CN104020234A - Method for separating and analyzing coloring agent in cosmetics by use of reverse micelle - Google Patents
Method for separating and analyzing coloring agent in cosmetics by use of reverse micelle Download PDFInfo
- Publication number
- CN104020234A CN104020234A CN201410289061.4A CN201410289061A CN104020234A CN 104020234 A CN104020234 A CN 104020234A CN 201410289061 A CN201410289061 A CN 201410289061A CN 104020234 A CN104020234 A CN 104020234A
- Authority
- CN
- China
- Prior art keywords
- cosmetics
- colorant
- reverse micelle
- organic solvent
- coloring agent
- 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.)
- Pending
Links
Abstract
The invention provides a method for separating and analyzing a coloring agent in cosmetics by use of reverse micelle and relates to a method for analyzing the coloring agent in cosmetics for solving the problems that an existing method for detecting the coloring agent in cosmetics has low enrichment capacity, poor selectivity, more impurities and poor purifying effect. The method comprises the steps of carrying out ultrasonic extraction on cosmetics containing the coloring agent by use of a surface active agent and an organic solvent A, adding deionized water and inorganic salt, mixing uniformly, centrifugally separating, adding an organic solvent B in supernatant, performing reextraction at certain temperature by use of a shaking table, standing for layering, filtering the lower layer by a 0.45-mircon filtering membrane, and analyzing filtrate by a high-performance liquid chromatography method, thereby achieving separation and analysis of the coloring agent in cosmetics by use of the reverse micelle. The method has the advantages of high selectivity, strong enrichment capacity, high accuracy, high precision, good reproducibility and low relative standard deviation less than 6%, and is mainly applied to analysis of the coloring agent in cosmetics.
Description
Technical field
The present invention relates to a kind of method of analyzing colorant in cosmetics.
Background technology
Along with the raising of people's living standard, cosmetics have become the part in people's daily life.Cosmetics are the products that directly contact with human body, and the objectionable constituent in cosmetics can produce potential impact to health, and its safety problem is the problem that consumer is extremely concerned about always.All use colorant at a lot of cosmetics in as lipstick, lipstick, eye shadow, muffin.The colorant majority using in cosmetics is synthetic dyestuffs, long-term or excessive use meeting produces potential harm to health, if any colorant can cause allergic reaction, the colorant also having can see through skin be absorbed by the body, use for a long time this series products even can bring out cancer.Therefore, the analytical approach of colorant in more reliable, the more effective rapid and accurate determination cosmetics of setting-up and development, for the quality supervision management of strengthening cosmetics, protection health tool is of great significance.
At present, the detection of cosmetics mainly adopts gas chromatography/mass spectrometry, and liquid chromatography ultraviolet-visible light detects, or Liquid Chromatography-Tandem Mass Spectrometry.But, before chromatogram detects, need to carry out pre-service to sample, general using organic solvent extracts under ultrasonic effect, extract directly detects after centrifugal or filtration afterwards, or extracts after nitrogen dries up, then or detects after Solid phase extraction.
In these methods, that directly detects does not have an accumulation ability; The method clean-up effect detecting after nitrogen dries up is bad, can not well remove impurity compound; Though solid phase extraction has the effect of some enrichments and purification, its selectivity is unsatisfactory.
If surfactant is joined in organic solvent, and make its concentration exceed critical micelle concentration, just can form aggregation in organic solvent, this aggregation becomes reverse micelle.In reverse micelle, the non-polar group of surfactant outside, contacts with nonpolar organic solvent, and in polar group is arranged in, forms a polarity core, and this polarity core has just formed pond after absorbing water, has the ability of dissolving polar material.
In sum, in existing detection cosmetics, the method accumulation ability of colorant is not strong, poor selectivity, and impurity is many, and clean-up effect is bad.
Summary of the invention
The method accumulation ability that the object of the invention is to solve colorant in existing detection cosmetics is not strong, poor selectivity, and impurity is many, the problem that clean-up effect is bad, and a kind of method of utilizing colorant in reverse micelle compartment analysis cosmetics is provided.
