CN103616378A - Method for detecting mercury in cosmetics - Google Patents

Method for detecting mercury in cosmetics Download PDF

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Publication number
CN103616378A
CN103616378A CN201310616292.7A CN201310616292A CN103616378A CN 103616378 A CN103616378 A CN 103616378A CN 201310616292 A CN201310616292 A CN 201310616292A CN 103616378 A CN103616378 A CN 103616378A
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China
Prior art keywords
cosmetics
mercury
reagent
aqueous solution
detection method
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Pending
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CN201310616292.7A
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Chinese (zh)
Inventor
郭狄
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ZHONGSHAN DINGSHENG BIOTECHNOLOGY Co Ltd
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ZHONGSHAN DINGSHENG BIOTECHNOLOGY Co Ltd
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Priority to CN201310616292.7A priority Critical patent/CN103616378A/en
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Abstract

The invention relates to a method for detecting mercury in cosmetics. The method comprises the following steps of: firstly, adding cosmetics to be detected in water, preparing into a cosmetics water solution; then preparing three parts of detection reagents; finally, separating the cosmetics water solutions prepared in the step (1) into three parts, respectively adding in the three parts of detection reagents, observing the change of the color of the water solution of the cosmetics; and if the three parts of cosmetic water solutions have characteristic chromogenic reactions, judging that the mercury is contained in a sample. Whether the mercury is contained in the cosmetics or not is judged by adopting a manner that three reagents simultaneously develop, thus the method is more accurate in comparison with a method of judging by only adopting two reagents, and the phenomenon of false negative usually occurring in a judging process caused by only adopting the two reagents is avoided.

Description

A kind of detection method of Mercury In Cosmetics
Technical field
The invention belongs to cosmetics safety detection field, be specifically related to the detection of Mercury In Cosmetics.
Background technology
Mercury is a kind of high toxicity heavy metal contaminants, also be unique heavy metal existing with liquid form at normal temperatures, mercury can carry out human body by alimentary canal, respiratory tract or skin and mucosa, and people's brain, kidney and body cell etc. are all caused to damage, also can cause that arthritis is even carcinogenic.Mercury is extensively present in the nature media such as atmosphere, water and soil, at present, along with industrial expansion, the burning of mineral fuel and solid waste, the use of mercury in chlorine industry and electrical equipment industry, the pollution of mercury is day by day serious at present, the mercury poisoning of continuous several times generation in recent years event, as the mercury poisoning event of the Mad Hatter's disease event of 20 middle of century Japan and U.S.'s generation.
Cosmetics are requisite skincare products during people live, and along with countries in the world economy and cultural development and progress, people are more and more to the demand of cosmetics, require also more and more higher.The negative ion of tyrosinase in the replaceable skin of the heavy metals such as mercury, this enzyme is lost activity, thereby melanin is gone down, make skin-whitening, make the skin gloss that becomes delicate, hair pore shrinkage, simultaneously also can anti-acne, nti-freckle, although these effects are temporary transient, but many illegal manufacturers, in order to make its product have quick whitening effect, to strive for more consumer, try to gain more interests, just the mercurous compound of illegal interpolation in the cosmetics of its production, and the mercury content adding is conventionally at 1-2.5%.Long term consumer is used the cosmetics of this content overproof, can produce larger injury to health.
