CN103712970A - Method for detecting content of dioxane in children cosmetics - Google Patents
Method for detecting content of dioxane in children cosmetics Download PDFInfo
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Abstract
The invention relates to a method for detecting the content of dioxane in children cosmetics. The method comprises the following steps: (1) pretreating a sample to be detected so as to form a sample solution; (2) uniformly mixing the sample solution with prepared nanometer silver colloid so as to form a sample mixed solution; (3) dropping the sample mixed solution on a substrate, and naturally airing, thus obtaining a detection sample; (4) detecting the detection sample by adopting surface-enhanced Raman scattering, thus obtaining an SERS (surface enhanced Raman spectrum) spectrogram of the detection sample; and (5) comparing the obtained SERS spectrogram of the detection sample with an SERS spectrogram of a dioxane standard solution, and calculating so as to obtain the content of the dioxane in the detection sample. The method is simple, convenient and fast to operate and can be used for rapidly carrying out qualitative and quantitative analysis on the content of the dioxane in children cosmetics.
Description
Technical field
The invention belongs to cosmetics objectionable impurities detection technique field, specifically relate to a kind of method of the children's of detection cosmetics diox content.
Background technology
Diox, another name dioxane, Isosorbide-5-Nitrae-dioxane, colourless transparent liquid, molecular formula is C
4h
8o
2, molecular weight is 88.1, slightly fragrance.The micro-toxicity of diox, belongs to the material banning use of in cosmetics, can to skin, eye and respiratory system, have anesthesia and pungency by sucking, eat and absorbing and enter in body through skin, has in vivo cumulative effect.Diox is not raw materials for production, it is the accessory substance of producing fatty alcohol polyoxyethylene ether sulfate (AES), main as solvent, emulsifying agent, scaling agent etc., compatibility to water in physical environment is stronger, and be difficult for being degraded by biological, per os is taken in, and liver cell is had to obvious carcinogenic activity, can cause mouse turbinate tumour and clear-cell carcinoma.If children's cosmetics contain diox, will children be produced to larger harm.Therefore ， diox is decided to be 2B class carcinogen, the European Community (EEC), China's hygienic standards for cosmetics (GB7916) 1987 by the international tumor research center of the World Health Organization (WHO) (IARC)) regulation dioxan is the banned substance in components of cosmetics.In cosmetics, diox is normally brought by raw material itself, not additive.
At present, in the washing agent such as shampoo both at home and abroad, body lotion, tableware, Contents of Dioxane detection method is more, generally adopts Headspace-Gas Chromatography Analysis to carry out quantitatively, with gas chromatography-mass spectrography (GC-MS), carries out qualitative confirmation.Chromatography has that separation efficiency is high, analysis speed is fast, selectivity is good and the advantage such as Simultaneous Analysis for Multicomponent, and particularly itself and mass spectroscopy coupling (GC-MS) or gas chromatography and flame ion coupling detection technique (GC-FID) are being born the conventional sense task of para-dioxane assay always.But these instrument and equipments are expensive, complicated operation, analysis cost is high, and detection sensitivity is not high, for the relatively low children's cosmetics of diox content, is not desirable practical detection method.
It is to take Raman scattering as the analysis and characterization technology that Foundation gets up that Surface enhanced raman spectroscopy (Surface-enhanced Raman Spectroscopy is called for short SERS) is analyzed, and its Raman signal intensity is strengthened greatly.Yi Bi family metal gold, silver, copper are substrate, and its SERS strengthens generally can reach 10
6-10
12doubly.The detection method sensitivity of Surface enhanced raman spectroscopy is higher, good stability, is applied gradually in the research of biology, diagnostics, medical science, material science, analysis science and Surface Science.At present, in prior art, also do not adopt Surface enhanced raman spectroscopy to report that in cosmetics, diox content detects.
Summary of the invention
Fundamental purpose of the present invention is to provide a kind of method of the children's of detection cosmetics diox content, and it is simple to operate, and accuracy of detection is high, and use cost is low.
