CN101498671A - Fast screening method for metronidazole in cosmetic - Google Patents
Fast screening method for metronidazole in cosmetic Download PDFInfo
- Publication number
- CN101498671A CN101498671A CNA2009100378599A CN200910037859A CN101498671A CN 101498671 A CN101498671 A CN 101498671A CN A2009100378599 A CNA2009100378599 A CN A2009100378599A CN 200910037859 A CN200910037859 A CN 200910037859A CN 101498671 A CN101498671 A CN 101498671A
- Authority
- CN
- China
- Prior art keywords
- cosmetic
- metronidazole
- cosmetics
- screening method
- quick screening
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Cosmetics (AREA)
Abstract
The invention discloses a method for rapidly selecting and detecting the cosmetic containing metronidazole, which comprises the steps of adding alkali liquor into the cosmetic to be detected, heating the alkali liquor and the cosmetic at a temperature of 50-80 DEG C in a water bath heating way so that the alkali liquor and the cosmetic conduct the color development reaction, judging whether the metronidazole is added in the cosmetic according to the color development reaction result. In the case of cream cosmetic, adding acid liquor into the cream cosmetic before adding the alkali liquor, heating the acid liquor and the cream cosmetic until the cream cosmetic is melted down, and adding the alkali liquor into the solution of the acid liquor and the cream cosmetic. The method does not need any large-sized instrument and is easy to operate; the cosmetic sample containing the metronidazole can be selected for the subsequent precision chromatogram detection according to the color development reaction judgment; the method is helpful for supervision departments to select large-batch cosmetic samples, simplifies the detection procedures, reduces the detection cost and can be used for high-flowability cosmetic sample detection.
Description
Technical field
The present invention relates to the detection method of metronidazole, be specifically related to the quick screening method of metronidazole in a kind of cosmetics.
Background technology
(English name is Metronidazole, and MNZ), its chemical name is: 2-methyl-5-nitro imidazoles-1-ethanol, molecular formula are C to metronidazole
6H
9N
3O
3, commodity are called metronidazole, flagyl, MET, Metronidazole.Metronidazole (MNZ) is a nitroimidazoles medicine, it is the wide spectrum anthelmintic, can kill Amoeba, also effective to anaerobic bacillus(cillus anaerobicus) and coccus, also being used for operation infects, selected to treating the essential drugs of anaerobic infection by The World Health Organization (WHO), in addition, metronidazole has good killing effect to itch mite, can treat scabies, kill the corynebacteria of causing inflammation property acne, so effective acne, be widely used in the cosmetics, especially some eliminations " small pox " and " acne " etc. in the cosmetics.
Yet, though metronidazole has antibiotic and effect anti-inflammatory, to eliminating " small pox ", " acne " etc. certain effect is arranged, but use Diazolidinyl Urea for a long time, cause contact dermatitis, show as erythema, oedema, erosion, furfur, itch, scorching hot etc., more seriously cause antimicrobial resistance, cause healthy hidden danger.
The chemical index analytical approach of China's " cosmetics health standard version in 2002 " formulation at present has only 22 standards only to relate to 57, much add the material of cosmetics to owing to lack composition, toxicity, the effect detection method of system and estimate requirement, make that the hygienic quality of present cosmetics only is " qualified " of act.std regulation, the true hygienic quality that can not effectively reflect cosmetics, particularly the illegal interpolation of cosmetics Chinese traditional medicine is just receiving increasing concern.Antibiotics materials such as China's " cosmetics health standard ", European Union's cosmetics rules (CoucilDirective76/768/EEC) regulation metronidazole, chloromycetin, lincomycin are forbidden using in cosmetics.
Institute of Environmental Health of Beijing Disease Prevention and Control Centre in Beijing, Jiangsu, Jiangxi area 122 anti-acnes of selling remove mite class cosmetics and detect, 122 samples detect 14 of metronidazoles, exceeding standard rate 11.5%, maximum addition reaches 3.9%, wherein detect 5 of metronidazoles in 28 in Guangdong, exceeding standard rate reaches 17.9%.
China's " cosmetics health standard " wherein proposes to have measured the high performance liquid chromatography of anti-acne except that hydrochloric acid minocycline, Oxytetracycline Dihydrate, quadracycline, aureomycin hydrochloride, Doxycycline Hyclate, 6 kinds of microbiotic of chloromycetin and metronidazole in the mite class cosmetics first in formal execution the on August 1st, 2007.
High performance liquid chromatography is the modern analysis method of using always, it has advantages such as chromatographic resolution efficient height, sensitivity height, under identical chromatographic condition, the need testing solution of metronidazole reference substance solution and sample extraction gained is sample introduction respectively, can judge according to chromatographic retention whether testing sample contains metronidazole.