Because the heavy metals exceeding standards such as Mercury In Cosmetics have larger impact to human body, < < cosmetics health standard > > (version in 2007) has done clear and definite restriction to the content of the heavy metals such as Mercury In Cosmetics, and wherein the content of mercury must not surpass 1 ppm.At present, in China < < cosmetics health standard > >, the method for inspection of regulation mercury comprises the instrument detection methods such as cold-vapour atomic absorption method and atom fluorescent luminosity method, although these method testing results are accurate, highly sensitive, but when these instruments detect, sample pre-treatments is loaded down with trivial details, in testing process, produce a large amount of harmful gases, environment has also been caused to larger pollution, and detecting instrument is valuable, field test is also subject to significant limitation, therefore, cannot meet supervision department's requirement that on-the-spot examination at random checks to cosmetics.
Summary of the invention
The object of the invention is to for deficiency of the prior art, a kind of detection method that can detect rapidly the content of Mercury In Cosmetics simple to operate is provided.
Technical scheme of the present invention is as follows:
A detection method for Mercury In Cosmetics, comprises the steps:
(1) cosmetics to be measured are added to the water, are mixed with cosmetics aqueous solution;
(2) alkyl polyoxyethylene ether, acid solution and the reagent that can produce sulphion are added in test tube, mix and be mixed with first part and detect reagent; Alkyl polyoxyethylene ether, acid solution and the reagent that can produce iodide ion are added to mix in test tube and be mixed with second part and detect reagent; Acid solution, stannous chloride are added in test tube and heated, then add copper sheet, remain micro-and boil, in heating process, add hot water, keep liquor capacity constant, be mixed with the 3rd part and detect reagent;
(3) the cosmetics aqueous solution making in step (1) is divided into three parts, adds respectively first part to detect reagent, second part of detection reagent and the 3rd part of detection reagent, observe the variation of the aqueous solution color of cosmetics; As feature chromogenic reaction all appears in three parts of cosmetics aqueous solution, mercurous in judgement sample.
Preferably, in the cosmetics aqueous solution described in step (1), the concentration of cosmetics is 0.1 ~ 0.3g/ml.
Preferably, the described water of step (1) is purified water.
Preferably, the addition of described alkyl polyoxyethylene ether is 5-10ml.
Preferably, described acid solution is hydrochloric acid solution, and concentration is 0.8-1.2mol/L, and the amount adding is 5ml.
Preferably, the described reagent that can produce sulphion is sodium sulfide solution or thioacetyl amine aqueous solution, and the concentration of described sodium sulfide solution or thioacetyl amine aqueous solution is 0.3 ~ 1.0mol/L, and addition is 5-10ml.
Preferably, the described reagent that can produce iodide ion is IodineSodium Solution or liquor kalii iodide, and described IodineSodium Solution or the concentration of liquor kalii iodide are 0.3-0.8mol/L, and addition is 5-10ml.
Preferably, described stannous chloride dosage enters for 0.5g, and in described step (2), the heat time is 10min, and heating-up temperature is 60-80 ℃.
Preferably, described copper sheet quality is 0.5-2g.
Preferably, described chromogenic reaction is specially in the cosmetics aqueous solution that adds first part of detection reagent and occurs black or grey; Add in second part of cosmetics aqueous solution that detects reagent and occur salmon pink precipitation; Add copper sheet surface color in the 3rd part of cosmetics aqueous solution that detects reagent to become silvery white.
 
