Background technology
The current raising along with domestic level, the demand of women to beauty treatment is increasing, various whitening product also emerges in an endless stream, add in cosmetics various whitening function composition also right and wrong usually see, quinhydrones is one of them, although treatment pigment increase chemical composition a lot, but quinhydrones is cheap, be easy to get, all there is the feature of sale in each chemical reagent shop, makes illegal situation of adding in cosmetics very common.In sampling observation to networking cosmetic of China 2014, quinhydrones, phenol or betamethasone chemical composition in most of whitening, Freckle removing cosmetics, are all detected.
Quinhydrones has another name called p-dihydroxy-benzene, it is the compound that two contraposition hydrogen of benzene are optionally substituted by a hydroxyl group formation, white crystals, p-dihydroxy-benzene is poisonous, and adult wrongly takes 1 gram, the symptoms such as headache, dizziness, tinnitus, pale complexion can be there is, further, because quinhydrones toxicity is very large, strong corrosive attack is had to skin, mucous membrane, central nervous system can be suppressed or damage liver, skin function, so it is classified as the banned substance in whitening, Freckle removing cosmetics by our country all the time.
At present for the detection adding quinhydrones illegal in cosmetics, mainly adopt the method for high performance liquid chromatography, liquid chromatography mass coupling.High performance liquid chromatography and LC-MS chromatographic process are state-of-the-art modern analysis means, it has, and separation efficiency is high, sensitivity advantages of higher, adopt standard control method, point-devicely can detect the content of quinhydrones in sample, but these need the checkout equipment of specialty, operating process is more complicated all, experimental period is long, experimental cost is high, are very large tests for the patience of Site Detection personnel, be therefore necessary to research and develop a kind of kit that can detect fast the carrying out of quinhydrones in cosmetics and detection method thereof.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide one very simple, fast, analysis cost is very low, strong, highly sensitive and be applicable to the kit of field quick detection to the specificity of quinhydrones.
The technical solution used in the present invention is as follows:
A quick detection kit for quinhydrones in cosmetics utilizes following several character of quinhydrones to realize detecting fast it.
1, quinhydrones and alkali ion form quinhydrones salt, and quinhydrones salt character is very unstable, are very fastly oxidized to 1,4-benzoquinone, and 1,4-benzoquinone and quinhydrones generate the molecular complex quinhydrone of quinhydrones-1,4-benzoquinone.
2, this reaction is very sensitive, even if also can very fast response in the matrix of cosmetics, cosmetic base affects its reaction hardly, matrix in addition in cosmetics does not almost have and alkali ion generation metachromasia, therefore, quinhydrones need not extract and can complete by this reaction from cosmetics, and testing process is simple and quick.
3, quinhydrone is blackish green, and color is very dark, and be very easy to show in the background color of cosmetics, therefore, the detectability reached is very low, can reach detect a small amount of object of adding fast completely.
Utilize the above-mentioned character of quinhydrones, quick detection kit provided by the invention comprises following component:
Described kit comprises solvent reagent and alkaline reagent, be equipped with the experiment consumptive materials such as reaction bulb, suction pipe, sample spoon, be assembled into kit, the reagent proportioning of taking in a certain amount of water and kit according to testing sample situation is only needed to observe colour developing during use, can judge whether add quinhydrones composition in testing sample, wherein said solvent reagent is one or more of the organic solvent such as purified water or ethanol, methyl alcohol, ether, methylene chloride.
Described alkaline reagent is basic ion solution or solid base, and described basic ion solution is the one of NaOH, potassium hydroxide, sodium hydride and aqueous solution thereof.
The concentration of described alkali ion solution is 0.5 ~ 5%, is wherein preferably 1.5 ~ 3.0%, because the alkali ion in the too high solution of concentration is easily by the chemical composition oxidation in cosmetics, disturbance reponse served by band, affects result and judges.
Another object of the present invention is to provide a kind of method for quick utilizing mentioned reagent box to detect quinhydrones chemical composition in cosmetics, and concrete steps are as follows:
1, get testing sample in tool reaction bulb, in testing sample, add appropriate solvent reagent dilutions, ensure that cosmetics have certain mobility;
2, drip appropriate alkaline solion or solid base in test sample to treating after dilution, shake up immediately, leave standstill under normal temperature and observe colour developing situation after 2-5 minute;
3, colour developing situation is observed: when reaction bulb occurs brown color to brownish black, then tentatively can judge that these cosmetics may with the addition of quinhydrones composition, if chromogenic reaction is unchanged, then illustrate in these cosmetics and do not add quinhydrones composition, and then the sample that may be added with quinhydrones carries out the meticulousr detection such as mass spectrum, liquid chromatography again.
In above-mentioned steps 1, described solvent reagent can be the one in purified water or ethanol, methyl alcohol, ether, methylene chloride, is wherein preferably purified water or distilled water.