A method of utilizing colorant in reverse micelle compartment analysis cosmetics, specifically completes according to the following steps:
The cosmetics that 0.2g～0.5g is contained to colorant join in centrifuge tube A, then add 0.5g～1g surfactant and 5mL～15mL organic solvent A, be placed in again ultrasonic oscillator, be to extract 3min～6min under 40KHz～80KHz in ultrasonic frequency, then add 5mL～15mL deionized water and 1g～4g inorganic salts, low whipping speed is to be stirred to and to mix under 2000r/min～3000r/min, then be placed in the centrifugal 4min～6min of centrifugal speed of supercentrifuge with 4500r/min～5500r/min, the upper strata liquid that centrifuging obtains is transferred in centrifuge tube B, add again 1mL～3mL organic solvent B, then be placed in shaking table, being 30～50 DEG C in temperature is the 8min～12min that strips under 200r/min～300r/min with shaking speed, stratification 2min～5min, the lower floor that stratification obtains adopts the membrane filtration of 0.45 μ m, the filtrate that filtration obtains adopts efficient liquid phase chromatographic analysis, complete and utilize colorant in reverse micelle compartment analysis cosmetics,
Described organic solvent A is isooctane, normal hexane, cyclohexane, isopropyl alcohol or n-octyl alcohol;
Described organic solvent B is methyl alcohol, ethanol or acetonitrile;
Described surfactant is cetab, two-(2-ethylhexyl) succinate sodium sulfonate or lauryl sodium sulfate.
Advantage of the present invention: 1. selectivity is high, is used the different types of ion of different types of SURFACTANT ADSORPTION.The topmost expulsive force of inverse micelle abstraction is the electrostatic attraction between positive and negative charge.Surfactant and extract are with charges of different polarity quantity more separately, and electrostatic attraction effect is just stronger, thereby is more easily extracted by the reverse micelle of oppositely charged, thereby improve the sensitivity of analytical approach.2. accumulation ability is strong.In the process of finally stripping, colorant can be enriched to a small amount of volume.3. accuracy is high, and the recovery can reach more than 90%.4. precision is high, favorable reproducibility, RSD<6%.
Brief description of the drawings
Fig. 1 is the high-efficient liquid phase chromatogram of test one.
Embodiment
Embodiment one: present embodiment is a kind of method of utilizing colorant in reverse micelle compartment analysis cosmetics, specifically completes according to the following steps:
The cosmetics that 0.2g～0.5g is contained to colorant join in centrifuge tube A, then add 0.5g～1g surfactant and 5mL～15mL organic solvent A, be placed in again ultrasonic oscillator, be to extract 3min～6min under 40KHz～80KHz in ultrasonic frequency, then add 5mL～15mL deionized water and 1g～4g inorganic salts, low whipping speed is to be stirred to and to mix under 2000r/min～3000r/min, then be placed in the centrifugal 4min～6min of centrifugal speed of supercentrifuge with 4500r/min～5500r/min, the upper strata liquid that centrifuging obtains is transferred in centrifuge tube B, add again 1mL～3mL organic solvent B, then be placed in shaking table, being 30～50 DEG C in temperature is the 8min～12min that strips under 200r/min～300r/min with shaking speed, stratification 2min～5min, the lower floor that stratification obtains adopts the membrane filtration of 0.45 μ m, the filtrate that filtration obtains adopts efficient liquid phase chromatographic analysis, complete and utilize colorant in reverse micelle compartment analysis cosmetics.
Organic solvent A described in present embodiment is isooctane, normal hexane, cyclohexane, isopropyl alcohol or n-octyl alcohol; Described organic solvent A is the organic solvent that polarity is less.
Organic solvent B described in present embodiment is methyl alcohol, ethanol or acetonitrile.Described organic solvent B is the organic solvent that polarity is larger.
Surfactant described in present embodiment is cetab (CTAB), two-(2-ethylhexyl) succinate sodium sulfonate (AOT) or lauryl sodium sulfate (SDS).
In the cosmetics that contain colorant described in present embodiment, colorant is that azogeramine, alkali blue, sunset yellow, orange I, orange II, acid orange 7, alkaline purple 1, alkalescence are purple 2, solvent is green 7, rhodamine B, crystal violet, malachite green, methylenum careuleum, Yihong Huang, Indian yellow 73 or solvent green 3.
It is the surfactant phase that contains colorant that present embodiment obtains upper strata through centrifuging, and lower floor is the water that comprises cosmetics.
The lower floor that present embodiment stratification obtains is the larger organic solvent phase (organic solvent B phase) of polarity that contains colorant.