Compared with the existing technology, beneficial effect has in the present invention:
1. the present invention adopts three kinds of reagent to develop the color to judge in cosmetics whether contain mercury simultaneously, more accurate than the method only judging with two kinds of reagent, has prevented from only adopting the false negative phenomenon often occurring in two kinds of reagent deterministic processes.
2. the present invention compares with the detection method of traditional cosmetics mercury, does not need to use exact instrument, only needs reagent can complete testing process, testing result judgement only needs to observe change color, and simple to operate, testing cost is low, can Site Detection, meet actual detection demand.
3. the present invention compares with the detection method of traditional cosmetics mercury, does not produce harmful gas, environmentally safe.
4. in the present invention, in first part of cosmetics aqueous solution, add can produce in the reagent of sulphion and the 3rd part of cosmetics aqueous solution to add stannous chloride, copper sheet, this two group reaction also can other heavy metal ion of preliminary judgement as existence plumbous, arsenic.In the present invention, in cosmetics reactant aqueous solution liquid, all add hydrochloric acid, can avoid the interference of ferric ion to the experiment of this group.The present invention has higher sensitivity, is applicable to the conventional sense of cosmetics supervision department to Mercury In Cosmetics.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail:
Embodiment 1:
The detection method of mercury in light spot frost, comprises the following steps:
(1) 5g cosmetics to be measured (light spot frost) are joined in 20ml purified water, be mixed with cosmetics aqueous solution;
(2) hydrochloric acid solution of 5ml alkyl polyoxyethylene ether, 5ml (0.8 mol/L) and 5ml sodium sulfide solution (0.5mol/L) are added in test tube, mix and be mixed with first part and detect reagent;
The hydrochloric acid solution of 5ml alkyl polyoxyethylene ether, 5ml (0.8 mol/L) and 5ml IodineSodium Solution (0.5mol/L) are added to mix in test tube and be mixed with second part and detect reagent;
The hydrochloric acid solution of 5ml (0.8 mol/L), 0.5g stannous chloride are added in test tube and be heated to 60 ℃, heat time 10min, then add 0.5g copper sheet, and remain micro-and boil, in heating process, add hot water, keep liquor capacity constant, be mixed with the 3rd part and detect reagent;
(3) the cosmetics aqueous solution making in step (1) is divided into three parts, adds respectively first part to detect reagent, second part of detection reagent and the 3rd part of detection reagent, observe the variation of the aqueous solution color of cosmetics;
There is black in first part of cosmetics aqueous solution or sample surfaces wherein, and salmon pink precipitation appears in second part of cosmetics aqueous solution or specimen surface, and in the 3rd part of cosmetics aqueous solution, copper sheet color becomes silvery white, can judge in these cosmetics mercurous.
Embodiment 2:
The detection method of mercury in skin whitener, comprises the following steps:
(1) 6g cosmetics to be measured (skin whitener) are joined in 20ml purified water, be mixed with cosmetics aqueous solution;
(2) hydrochloric acid solution of 5ml alkyl polyoxyethylene ether, 5ml (0.8 mol/L) and 5ml sodium sulfide solution (0.5mol/L) are added in test tube, mix and be mixed with first part and detect reagent;
The hydrochloric acid solution of 5ml alkyl polyoxyethylene ether, 5ml (1.2 mol/L) and 5ml IodineSodium Solution (0.3mol/L) are added to mix in test tube and be mixed with second part and detect reagent;
The hydrochloric acid solution of 5ml (1.2 mol/L), 0.5g stannous chloride are added in test tube and be heated to 80 ℃, heat time 10min, then add 2g copper sheet, and remain micro-and boil, in heating process, add hot water, keep liquor capacity constant, be mixed with the 3rd part and detect reagent;
(3) the cosmetics aqueous solution making in step (1) is divided into three parts, adds respectively first part to detect reagent, second part of detection reagent and the 3rd part of detection reagent, observe the variation of the aqueous solution color of cosmetics;
There is grey in first part of cosmetics aqueous solution or sample surfaces wherein, the nondiscolouring of second part of cosmetics aqueous solution, and in the 3rd part of cosmetics aqueous solution, there is not change color in copper sheet, can judge in these cosmetics not mercurous.
Embodiment 3
The detection method of mercury in whitening spot-relieving cream, comprises the following steps:
(1) 2g cosmetics to be measured (whitening spot-relieving cream) are joined in 20ml purified water, be mixed with cosmetics aqueous solution;
(2) hydrochloric acid solution of 5ml alkyl polyoxyethylene ether, 5ml (1.0 mol/L) and 5ml thioacetyl amine aqueous solution (0.5mol/L) are added in test tube, mix and be mixed with first part and detect reagent;
The hydrochloric acid solution of 8ml alkyl polyoxyethylene ether, 5ml (1.0 mol/L) and 5ml liquor kalii iodide (0.8mol/L) are added to mix in test tube and be mixed with second part and detect reagent;
The hydrochloric acid solution of 5ml (1.0 mol/L), 0.5g stannous chloride are added in test tube and be heated to 70 ℃, heat time 10min, then add 1.0g copper sheet, and remain micro-and boil, in heating process, add hot water, keep liquor capacity constant, be mixed with the 3rd part and detect reagent;
(3) the cosmetics aqueous solution making in step (1) is divided into three parts, adds respectively first part to detect reagent, second part of detection reagent and the 3rd part of detection reagent, observe the variation of the aqueous solution color of cosmetics;
There is grey in first part of cosmetics aqueous solution or sample surfaces wherein, and salmon pink precipitation appears in second part of cosmetics aqueous solution or specimen surface, and in the 3rd part of cosmetics aqueous solution, copper sheet color becomes silvery white, can judge in these cosmetics mercurous.
The above embodiment is preferred embodiments of the present invention, is not to limit the scope of the present invention, and the equivalence of doing according to structure, feature and principle described in the present patent application the scope of the claims therefore all changes or modifies, and all should comprise in patent claim of the present invention.