Present detection at metronidazole in the cosmetics, except liquid phase chromatography commonly used, outside liquid chromatography mass coupling method and the thin layer chromatography, also has plenty of the indirect competitive ELISA of employing method, on the ELISA Plate capillary strip, wrap in advance by coupled antigen, in the sample on residual metronidazole and the capillary strip coupled antigen of pre-bag quilt compete anti-metronidazole antibody, after adding ELIAS secondary antibody, develop the color with tmb substrate, the sample light absorption value becomes negative correlation with the content of its residue metronidazole, multiply by its corresponding extension rate more again with typical curve, can draw the content of metronidazole in the sample.
Though above-mentioned chromatography and ELISA method can both detect the metronidazole in cosmetics etc. exactly, yet these two kinds of methods all exist complicated operation, sample preparation time length, can't accomplish rapid screening for detected sample in enormous quantities, problems such as the testing amount is big, chromatography also exists instrument to cost an arm and a leg in addition, and chromatographic column vulnerable to pollution, analysis cost are high and be not suitable for doing mobile big problems such as scene detection.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of large-scale detecting instrument that need not is provided, detection method is easy fast, detect the low and testing result of cost accurately at the quick screening method that whether contains metronidazole in the cosmetics, this method helps supervision department's on-site quick screening, especially at the rapid screening of batch samples.
Above-mentioned purpose of the present invention is achieved by following scheme:
Aromatic nitro compound is easy to be reduced, after metronidazole is reduced by alkali lye, can generate mauve azobenzene and colourless hydrazobenzene, therefore can utilize alkali lye to develop the color and identify whether contain metronidazole in the testing sample, if alkali lye colour developing result is pink or aubergine, illustrate then and contain metronidazole in the testing sample that metronidazole change color occurred after being reduced by alkali lye, if the result is not for there being change color in the alkali lye colour developing, then illustrating does not have metronidazole in the testing sample.
The quick screening method of metronidazole in a kind of cosmetics of the present invention, just be based on above-mentioned principle, employing adds alkali lye in cosmetics to be measured, chromogenic reaction is carried out in the water-bath heating then, if solution colour becomes pink or aubergine, then contain metronidazole in these cosmetics to be measured of explanation,, then do not contain metronidazole in these cosmetics to be measured of explanation if solution does not have change color.
Cosmetics generally are divided into solution class and ointments:
(1) when cosmetics to be measured is solution, because the cosmetics of solution class do not contain the insoluble impurity of solid, so solution class cosmetics can directly add alkali lye, chromogenic reaction is carried out in the water-bath heating, jolting and constantly observation a little therebetween, become aubergine or pink as the chromogenic reaction result for solution becomes, then can be judged to and suspect the positive, otherwise be judged to feminine gender;
(2) when cosmetics to be measured are ointment, because contain a lot of insoluble impurity and additive component complexity in the ointments cosmetics, so need in the ointments cosmetics, to add acid solution earlier, heating then, treat that ointment dissolves after, filter, get filtrate and add alkali lye, chromogenic reaction is carried out in the water-bath heating, therebetween jolting and constantly observation a little, as the result that develops the color becomes aubergine for solution or pink is judged to the suspection positive, otherwise be judged to feminine gender; Heating after the adding acid solution, its objective is ointment is dissolved, thereby metronidazole is discharged, because metronidazole dissolves in acid, so adding the heating of acid back, employing here dissolves, also can only keep solution, thereby reach the purpose that height ratio extracts metronidazole in the ointments cosmetics so that a part is insoluble to acid or insoluble material is got rid of; Add the heating after the acid,, can select 50 ℃～80 ℃ heating-up temperature during practical operation as long as its temperature makes ointment dissolve.
In the above-mentioned quick screening method, the acid solution that adds in the ointments cosmetics can be selected any common acid, as acetic acid, hydrochloric acid etc., and for the consideration to environmental protection, preferred acetic acid, because acetic acid not only environmental protection but also corrosivity is good, the concentration of acetic acid can be selected≤1mol/L, as the 0.3mol/L acetum.
In the quick screening method of the present invention, can select this area alkali lye commonly used as the alkali lye that chromogenic reagent is used, as NaOH, potassium hydroxide etc., because the present invention has added acid solution in front, when carrying out chromogenic reaction here, the alkali lye of part may carry out neutralization reaction with the acid solution of front, therefore in order to guarantee the higher sensitivity of chromogenic reaction, here the NaOH of the preferred high concentration of alkali lye, 20 quality %～40 quality % sodium hydroxide solutions are more preferably 30 quality % sodium hydroxide solutions.