The present invention adopts following technical scheme:
Detect a method for children's cosmetics diox content, carry out according to the following steps: (1) carries out pre-service to testing sample, make it to form sample solution; (2) sample solution is mixed with the nano silver colloidal sol of preparation, form sample mix solution; (3) sample thief mixed solution, drips on substrate, naturally dries, and obtains detecting sample; (4) adopt Surface enhanced raman spectroscopy to detect in detection sample, obtain detecting the SERS spectrogram of sample; (5) gained is detected to the SERS spectrogram of sample Yu the SERS spectrogram of diox standard solution contrasts, calculate the content that detects sample diox.
The pre-service of testing sample described in step (1) is carried out as follows: first take testing sample, testing sample is poured in the beaker that ethanol is housed, soak 6-24h, then stir 2-6h; Finally, suction filtration, concentrated filtrate, and sealing is placed standby.
Described in step (2), the preparation method of nano silver colloidal sol is: in container, add aqueous solution to stir, described aqueous solution contains 0.2-2mM silver nitrate, 0.1-1mM sodium dodecylsulphonate and 0.1-2mM ethylenediamine tetraacetic acid, and the pH value of aqueous solution is adjusted to 9-12; Then, add 0.1-1mM ascorbic acid solution, keep stirring 5-60min; Finally, centrifugal concentrating 1-5 time, makes nano silver colloidal sol.
The concentration ratio that in step (2), nano silver colloidal sol mixes with sample solution is 1:1～100:1, at least standing 3min.
Described in step (3), substrate is mica sheet, silicon chip or quartz glass plate.
In step (4), each detection sample adopts Surface enhanced raman spectroscopy detection to be no less than 5 points.
In step (5), the drafting of the SERS spectrogram of diox standard solution adopts following steps: get accurate concentration diox standard solution and mix with nano silver colloidal sol, add potassium chloride, the addition of potassium chloride reaches 10mM with the concentration of Chlorine in Solution potassium and is as the criterion, and stirs; Then, with Raman spectrometer, scan, instrument parameter be set: optical maser wavelength be 632.8nm, laser power be 5mW, sweep time 20s and scanning cumulative frequency be 2 times.
In step (5), calculate and adopt following computing formula:
Detect that the content of sample diox=(sample to be tested diox is the SERS intensity/diox standard solution concentration of the SERS intensity) × diox standard solution of strong characteristic peak of strong characteristic peak.
Adopt after technique scheme, the present invention compares with existing background technology, and tool has the following advantages:
1, the present invention is easy and simple to handle, quick, can to the content of cosmetics diox, carry out qualitative and quantitative analysis fast.
2, the present invention adopts nano silver colloidal sol as surface enhanced Raman substrate, strengthen the SERS signal that detects sample, can greatly improve detection sensitivity, reduce detectability, the detection of realization to the relatively low children's cosmetics of diox content, the detection of the cosmetics that are simultaneously also applicable to be grown up.
3, the present invention adopts the nano silver colloidal sol of being convenient to make as material, with Raman spectrometer, detects, and has saved cost, is easy to popularization and application.
Accompanying drawing explanation
The SERS spectrogram of Fig. 1 Wei diox standard solution;
Fig. 2 is for detecting the SERS spectrogram of a certain sampling point of sample diox.
Embodiment
Some embodiments of the present invention are below provided, to help further, understand the present invention, but protection scope of the present invention are not limited in these embodiment.
The common Raman standard spectrogram of sterling diox is 428,479,821,1000,1091,1112,1200,1287 and 1425 cm
-1there is obvious raman characteristic peak at place.428 cm
-1characteristic peak derives from C-O-C flexural vibrations, 479 cm
-1characteristic peak derives from C-C-O flexural vibrations, 821cm
-1characteristic peak derives from ring breathing vibration, 1000 cm
-1characteristic peak derives from C-C stretching vibration in ring, 1091 cm
-1characteristic peak derives from the asymmetric stretching vibration of C-O-C, 1112cm
-1characteristic peak derives from C-H rocking vibration, 1200cm
-1characteristic peak derives from C-H rocking vibration, 1287cm
-1characteristic peak derives from C-H rocking vibration, 1425 cm
-1characteristic peak derives from H-C-H flexural vibrations.Wherein, 821cm
-1characteristic peak is the strongest characteristic peak.