Claims (10)

1. a detection method for Mercury In Cosmetics, is characterized in that, comprises the steps:
(1) cosmetics to be measured are added to the water, are mixed with cosmetics aqueous solution;
(2) alkyl polyoxyethylene ether, acid solution and the reagent that can produce sulphion are added in test tube, mix and be mixed with first part and detect reagent; Alkyl polyoxyethylene ether, acid solution and the reagent that can produce iodide ion are added to mix in test tube and be mixed with second part and detect reagent; Acid solution, stannous chloride are added in test tube and heated, then add copper sheet, remain micro-and boil, in heating process, add hot water, keep liquor capacity constant, be mixed with the 3rd part and detect reagent;
(3) the cosmetics aqueous solution making in step (1) is divided into three parts, adds respectively first part to detect reagent, second part of detection reagent and the 3rd part of detection reagent, observe the variation of the aqueous solution color of cosmetics; As feature chromogenic reaction all appears in three parts of cosmetics aqueous solution, mercurous in judgement sample.
2. the detection method of a kind of Mercury In Cosmetics according to claim 1, is characterized in that, in the cosmetics aqueous solution described in step (1), the concentration of cosmetics is 0.1 ~ 0.3g/ml.
3. the detection method of a kind of Mercury In Cosmetics according to claim 1 and 2, is characterized in that, the described water of step (1) is purified water.
4. the detection method of a kind of Mercury In Cosmetics as claimed in claim 1, is characterized in that, the addition of described alkyl polyoxyethylene ether is 5-10ml.
5. the detection method of a kind of Mercury In Cosmetics as claimed in claim 1, is characterized in that, described acid solution is hydrochloric acid solution, and concentration is 0.8-1.2mol/L, and the amount adding is 5ml.
6. the detection method of a kind of Mercury In Cosmetics as claimed in claim 1, it is characterized in that, the described reagent that can produce sulphion is sodium sulfide solution or thioacetyl amine aqueous solution, and the concentration of described sodium sulfide solution or thioacetyl amine aqueous solution is 0.3 ~ 1.0mol/L, and addition is 5-10ml.
7. the detection method of a kind of Mercury In Cosmetics as claimed in claim 1, it is characterized in that, the described reagent that can produce iodide ion is IodineSodium Solution or liquor kalii iodide, and described IodineSodium Solution or the concentration of liquor kalii iodide are 0.3-0.8mol/L, and addition is 5-10ml.
8. the detection method of a kind of Mercury In Cosmetics as claimed in claim 1, is characterized in that, described stannous chloride dosage enters for 0.5g, and in described step (2), the heat time is 10min, and heating-up temperature is 60-80 ℃.
9. the detection method of a kind of Mercury In Cosmetics as claimed in claim 1, is characterized in that, described copper sheet quality is 0.5-2g.
10. the detection method of a kind of Mercury In Cosmetics as claimed in claim 1, is characterized in that, described chromogenic reaction is specially in the cosmetics aqueous solution that adds first part of detection reagent and occurs black or grey; Add in second part of cosmetics aqueous solution that detects reagent and occur salmon pink precipitation; Add copper sheet surface color in the 3rd part of cosmetics aqueous solution that detects reagent to become silvery white.
CN201310616292.7A 2013-11-28 2013-11-28 Method for detecting mercury in cosmetics Pending CN103616378A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104198475A (en) * 2014-08-16 2014-12-10 中山鼎晟生物科技有限公司 Fast detection method of mercury in cosmetics
CN104198477A (en) * 2014-08-16 2014-12-10 中山鼎晟生物科技有限公司 Rapid detection kit for mercury in cosmetics and detection method
CN104280386A (en) * 2014-09-20 2015-01-14 中山鼎晟生物科技有限公司 Method for rapidly detecting mercury in shampoo
CN104297238A (en) * 2014-10-18 2015-01-21 中山鼎晟生物科技有限公司 Rapid detection method for mercury in lipstick
CN106769388A (en) * 2016-12-23 2017-05-31 大工(青岛)新能源材料技术研究院有限公司 The processing detection method of Mercury In Cosmetics content

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Publication number Priority date Publication date Assignee Title
CN101782522A (en) * 2010-02-09 2010-07-21 广东省疾病预防控制中心 Quick detection method of mercury in cosmetics and reagent kit thereof

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN101782522A (en) * 2010-02-09 2010-07-21 广东省疾病预防控制中心 Quick detection method of mercury in cosmetics and reagent kit thereof

Non-Patent Citations (1)

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Title
龚来芳: "《美容美发企业管理》", 30 June 2009, 南海出版公司 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104198475A (en) * 2014-08-16 2014-12-10 中山鼎晟生物科技有限公司 Fast detection method of mercury in cosmetics
CN104198477A (en) * 2014-08-16 2014-12-10 中山鼎晟生物科技有限公司 Rapid detection kit for mercury in cosmetics and detection method
CN104280386A (en) * 2014-09-20 2015-01-14 中山鼎晟生物科技有限公司 Method for rapidly detecting mercury in shampoo
CN104297238A (en) * 2014-10-18 2015-01-21 中山鼎晟生物科技有限公司 Rapid detection method for mercury in lipstick
CN106769388A (en) * 2016-12-23 2017-05-31 大工(青岛)新能源材料技术研究院有限公司 The processing detection method of Mercury In Cosmetics content

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Application publication date: 20140305