In the quick screening method of the present invention, after alkali lye adds, need to adopt the water-bath heating to carry out color reaction, here chromogenic reaction bath temperature control is important, because it is too fast to fade after the too high then chromogenic reaction of bath temperature, may influence observation, if bath temperature is low excessively, then the chromogenic reaction time can be long, influences the rapidity of examination, the color of chromogenic reaction also can be lighter simultaneously, influence is observed, and therefore the bath temperature of chromogenic reaction is controlled between 50 ℃～80 ℃ here, thereby can guarantee quick colour-developing, simultaneously also can guarantee the developing time long enough, the bath temperature of preferred chromogenic reaction is 60 ℃～70 ℃.
Whether illegal quick screening method of the present invention mainly be to have added the primary dcreening operation that metronidazole carries out in the cosmetics, so long as after utilizing the inventive method to develop the color, pink or mauve cosmetics appear, then can tentatively judge in these cosmetics and may be added with metronidazole, if chromogenic reaction is a no change, then illustrate in these cosmetics and do not add metronidazole certainly, the cosmetics that may be added with metronidazole then carry out meticulousr detections such as mass spectrum, chromatogram again.Though be primary dcreening operation, but method of the present invention is easy and simple to handle, and the used time is short, can finish inspection in general 3 minutes, and visual result can be chosen a spot of suspicious specimen by seeing color relation from large batch of cosmetics to be measured, simplified the step that detects greatly, and only need carry out meticulous detections such as mass spectrum, chromatogram to a small amount of suspicious sample, make that also detecting cost reduces greatly, the needs that are suitable for supervision department's quick check are to the operational paradigm that improves supervision department, hit the lawless person fast the important social benefit is arranged.
Compared with prior art, the present invention has following beneficial effect:
1. quick screening method of the present invention adopts the easy steps that adds acid, adds alkali and water-bath heating, both can detect and whether contain metronidazole in the testing sample, and method is easy, and left-hand seat does not need the testing staff is trained especially easily;
2. its raw material of quick screening method of the present invention only need be used acid, alkali and water-bath equipment etc., and it is with low cost to detect materials, only 2 yuan of the every batch of expenses, and do not need large-sized analytic instrument, be suitable for doing mobile big detection;
3. quick screening method of the present invention develops the color by alkali lye, can finish in 3 minutes whether adding the inspection of metronidazole in the cosmetics, check result is intuitive and reliable, through the liquid chromatography mass coupling method comparatively validate very high with generally acknowledged accuracy, accuracy is higher than 95% as a result, and false negative rate is 0, has reached easy inexpensive purpose accurately fast, meet the needs of supervising on-the-spot quick check, to the operational paradigm that improves supervision department, hit the lawless person fast the important social benefit is arranged.
Embodiment
The present invention will be further described below in conjunction with specific embodiment, but specific embodiment is not done any qualification to the present invention.
Embodiment 1 Qu Man mildy wash
Present embodiment De Qu Man mildy wash is the ointments cosmetics, at first the preparing experiment utensil:
Beaker, glass rod, dropper, test tube, reagent bottle and electric cup.
The about 1g of Qu Qu Man mildy wash, place small beaker, add 0.3mol/L acetum solution 2ml, heated and stirred is boiled moltenly in 60 ℃ of water-baths, pours in the test tube boiling the liquid that obtains after molten, add 5 of 30 quality % sodium hydroxide solutions, place electric cup, heating is 2 minutes in 50 ℃ of water-baths, therebetween jolting and constantly observation a little, color observation finds that solution colour becomes pink, illustrates in Gai Qu Man mildy wash to be added with metronidazole.
Embodiment 2 anti-acnes benefit skin water
The anti-acne benefit skin water of present embodiment is solution class cosmetics, at first preparing experiment utensil:
Beaker, glass rod, dropper, test tube, reagent bottle and electric cup.
Get anti-acne benefit skin water 2ml, place test tube, add 8 of 30 quality % sodium hydroxide solutions, 60 ℃ of water-baths were heated 2 minutes, jolting and constantly observation a little therebetween, color observation finds that solution colour becomes aubergine, illustrates in this anti-acne benefit skin water to be added with metronidazole.
Embodiment 3 potent dark sore repair creams
The potent dark sore repair cream of present embodiment is the ointments cosmetics, at first the preparing experiment utensil:
Beaker, glass rod, dropper, test tube, reagent bottle and electric cup.