Embodiment mono-
Detect a method for children's cosmetics diox content, carry out according to the following steps:
(1) testing sample is carried out to pre-service, make it to form sample solution.Described testing sample pre-service can adopt common method to process, and such as one or more in dissolving, extraction, micro-extraction, distillation and chromatography, specifically can carry out as follows: first take testing sample 20g, be accurate to 0.0001g; Then testing sample is poured in the beaker that 100ml ethanol is housed, soaked 10h, then stir 3h; Finally, suction filtration, filtrate is concentrated into 5ml, and sealing is placed standby.
(2) in container, add 20ml aqueous solution to stir, described aqueous solution contains 1mM silver nitrate, 0.25mM sodium dodecylsulphonate and 1mM ethylenediamine tetraacetic acid, and the pH value of aqueous solution is adjusted to 11; Then, add 50 μ L0.1mol/L ascorbic acid solutions, keep stirring 30min; Finally, centrifugal concentrating 2 times, makes the nano silver colloidal sol that volume is 5ml.The particle size of nano silver colloidal sol is 10-100 nm, and the shape of particle of nano silver colloidal sol is one or more of spherical, linear, triangle, cube and Hua Xingzhong.
The nano silver colloidal sol of preparation is mixed with sample solution, form sample mix solution.The concentration ratio that nano silver colloidal sol mixes with sample solution is 1:1, standing 5min.
(3) sample thief mixed solution, drips on mica sheet, naturally dries, and obtains detecting sample.
(the drafting of 4) diox standard solution collection of illustrative plates: get the accurate concentration diox of 5ml standard solution and mix with 5ml nano silver colloidal sol, add potassium chloride, the addition of potassium chloride reaches 10mM with the concentration of Chlorine in Solution potassium and is as the criterion, and stirs.
Then, with Raman spectrometer, scan, instrument parameter be set: optical maser wavelength be 632.8nm, laser power be 5mW, sweep time 20s and scanning cumulative frequency be 2 times.After scanning, obtain diox standard solution Raman spectrogram.From figure, can draw the characteristic peak 821cm that diox is the strongest
-1sERS intensity, as shown in Figure 1.
The Raman spectrum that detects sample detects: by the detection sample arriving in step (3), gather 5 representational sampling points, with Raman spectrometer, detect respectively, instrument parameter be set: optical maser wavelength be 632.8nm, laser power be 5mW, sweep time 20s and scanning cumulative frequency be 2 times.Scanning obtains detecting sample diox Raman spectrogram.Calculate and detect 5 sampling point diox characteristic peak 821cm of sample
-1average SERS intensity.
(5) are linear Yin concentration and its SERS intensity of diox, according to formula, can calculate the content (concentration) that detects sample diox.Computing formula is as follows:
Detect content=(the detection sample diox 821cm of sample diox
-1sERS intensity/diox standard solution 821cm
-1the concentration of SERS intensity) × diox standard solution.
Embodiment bis-
Detect a method for children's cosmetics diox content, carry out according to the following steps:
(1) testing sample is carried out to pre-service, make it to form sample solution.Described testing sample pre-service can adopt common method to process, and such as one or more in dissolving, extraction, micro-extraction, distillation and chromatography, specifically can carry out as follows: first take testing sample 20g, be accurate to 0.0001g; Then testing sample is poured in the beaker that 100ml ethanol is housed, soaked 12h, then stir 4h; Finally, suction filtration, filtrate is concentrated into 5ml, and sealing is placed standby.
(2) in container, add 20ml aqueous solution to stir, described aqueous solution contains 1.2mM silver nitrate, 0.5mM sodium dodecylsulphonate and 0.8mM ethylenediamine tetraacetic acid, and the pH value of aqueous solution is adjusted to 10; Then, add 50 μ L0.5mol/L ascorbic acid solutions, keep stirring 30min; Finally, centrifugal concentrating 3 times, makes the nano silver colloidal sol that volume is 6ml.
