Tong incorporated company, tablet indicate 2 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 5ml water in residue, jolting makes dissolving, gets need testing solution.Drip 2 of ferric trichloride test solutions in this solution, 2 of iron potassuim cyanide test liquids generate the mazarine complex compound immediately.
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 this solution, drip 2 of ferric trichloride test solutions, 2 of iron potassuim cyanide test liquids, solution becomes green suspension.
Embodiment 6
Musk rheumatic capsule (Jiangxi Yaodu Renhe Pharmaceutical Co., Ltd, capsule indicate 4/time of doses)
It is tolerant to get 2 intragranulars, 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, in residue, add 5ml water with hair dryer, jolting makes dissolving, gets need testing solution.Drip 2 of ferric trichloride test solutions in this solution, 2 of iron potassuim cyanide test liquids generate the mazarine complex compound immediately.
The negative control specimen test: it is tolerant to get same sample 2 intragranulars, places the 10ml sample hose, is dissolved in water, and after this operates the samely, filters, extraction the preparation need testing solution.In this solution, drip 2 of ferric trichloride test solutions, 2 of iron potassuim cyanide test liquids, solution becomes green suspension.
Embodiment 7
Yaotongning capsules (Chengde JingFuKang pharmacy Group Co.,Ltd, capsule indicate 4/time of doses)
It is tolerant to get 2 intragranulars, 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, in residue, add 5ml water with hair dryer, jolting makes dissolving, gets need testing solution.Drip 2 of ferric trichloride test solutions in this solution, 2 of iron potassuim cyanide test liquids generate the mazarine complex compound immediately.
The negative control specimen test: it is tolerant to get same sample 2 intragranulars, places the 10ml sample hose, is dissolved in water, and after this operates the samely, filters, extraction the preparation need testing solution.In this solution, drip 2 of ferric trichloride test solutions, 2 of iron potassuim cyanide test liquids, solution becomes green suspension.
Embodiment 8
FENGSHI GUANJIEYAN PIAN (Jilin biochemical Pharma Inc. over strait, tablet indicate 4 slices/time of doses)
2 of sample thiefs grind in mortar, add aminopyrine 0.01g and (are equivalent to 1/10th of clinical minimum effective dose,), 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, in residue, add 5ml water with hair dryer, jolting makes dissolving, gets need testing solution.Drip 2 of ferric trichloride test solutions in this solution, 2 of iron potassuim cyanide test liquids generate the mazarine complex compound immediately.
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 this solution, drip 2 of ferric trichloride test solutions, 2 of iron potassuim cyanide test liquids, solution becomes green suspension.
Claims (4)
1. the rapid assay methods of doping aminopyrine in a medicine, the health food, form by following steps successively:
(1) water extracts the aminopyrine composition in medicine and the health food, obtains extract;
(2) with solvent extraction described extract, separating and extracting liquid, concentrate residue, described extraction solvent is an ethyl acetate;
(3) with the water dissolving once more of described residue, get need testing solution;
(4) add detection agent in described need testing solution, described detection agent is ferric trichloride test solution and iron potassuim cyanide test liquid.
2. assay method as claimed in claim 1, form by following steps successively:
(1) get it filled product or health food are dissolved in water, and jolting makes dispersion, leave standstill a moment, remove by filter insolubles, collect filtrate;
(2) with ethyl acetate extraction described filtrate, leave standstill a moment after the jolting, the separating ethyl acetate extract, concentrate residue;
(3) with described residue water dissolving, get need testing solution;
(4) in described need testing solution, add detection agent ferric trichloride test solution and iron potassuim cyanide test liquid successively.
3. the application of the described assay method of claim 1 in preparation aminopyrine reagent for quickly examining box.
4. whether the described assay method of claim 1 mixes application in the examination check of aminopyrine at medicine and health food.
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Address after: 518000 high tech Zone, No. 28, central high tech Zone, Nanshan, Guangdong, Shenzhen, China, No. two Patentee after: Shenzhen Institute for drug control (Shenzhen medical instrument testing center) Address before: 518057 Shenzhen City, Nanshan District Province, Central District, high tech, No. two, No. 28, No. Patentee before: Shenzhen Institute For Drug Control |