Get the about 1.5g of potent dark sore repair cream, place small beaker, add 1mol/L acetum solution 2ml, heated and stirred is boiled moltenly in 50 ℃ of water-baths, pours in the test tube boiling the liquid that obtains after molten, add 6 of 40 quality % sodium hydroxide solutions, place electric cup, heating is 2 minutes in 70 ℃ of water-baths, therebetween jolting and constantly observation a little, color observation finds that solution colour does not change, and illustrates in this potent dark sore repair cream and does not add metronidazole.
The flat scar Essence of embodiment 4 plant anti-acnes
The flat scar Essence of the plant anti-acne of present embodiment is solution class cosmetics, at first preparing experiment utensil:
Beaker, glass rod, dropper, test tube, reagent bottle and electric cup.
Get the flat scar Essence of plant anti-acne 2ml, place test tube, add 7 of 35 quality % sodium hydroxide solutions, 80 ℃ of water-baths were heated 2 minutes, jolting and constantly observation a little therebetween, color observation find that solution colour does not change, and illustrates in the flat scar Essence of this plant anti-acne and does not add metronidazole.
Claims (10)
1, the quick screening method of metronidazole in a kind of cosmetics is characterized in that this method is to add alkali lye in cosmetics to be measured, and chromogenic reaction is carried out in 50 ℃～80 ℃ water-bath heating, judges whether be added with metronidazole in the cosmetics to be measured according to the chromogenic reaction result.
2, according to the described quick screening method of claim 1, when it is characterized in that described cosmetics to be measured are ointment, before adding alkali lye, need in cosmetics to be measured, to add acid solution earlier, after heating is dissolved, get solution and add alkali lye.
3,, it is characterized in that the temperature of described water-bath heating chromogenic reaction is 60 ℃～70 ℃ according to the described quick screening method of claim 1.
4,, it is characterized in that described heating melting temperature is 50 ℃～80 ℃ according to the described quick screening method of claim 2.
5,, it is characterized in that described alkali lye is NaOH or potassium hydroxide according to the described quick screening method of claim 1.
6,, it is characterized in that described alkali lye is 20 quality %～40 quality % sodium hydroxide solutions according to the described quick screening method of claim 5.
7,, it is characterized in that described alkali lye is 30 quality % sodium hydroxide solutions according to the described quick screening method of claim 6.
8,, it is characterized in that described acid solution is acetic acid or hydrochloric acid according to the described quick screening method of claim 2.
9, described according to Claim 8 quick screening method is characterized in that described acid solution is the acetic acid of concentration smaller or equal to 1mol/L.
10,, it is characterized in that described acid solution is the 0.3mol/L acetum according to the described quick screening method of claim 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100378599A CN101498671B (en) | 2009-03-12 | 2009-03-12 | Fast screening method for metronidazole in cosmetic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100378599A CN101498671B (en) | 2009-03-12 | 2009-03-12 | Fast screening method for metronidazole in cosmetic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101498671A true CN101498671A (en) | 2009-08-05 |
| CN101498671B CN101498671B (en) | 2011-01-19 |
Family
ID=40945842
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100378599A Active CN101498671B (en) | 2009-03-12 | 2009-03-12 | Fast screening method for metronidazole in cosmetic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101498671B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018239A (en) * | 2012-12-13 | 2013-04-03 | 广东药学院 | Quick screening method for phenol estrogen in cosmetics |
| CN104165888A (en) * | 2014-08-13 | 2014-11-26 | 国家电网公司 | Method for determining content of sodium chlorate in industrial alkali liquor |
| CN104198478A (en) * | 2014-08-16 | 2014-12-10 | 中山鼎晟生物科技有限公司 | Rapid detection kit for metronidazole in cosmetics and detection method |
| CN104297239A (en) * | 2014-10-18 | 2015-01-21 | 中山鼎晟生物科技有限公司 | Kit applied to rapid detection of metronidazole in cosmetic and detection method |
| CN106770222A (en) * | 2016-11-23 | 2017-05-31 | 百奥森（江苏）食品安全科技有限公司 | The detection kit of metronidazole in a kind of food |
| CN107607529A (en) * | 2017-08-18 | 2018-01-19 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | A kind of quick screening method for being used for formaldehyde in perfume |
| CN108303307A (en) * | 2017-12-25 | 2018-07-20 | 陕西佰傲再生医学有限公司 | A method of quantitatively detecting hyaluronic acid contents in skin preparation |