Principle: reverse micelle must just can form at the organic solvent less with the mutual exclusive polarity of water (as isooctane, normal hexane, cyclohexane, isopropyl alcohol or n-octyl alcohol), now the hydrophobic afterbody of surfactant is towards the organic solvent of outside, polar head is towards inside, and centre forms " core " of polarity.The topmost expulsive force of inverse micelle abstraction is the electrostatic attraction between positive and negative charge, thereby the material being extracted is all generally negative ion or cationic compound with electric charge.For convenient stratographic analysis below, colorant need to be stripped out.What strippant was selected is the organic solvent that polarity is larger (as methyl alcohol, ethanol or acetonitrile), and object is to improve the dissolving power of object.
Embodiment two: the difference of present embodiment and embodiment one is: the described cosmetics that contain colorant are lipstick, lipstick, eye shadow, rouge or muffin.Other are identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two difference is: described inorganic salts are potassium chloride, sodium chloride or sodium sulphate.Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three difference is: the cosmetics that 0.2g～0.5g is contained to colorant join in centrifuge tube A, then add 0.5g～1g surfactant and 5mL～15mL organic solvent A, being placed in ultrasonic oscillator, is under 50KHz～70KHz, to extract 4min～6min other are identical with embodiment one to three in ultrasonic frequency again.
Embodiment five: one of present embodiment and embodiment one to four difference is: add 5mL～15mL deionized water and 1g～4g inorganic salts, low whipping speed is to be stirred to and to mix under 2200r/min～2800r/min, is then placed in the centrifugal speed centrifugal 4min～6min of supercentrifuge with 4600r/min～5300r/min.Other are identical with embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five difference is: the upper strata liquid that centrifuging obtains is transferred in centrifuge tube B, add again 1mL～3mL organic solvent B, then be placed in shaking table, being 30～50 DEG C in temperature is the 9min～11min that strips under 220r/min～280r/min with shaking speed, stratification 2min～5min, the lower floor that stratification obtains adopts the membrane filtration of 0.45 μ m, the filtrate that filtration obtains adopts efficient liquid phase chromatographic analysis, completes and utilizes colorant in reverse micelle compartment analysis cosmetics.Other are identical with embodiment one to five.
Adopt following verification experimental verification effect of the present invention
Test one: a kind of method of utilizing reverse micelle compartment analysis eye shadow neutral and alkali purple 1, specifically completes according to the following steps:
The eye shadow that 0.3g is contained to alkaline purple 1 joins in centrifuge tube A, then add 0.8g bis--(2-ethylhexyl) succinate sodium sulfonate and 10mL isooctane, be placed in again ultrasonic oscillator, be to extract 5min under 40KHz in ultrasonic frequency, then add 10mL deionized water and 3g potassium chloride, low whipping speed is to be stirred to and to mix under 2500r/min, then be placed in the centrifugal 5min of centrifugal speed of supercentrifuge with 5000r/min, it is the surfactant phase that contains alkaline purple 1 that centrifuging obtains upper strata, lower floor is the water that comprises eye shadow, the surfactant phase transfer that alkaline purple 1 is contained on the upper strata that centrifuging is obtained is to centrifuge tube B, add again 2mL methyl alcohol, then be placed in shaking table, being 35 DEG C in temperature is the 10min that strips under 250r/min with shaking speed, stratification 2min～5min, the lower floor that stratification obtains is the methyl alcohol phase that contains alkaline purple 1, the methyl alcohol that alkaline purple 1 is contained in the lower floor that stratification obtains uses syringe with minute hand head by its sucking-off mutually, then adopt the membrane filtration of 0.45 μ m, the filtrate that filtration obtains is got 20 μ L and is carried out efficient liquid phase chromatographic analysis, complete and utilize reverse micelle compartment analysis eye shadow neutral and alkali purple 1.
The recovery of the eye shadow neutral and alkali purple 1 that in this test of table 1, analyzing and testing contains alkaline purple 1 and relative partially accurate deviation (RSD)
Can draw the recovery and relative partially accurate deviation (RSD) that under the horizontal different condition of mark-on, obtain by table one, can find out the recovery >90% of this experiment, thereby it be good to have good accuracy; RSD<6, thereby there is good precision.
Fig. 1 is the high-efficient liquid phase chromatogram of this test; The condition of high performance liquid chromatography is selected as follows:
Chromatographic column: HypersilODS2-C18 (4.6 × 150mm, 5 μ m), Dalian Yi Lite company
Mobile phase: acetonitrile: 0.5%H
3pO
4solution (80:20, v/v)
Flow velocity: 1.0mL/min
Column temperature: room temperature
Sample size: 20 μ L
Detect wavelength: 530nm
Under the chromatographic condition that can obtain using at us by Fig. 1, colorant alkaline purple 1 can be carried out chromatographic resolution well, and separates comparatively fast, and its retention time is 1.9min.