The nano silver colloidal sol of preparation is mixed with sample solution, form sample mix solution.The concentration ratio that nano silver colloidal sol mixes with sample solution is 50:1, standing 5min.
(3) sample thief mixed solution, drips on silicon chip, naturally dries, and obtains detecting sample.
(the drafting of 4) diox standard solution collection of illustrative plates: get the accurate concentration diox of 5ml standard solution and mix with 5ml nano silver colloidal sol, add potassium chloride, the addition of potassium chloride reaches 12mM with the concentration of Chlorine in Solution potassium and is as the criterion, and stirs.
Then, with Raman spectrometer, scan, instrument parameter be set: optical maser wavelength be 632.8nm, laser power be 5mW, sweep time 20s and scanning cumulative frequency be 2 times.After scanning, obtain diox standard solution Raman spectrogram.From figure, can draw the characteristic peak 821cm that diox is the strongest
-1sERS intensity.
The Raman spectrum that detects sample detects: by the detection sample arriving in step (3), gather 5 representational sampling points, with Raman spectrometer, detect respectively, instrument parameter be set: optical maser wavelength be 632.8nm, laser power be 5mW, sweep time 30s and scanning cumulative frequency be 2 times.Scanning obtains detecting sample diox Raman spectrogram.Calculate and detect 5 sampling point diox characteristic peak 821cm of sample
-1average SERS intensity.
(5) according to formula, can calculate the content (concentration) that detects sample diox.Computing formula is as follows:
Detect content=(detection sample diox 821 cm of sample diox
-1sERS intensity/diox standard solution 821 cm
-1the concentration of SERS intensity) × diox standard solution.
Embodiment tri-
Detect a method for children's cosmetics diox content, carry out according to the following steps:
(1) testing sample is carried out to pre-service, make it to form sample solution.Described testing sample pre-service can adopt common method to process, and such as one or more in dissolving, extraction, micro-extraction, distillation and chromatography, specifically can carry out as follows: first take testing sample 20g, be accurate to 0.0001g; Then testing sample is poured in the beaker that 100ml ethanol is housed, soaked 18h, then stir 5h; Finally, suction filtration, filtrate is concentrated into 5ml, and sealing is placed standby.
(2) in container, add 20ml aqueous solution to stir, described aqueous solution contains 0.8mM silver nitrate, 1mM sodium dodecylsulphonate and 2mM ethylenediamine tetraacetic acid, and the pH value of aqueous solution is adjusted to 10.5; Then, add 50 μ L1mol/L ascorbic acid solutions, keep stirring 50min; Finally, centrifugal concentrating 5 times, makes the nano silver colloidal sol that volume is 5ml.The particle size of nano silver colloidal sol is 10-100 nm, and the shape of particle of nano silver colloidal sol is one or more of spherical, linear, triangle, cube and Hua Xingzhong.
The nano silver colloidal sol of preparation is mixed with sample solution, form sample mix solution.The concentration ratio that nano silver colloidal sol mixes with sample solution is 100:1, standing 4min.
(3) sample thief mixed solution, drips on quartz glass plate, naturally dries, and obtains detecting sample.
(the drafting of 4) diox standard solution collection of illustrative plates: get the accurate concentration diox of 5ml standard solution and mix with 5ml nano silver colloidal sol, add potassium chloride, the addition of potassium chloride reaches 10mM with the concentration of Chlorine in Solution potassium and is as the criterion, and stirs.
Then, with Raman spectrometer, scan, instrument parameter be set: optical maser wavelength be 632.8nm, laser power be 5mW, sweep time 20s and scanning cumulative frequency be 2 times.After scanning, obtain diox standard solution Raman spectrogram.From figure, can draw the characteristic peak 821cm that diox is the strongest
-1sERS intensity.
The Raman spectrum that detects sample detects: by the detection sample arriving in step (3), gather 5 representational sampling points, with Raman spectrometer, detect respectively, instrument parameter be set: optical maser wavelength be 632.8nm, laser power be 5mW, sweep time 20s and scanning cumulative frequency be 2 times.Scanning obtains detecting sample diox Raman spectrogram.Calculate and detect 5 sampling point diox characteristic peak 821cm of sample
-1average SERS intensity.
(5) are linear Yin concentration and its SERS intensity of diox, according to formula, can calculate the content (concentration) that detects sample diox.Computing formula is as follows:
Detect content=(the detection sample diox 821cm of sample diox
-1sERS intensity/diox standard solution 821cm
-1the concentration of SERS intensity) × diox standard solution.
It should be noted that, that in above each embodiment, mentions " detects sample diox 821cm
-1sERS intensity ", refer to the strongest characteristic peak (821cm that detects sample diox
-1left and right) SERS intensity.Due to the difference of base material, can there is certain deviation (as shown in Figure 2) in the strongest characteristic peak positions that detects the Raman spectrogram of sample.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under Spirit Essence of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (8)
1. a method that detects children's cosmetics diox content, is characterized in that: carry out according to the following steps: (1) carries out pre-service to testing sample, makes it to form sample solution; (2) sample solution is mixed with the nano silver colloidal sol of preparation, form sample mix solution; (3) sample thief mixed solution, drips on substrate, naturally dries, and obtains detecting sample; (4) adopt Surface enhanced raman spectroscopy to detect in detection sample, obtain detecting the SERS spectrogram of sample; (5) gained is detected to the SERS spectrogram of sample Yu the SERS spectrogram of diox standard solution contrasts, calculate the content that detects sample diox.
2. a kind of method that detects children's cosmetics diox content according to claim 1, it is characterized in that: the pre-service of testing sample described in step (1) is carried out as follows: first take testing sample, testing sample is poured in the beaker that ethanol is housed, soak 6-24h, then stir 2-6h; Finally, suction filtration, concentrated filtrate, and sealing is placed standby.
3. a kind of method that detects children's cosmetics diox content according to claim 1 and 2, it is characterized in that: described in step (2), the preparation method of nano silver colloidal sol is: in container, add aqueous solution to stir, described aqueous solution contains 0.2-2mM silver nitrate, 0.1-1mM sodium dodecylsulphonate and 0.1-2mM ethylenediamine tetraacetic acid, and the pH value of aqueous solution is adjusted to 9-12; Then, add 0.1-1M ascorbic acid solution, keep stirring 5-60min; Finally, centrifugal concentrating 1-5 time, makes nano silver colloidal sol.
4. a kind of method that detects children's cosmetics diox content according to claim 3, is characterized in that: the concentration ratio that in step (2), nano silver colloidal sol mixes with sample solution is 1:1～100:1, at least standing 3min.
5. a kind of method that detects children's cosmetics diox content as claimed in claim 3, is characterized in that: described in step (3), substrate is mica sheet, silicon chip or quartz glass plate.
6. a kind of method that detects children's cosmetics diox content as claimed in claim 4, is characterized in that: in step (4), each detection sample adopts Surface enhanced raman spectroscopy detection to be no less than 5 points.
7. a kind of method that detects children's cosmetics diox content as claimed in claim 4, it is characterized in that: in step (5), the drafting of the SERS spectrogram of diox standard solution adopts following steps: get accurate concentration diox standard solution and mix with nano silver colloidal sol, add potassium chloride, the addition of potassium chloride reaches 10mM with the concentration of Chlorine in Solution potassium and is as the criterion, and stirs; Then, with Raman spectrometer, scan, instrument parameter be set: optical maser wavelength be 632.8nm, laser power be 5mW, sweep time 20s and scanning cumulative frequency be 2 times.
8. a kind of method that detects children's cosmetics diox content as claimed in claim 7, is characterized in that: in step (5), calculate and adopt following computing formula:
Detect the content of sample diox=(detect the SERS intensity/diox standard solution concentration of the SERS intensity) × diox standard solution of strong characteristic peak of strong characteristic peak of sample diox.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310742607.2A CN103712970B (en) | 2013-12-30 | 2013-12-30 | Method for detecting content of dioxane in children cosmetics |
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| CN113740456A (en) * | 2021-09-03 | 2021-12-03 | 广东省中鼎检测技术有限公司 | Detection method for testing 1, 4-dioxane in consumer product |
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