In above-mentioned steps 1, the consumption of described solvent reagent is 0 ~ 10ml, and testing sample amount is 0.1 ~ 10g or 1 ~ 10ml, and the volume of described solvent reagent can 0.5 ~ 2 times of preferred institute's sample thief cosmetics amount, cosmetics dilution can be kept certain mobility like this, can Detection results be ensured again.
In above-mentioned steps 2, the alkali ion solution added or solid base are preferably alkali ion solution, and alkali ion Solution Dispersion is good, can be dispersed in very short time after adding, intensified response effect.
In above-mentioned steps 2, the addition of described solid base is 1mg ~ 1g.
The alkali ion solution added in above-mentioned steps 2 is preferably concentration 2.0 ~ 3.0% sodium hydroxide solution.
The volume adding alkali ion solution in above-mentioned steps 2 is preferably 50 ~ 1000 microlitres.
For the testing sample of some inherently liquid type, can directly add alkali ion solution, save the process of step 1.
Compared with prior art, the present invention has following beneficial effect:
Whether method for quick of the present invention mainly illegally adds the rapid screening carrying out quinhydrones chemical composition in brightening, dispelling spots, dispelling class cosmetics, have sensitivity very high, colour developing is obvious, the advantage that testing result accuracy rate is higher, accuracy rate can reach more than 99%, and false negative rate is zero, in addition, detection method of the present invention is simple to operate, convenient, do not need precision or large-scale instrument, detection time is short, detection can be completed in general 2 ~ 5 minutes, and testing result is intuitively by seeing that color change just can judge, be applicable to very much from gross sample, pick out a small amount of suspicious specimen, enormously simplify the step of detection, and only need sample suspicious on a small quantity to carry out mass spectrum again, the Precision measurement such as chromatogram, this also makes testing cost greatly reduce, be applicable to very much the needs of supervision department's rapid screening, to the operational paradigm improving supervision department, rapid strike lawless person has great social benefit.
Embodiment 3:
Getting the tender bloom 1ml of certain brand nti-freckle adds in reaction bulb, add ethanol 1ml, shake up to be measured, the sodium hydroxide solution that 250 lli are 2.5% is dripped in reaction bulb, shake up, observe after 2 ~ 3 minutes, reaction bulb content shows brown color, then can judge in the tender bloom of the present embodiment nti-freckle containing quinhydrones composition.
Implement 4:
Getting certain brand freckle removing and whitening element frost 1ml adds in reaction bulb, add purified water 1ml, shake up to be measured, the sodium hydroxide solution that 250 lli are 1.5% is dripped in reaction bulb, shake up, observe after 5 minutes, reaction bulb content does not have variable color, then can judge in this freckle removing and whitening element frost not containing quinhydrones composition.
Implement 5:
Get certain brand whitening and moisturizing moisturizing freckle-removing mask a slice, extruding liquid 1ml adds in reaction bulb, directly to dripping the sodium hydroxide solution that 250 lli are 3% in reaction bulb, shake up, observe after 3 minutes, reaction bulb content shows brownish black, then can judge in the present embodiment whitening and moisturizing moisturizing freckle-removing mask containing quinhydrones composition.
Implement 6:
Getting certain brand whitening day cream 10g adds in reaction bulb, adds purified water 1ml, shakes up to be measured, in reaction bulb, drip 1500 lli is 5% sodium hydroxide solution, shakes up, and observes after 5 minutes, reaction bulb content shows brownish black, then can judge in the tender bloom of the present embodiment nti-freckle containing quinhydrones composition.
Example 7 quinhydrones detects situation contrast
Whether adopt described in example 6 and detect reagent and detection method, carry out contrast testing result, detect 30 batch samples altogether with vapor-phase chromatography, first detect containing quinhydrones composition in judgement sample by this law, then compare by vapor-phase chromatography, result is as follows:
Sample number into spectrum |
This method |
Vapor-phase chromatography |
001 |
- |
- |
002 |
- |
- |
003 |
+ |
+ |
004 |
- |
- |
005 |
- |
- |
006 |
- |
- |
007 |
- |
- |
008 |
- |
- |
009 |
+ |
+ |
010 |
+ |
+ |
011 |
- |
- |
012 |
- |
- |
013 |
- |
- |
014 |
- |
- |
015 |
- |
- |
016 |
- |
- |
017 |
- |
- |
018 |
- |
- |
019 |
+ |
+ |
020 |
- |
- |
021 |
- |
- |
022 |
+ |
+ |
023 |
- |
- |
024 |
- |
- |
025 |
- |
- |
026 |
- |
- |
027 |
- |
- |
028 |
- |
- |
029 |
+ |
+ |
030 |
- |
- |
Note: "-" expression does not detect, "+" expression detects the positive.
As can be seen from the above table, the identical rate of two kinds of methods is 100%, visible chromogenic reaction result accuracy rate of the present invention is higher, false positive rate is 0, suspicious specimen can narrow down to very among a small circle by the present invention rapidly, finally only need to carry out the Precision measurement such as chromatogram, mass spectrum to these few suspicious specimen, the illegal sample containing quinhydrones can be detected.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.