Claims (6)
1. utilize a method for colorant in reverse micelle compartment analysis cosmetics, it is characterized in that utilizing the method for colorant in reverse micelle compartment analysis cosmetics to complete according to the following steps:
The cosmetics that 0.2g～0.5g is contained to colorant join in centrifuge tube A, then add 0.5g～1g surfactant and 5mL～15mL organic solvent A, be placed in again ultrasonic oscillator, be to extract 3min～6min under 40KHz～80KHz in ultrasonic frequency, then add 5mL～15mL deionized water and 1g～4g inorganic salts, low whipping speed is to be stirred to and to mix under 2000r/min～3000r/min, then be placed in the centrifugal 4min～6min of centrifugal speed of supercentrifuge with 4500r/min～5500r/min, the upper strata liquid that centrifuging obtains is transferred in centrifuge tube B, add again 1mL～3mL organic solvent B, then be placed in shaking table, being 30～50 DEG C in temperature is the 8min～12min that strips under 200r/min～300r/min with shaking speed, stratification 2min～5min, the lower floor that stratification obtains adopts the membrane filtration of 0.45 μ m, the filtrate that filtration obtains adopts efficient liquid phase chromatographic analysis, complete and utilize colorant in reverse micelle compartment analysis cosmetics,
Described organic solvent A is isooctane, normal hexane, cyclohexane, isopropyl alcohol or n-octyl alcohol;
Described organic solvent B is methyl alcohol, ethanol or acetonitrile;
Described surfactant is cetab, two-(2-ethylhexyl) succinate sodium sulfonate or lauryl sodium sulfate.
2. a kind of method of utilizing colorant in reverse micelle compartment analysis cosmetics according to claim 1, is characterized in that the described cosmetics that contain colorant are lipstick, lipstick, eye shadow, rouge or muffin.
3. a kind of method of utilizing colorant in reverse micelle compartment analysis cosmetics according to claim 1, is characterized in that described inorganic salts are potassium chloride, sodium chloride or sodium sulphate.
4. a kind of method of utilizing colorant in reverse micelle compartment analysis cosmetics according to claim 1, it is characterized in that the cosmetics that 0.2g～0.5g is contained to colorant join in centrifuge tube A, then add 0.5g～1g surfactant and 5mL～15mL organic solvent A, being placed in ultrasonic oscillator, is to extract 4min～6min under 50KHz～70KHz in ultrasonic frequency again.
5. a kind of method of utilizing colorant in reverse micelle compartment analysis cosmetics according to claim 1, it is characterized in that adding 5mL～15mL deionized water and 1g～4g inorganic salts, low whipping speed is to be stirred to and to mix under 2200r/min～2800r/min, is then placed in the centrifugal speed centrifugal 4min～6min of supercentrifuge with 4600r/min～5300r/min.
6. a kind of method of utilizing colorant in reverse micelle compartment analysis cosmetics according to claim 1, it is characterized in that the upper strata liquid that centrifuging obtains is transferred in centrifuge tube B, add again 1mL～3mL organic solvent B, then be placed in shaking table, being 30～50 DEG C in temperature is the 9min～11min that strips under 220r/min～280r/min with shaking speed, stratification 2min～5min, the lower floor that stratification obtains adopts the membrane filtration of 0.45 μ m, the filtrate that filtration obtains adopts efficient liquid phase chromatographic analysis, complete and utilize colorant in reverse micelle compartment analysis cosmetics.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410289061.4A CN104020234A (en) | 2014-06-24 | 2014-06-24 | Method for separating and analyzing coloring agent in cosmetics by use of reverse micelle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410289061.4A CN104020234A (en) | 2014-06-24 | 2014-06-24 | Method for separating and analyzing coloring agent in cosmetics by use of reverse micelle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104020234A true CN104020234A (en) | 2014-09-03 |
Family
ID=51437105
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410289061.4A Pending CN104020234A (en) | 2014-06-24 | 2014-06-24 | Method for separating and analyzing coloring agent in cosmetics by use of reverse micelle |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104020234A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108508099A (en) * | 2017-02-23 | 2018-09-07 | 青岛谱尼测试有限公司 | The assay method of Unisol S-22 content in a kind of cosmetics |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130004716A1 (en) * | 2011-07-01 | 2013-01-03 | Samsung Electronics Co., Ltd. | Paste, method of preparing same, and electronic device |
-
2014
- 2014-06-24 CN CN201410289061.4A patent/CN104020234A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130004716A1 (en) * | 2011-07-01 | 2013-01-03 | Samsung Electronics Co., Ltd. | Paste, method of preparing same, and electronic device |
Non-Patent Citations (4)
| Title |
|---|
| MUSTAFA SOYLAK ET AL.: "Determination of rhodamine B in soft drink, waste water and lipstick samples after solid phase extraction", 《FOOD AND CHEMICAL TOXICOLOGY》, vol. 49, 31 December 2011 (2011-12-31) * |
| 刘海山 等: "高效液相色谱法同时测定化妆品中的10种合成着色剂", 《色谱》, vol. 31, no. 11, 30 November 2013 (2013-11-30), pages 1107 - 1111 * |
| 周子彦 等: "SEDSS/异辛烷/水反胶束体系对Cyt-C的提取", 《东北师大学报自然科学版》, vol. 33, no. 1, 31 March 2001 (2001-03-31) * |
| 孟凡涛 等: "新型阴离子表面活性剂的合成及其反胶束体系对cyt-C的提取", 《东北师大学报自然科学版》, vol. 34, no. 1, 31 March 2002 (2002-03-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108508099A (en) * | 2017-02-23 | 2018-09-07 | 青岛谱尼测试有限公司 | The assay method of Unisol S-22 content in a kind of cosmetics |
| CN108508099B (en) * | 2017-02-23 | 2021-06-08 | 广东悠质检测技术有限公司 | Method for measuring content of 3-benzylidene camphor in cosmetics |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103487524B (en) | HPLC (high performance liquid chromatography) method for determining ten synthetic colorants in cosmetic | |
| CN205153630U (en) | Take charging device's lifting and horizontal moving formula stereo garage | |
| Aman et al. | Determination of olanzapine by UV spectrophotometry and non-aquous titration | |
| CN103399102B (en) | Method for determining total solanesol in tobaccos and tobacco products | |
| CN101249425A (en) | Raw material prescription with hydrophile ion interchange and inphase opposition ion interchange separation mode chromatographic column and preparation | |
| CN109020973B (en) | A kind of fluorine-containing sulfimide spiro quaternary ammonium salt electrolyte, preparation method and the usage | |
| CN106048221A (en) | Method for extracting light rare earth elements in acidic solution by using ionic liquid [OMIM] BF4 | |
| CN104020234A (en) | Method for separating and analyzing coloring agent in cosmetics by use of reverse micelle | |
| CN106033826A (en) | Multi-rotary-wing unmanned aerial vehicle returning automatic charging method | |
| CN106433187A (en) | Organic dye based on tetrathienopyrrole as well as preparation method and application thereof | |
| CN101638722A (en) | Method for extracting and separating uranyl ions from aqueous phase | |
| CN101638721A (en) | Method for extracting and separating cesium ions from aqueous phase | |
| CN101381430A (en) | Molecule brand polymer of curcumin, preparation method and application thereof | |
| TWI443323B (en) | Method for analyzing phthalate esters | |
| CN103396512A (en) | Hybrid template molecularly imprinted polymer as well as preparation method and application of hybrid template molecularly imprinted solid-phase extraction column | |
| CN103134882B (en) | Assay method of metabolite of bergenin in animal body | |
| CN102600226A (en) | Method for extracting serrate clubmoss herb huperzia total alkali | |
| CN103589678A (en) | Method for extraction of Crassulaceae plant cell vacuoles | |
| Yang et al. | Orthogonal array optimization of ionic liquid based dispersive liquid-liquid microextraction for toxic anilines in foods | |
| CN103474721B (en) | A kind of LiFePO 4the recovery method of cell negative electrode material | |
| CN110501200B (en) | Method for extracting and separating effective components of recyclable black nightshade | |
| CN102911518B (en) | Method for refining gardenia yellow pigment through solvent extraction | |
| CN107525847B (en) | method for rapidly detecting forbidden colorant in crayon and water sticker | |
| CN105001076A (en) | Extraction separation method for methacrylic acid by using ionic liquid | |
| CN102775420A (en) | Method for extracting wedelia lactone by using microwave-assisted technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140903 |