| CN115267011A (en) * | 2022-09-06 | 2022-11-01 | 重庆市食品药品检验检测研究院 | Liquid chromatography-mass spectrometry chromatography method for qualitative detection of illegally added drugs in oil control cosmetics |
-
2009
- 2009-03-12 CN CN2009100378599A patent/CN101498671B/en active Active
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018239A (en) * | 2012-12-13 | 2013-04-03 | 广东药学院 | Quick screening method for phenol estrogen in cosmetics |
| CN104165888A (en) * | 2014-08-13 | 2014-11-26 | 国家电网公司 | Method for determining content of sodium chlorate in industrial alkali liquor |
| CN104198478A (en) * | 2014-08-16 | 2014-12-10 | 中山鼎晟生物科技有限公司 | Rapid detection kit for metronidazole in cosmetics and detection method |
| CN104297239A (en) * | 2014-10-18 | 2015-01-21 | 中山鼎晟生物科技有限公司 | Kit applied to rapid detection of metronidazole in cosmetic and detection method |
| CN106770222A (en) * | 2016-11-23 | 2017-05-31 | 百奥森（江苏）食品安全科技有限公司 | The detection kit of metronidazole in a kind of food |
| CN107607529A (en) * | 2017-08-18 | 2018-01-19 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | A kind of quick screening method for being used for formaldehyde in perfume |
| CN107607529B (en) * | 2017-08-18 | 2019-12-06 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | Rapid screening method for formaldehyde in perfume |
| CN108303307A (en) * | 2017-12-25 | 2018-07-20 | 陕西佰傲再生医学有限公司 | A method of quantitatively detecting hyaluronic acid contents in skin preparation |
| CN115267011A (en) * | 2022-09-06 | 2022-11-01 | 重庆市食品药品检验检测研究院 | Liquid chromatography-mass spectrometry chromatography method for qualitative detection of illegally added drugs in oil control cosmetics |
| CN115267011B (en) * | 2022-09-06 | 2024-05-07 | 重庆市食品药品检验检测研究院 | Liquid chromatography-mass spectrometry chromatography method for qualitative detection of illegally added drugs in oil-control cosmetics |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101498671B (en) | 2011-01-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101498671B (en) | Fast screening method for metronidazole in cosmetic | |
| Wang et al. | Detection of honey adulteration with starch syrup by high performance liquid chromatography | |
| Leng et al. | A rapid and sensitive method for determination of trace amounts of glucose by anthrone-sulfuric acid method | |
| US20200158696A1 (en) | Detection of free mannose and glucose in serum using high performance liquid chromatography | |
| CN104897907B (en) | A kind of test kit detecting glycolated hemoglobin and detection method thereof | |
| CN107449850B (en) | Method for determining alkylphenol in environmental water sample by combining fast synergistic cloud point extraction and high performance liquid chromatography | |
| Liu et al. | A smart reaction-based fluorescence probe for ratio detection of hydrazine and its application in living cells | |
| Jiang et al. | Design of a naphthalimide-based probe for acrolein detection in foods and cells | |
| CN105802608A (en) | Preparation method of fluorescent probe and application of fluorescent probe in aluminum ion detection | |
| CN101504372B (en) | Fast detection method and detection reagent kit for metronidazole, and its use in detection of cosmetic and disinfector added with metronidazole | |
| CN114524453B (en) | ZIF-8 derived ZnO/g-C 3 N 4 Preparation method of (C) and application of C in terramycin sensor | |
| CN107255686A (en) | The analysis method of many residues of veterinary drug in a kind of measure cultivation water | |
| CN104515768B (en) | Tumor specific growth factor detection kit | |
| Chen et al. | Simultaneous quantification of twelve active components in Yiqing granule by ultra‐performance liquid chromatography: application to quality control study | |
| Zhou et al. | Molecularly imprinted ratiometric fluorescence detection of tetracycline based on its fluorescence enhancement effect caused by tungsten trioxide quantum dots | |
| CN108760920A (en) | A method of cyazofamid and its metabolite residue amount are measured based on HPLC-MSMS methods | |
| CN108982733A (en) | A method of analysis polysaccharide composed structure | |
| CN100494995C (en) | Leather Cr6+ automatic analysis method | |
| CN102125598A (en) | Quality control method of watermelon frost | |
| CN106841452A (en) | A kind of method that HPLC combinations UPLC MS detections PQQ is acted on lactic acid | |
| Shuang-Min et al. | Development of enzyme-linked immunosorbent assay and colloidal gold-based immunochromatographic assay for the rapid detection of gentamicin in chicken muscle and milk | |
| CN103901121B (en) | Gas chromatograph-mass spectrometer analyzes the method for chloracetic acid in drinking water | |
| CN113009007B (en) | Method for detecting content of root-resisting agent in root-puncture-resistant material | |
| CN101226139A (en) | Method for chemistry testing potassium bromate in flour, amendment or food | |
| CN110873713B (en) | Method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosive |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |