CN105588871B - The rapid detection method of Sudan red dyes is disabled in a kind of eye shadow or muffin - Google Patents
The rapid detection method of Sudan red dyes is disabled in a kind of eye shadow or muffin Download PDFInfo
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- CN105588871B CN105588871B CN201610024215.6A CN201610024215A CN105588871B CN 105588871 B CN105588871 B CN 105588871B CN 201610024215 A CN201610024215 A CN 201610024215A CN 105588871 B CN105588871 B CN 105588871B
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- sudan red
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
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Abstract
The invention discloses the rapid detection method for disabling Sudan red dyes in a kind of eye shadow or muffin, include the following steps: that (1) makes triangle carrier；(2) it is loaded；(3) detection device is made；(4) it detects: the mixed solution of methylene chloride, ethyl alcohol and formic acid being added dropwise on the triangle carrier, 4.0kV voltage is applied to the metal crocodile clip using the high voltage power supply, the mixed solution extracts the disabling Sudan red dyes to be measured in the eye shadow or muffin sample, and then it is migrated on the triangle carrier to its tip direction, it is finally formed at tip by spraying, the ion trap mass spectrometer is detected using positive ion mode.The accurate quick detection of eye shadow or muffin sample may be implemented in the rapid detection method that Sudan red dyes are disabled in eye shadow or muffin of the present invention, and the apparatus structure used is simple, low in cost, easy to operate.
Description
Technical field
The present invention relates to cosmetics quality safety testing field, more particularly to disabling tonyred in a kind of eye shadow or muffin
The rapid detection method of dyestuff.
Background technique
Cosmetics are closely related with human lives, with Chinese national economy fast development and living standards of the people not
Disconnected to improve, cosmetics have become the indispensable necessity of daily life.According to national statistics office data, cosmetics in 2014
For the home sale total value of class commodity up to 1824.7 hundred million yuans, nearly 3 years average amplification is 13.4%.In face of conduct of making up
The high speed development of industry and cosmetics demand it is growing day by day, the product quality of cosmetics and safety are increasingly disappeared by vast
The concern and attention of the person of expense.Sudan red dyes are the disabling component of the cosmetics including eye shadow or muffin, but due to its color
Pool is bright-coloured, low in cost, its violation may be added in eye shadow or muffin product by some illegal producers, then may be to consumption
The healthy and safe of person causes to seriously endanger, therefore there is an urgent need to develop related detecting methods.
Summary of the invention
That the technical problem to be solved in the present invention is to provide a kind of structures is simple, at low cost, easy to operate, it is accurate to may be implemented
Detect the rapid detection method that Sudan red dyes are disabled in eye shadow or muffin.
The rapid detection method that Sudan red dyes are disabled in a kind of eye shadow or muffin, includes the following steps:
(1) make triangle carrier: the triangle carrier is using Whatman Grade 31ET Chr type chromatographic paper
The triangle scraps of paper being cut into；
(2) it is loaded: few drops of ethyl alcohol is added dropwise by the cotton parts complete wetting of the swab stick in swab stick front end with dropper, use institute
It states swab stick and dips eye shadow or muffin sample to be tested, and be uniformly applied on the triangle carrier；
(3) make detection device: the detection device includes metal crocodile clip, metal frame, high voltage power supply and ion trap matter
Spectrometer, the metal crocodile clip are fixed in the metal frame, are fixed on the metal in the middle part of the bottom edge of the triangle carrier
On crocodile clip, the rear end of the metal crocodile clip is connected with the high voltage power supply, and the triangle carrier is placed on the ion
At the mass spectrometric injection port front end of trap；
(4) it detects: the mixed solution of methylene chloride, ethyl alcohol and formic acid being added dropwise on the triangle carrier, using described
High voltage power supply applies 4.0kV voltage to the metal crocodile clip, the mixed solution in the eye shadow or muffin sample to
It surveys disabling Sudan red dyes to extract, and then is migrated on the triangle carrier to its tip direction, finally at tip
It is formed by spraying, the ion trap mass spectrometer is detected using positive ion mode.
The rapid detection method of Sudan red dyes is disabled in eye shadow or muffin of the present invention, wherein the mixing is molten
Liquid is made of methylene chloride, ethyl alcohol and the formic acid that volume ratio is 40:60:0.3, and dosage is 20 μ L.
The rapid detection method of Sudan red dyes is disabled in eye shadow or muffin of the present invention, wherein the smearing side
Formula are as follows: the eye shadow or muffin sample are uniformly smeared into a thin layer on the surface of the triangle carrier.
The rapid detection method of Sudan red dyes is disabled in eye shadow or muffin of the present invention, wherein the triangle
Carrier is isosceles triangle, and a length of 0.5cm in bottom edge, a height of 0.75cm, apex angle are 30 °.
The rapid detection method of Sudan red dyes is disabled in eye shadow or muffin of the present invention, wherein the ion trap
Mass spectrograph is small portable ion trap mass spectrometer.
In eye shadow or muffin of the present invention disable Sudan red dyes rapid detection method, wherein it is described it is small-sized just
Taking formula ion trap mass spectrometer is 12 type small portable rectangle linear ion trap mass spectrometer of Mini.
The rapid detection method of Sudan red dyes is disabled in eye shadow or muffin of the present invention, wherein the triangle
The distance between the tip of carrier and the injection port front end of the ion trap mass spectrometer are 5mm.
The rapid detection method of Sudan red dyes is disabled in eye shadow or muffin of the present invention, wherein the taboo to be measured
It is Sudan red 1, Sudan II, Sudan red III and Sudan IV with Sudan red dyes.
The rapid detection method of Sudan red dyes is disabled in eye shadow or muffin of the present invention, wherein the taboo to be measured
It is as shown in table 1 with the test condition of Sudan red dyes:
1 test condition of table
The rapid detection method of Sudan red dyes is disabled in eye shadow or muffin of the present invention, wherein the method is also
Preparation method including the positive eye shadow containing disabling Sudan red dyes or muffin sample, specifically comprise the following steps: to weigh through
Detection disables the eye shadow or muffin of Sudan red dyes without containing Sudan red 1, Sudan II, Sudan red III and 4 kinds of Sudan IV
Sample 1g is placed in a surface plate, and the concentration that the dichloromethane-ethanol mixed solution with volume ratio for 40:60 is prepared is added and is
The disabling Sudan red dyes mixed standard solution 2mL of 0.5mg/mL, is mixed evenly with glass bar, is placed in draught cupboard extremely
Solvent volatilizees completely completely, then is stirred evenly dried eye shadow or muffin matrix with glass bar, obtains containing the Sudan
Red I, Sudan II, Sudan red III and 4 kinds of Sudan IV disable the positive eye shadow or muffin sample of Sudan red dyes.
The rapid detection method difference from prior art that Sudan red dyes are disabled in eye shadow or muffin of the present invention is:
The rapid detection method that Sudan red dyes are disabled in eye shadow or muffin of the present invention uses Whatman Grade 31ET
The isosceles triangle scraps of paper that Chr type chromatographic paper is cut into are low in cost, easy to make as triangle carrier, and using by body
Product extracts the disabling Sudan red dyes in sample than the mixed solution for methylene chloride, ethyl alcohol and the formic acid composition for being 40:60:0.3,
Extraction effect is good, and detection sensitivity is high；The present invention uses triangle carrier, metal crocodile clip, metal clip, high voltage power supply and ion
Trap mass spectrograph combines to have obtained a set of device for quickly detecting, and detection quickly, accurately, is not necessarily to sample pre-treatments, in the several seconds
Operating process can be completed；The ion trap mass spectrometer that the present invention uses is small portable ion trap mass spectrometer, preferably Mini
12 type small portable rectangle linear ion trap mass spectrometers, are convenient for carrying and transport, it can be achieved that field quick detection.Miniature portable
The second order ms function of formula ion trap mass spectrometer can effectively improve the sensitivity and specificity of sample detection.
The rapid detection method that Sudan red dyes are disabled in eye shadow or muffin of the invention is made into one with reference to the accompanying drawing
Walk explanation.
Detailed description of the invention
Fig. 1 is two detected using the rapid detection method for disabling Sudan red dyes in eye shadow or muffin of the invention
Grade mass spectrogram.
Specific embodiment
One, detection method:
The rapid detection method that Sudan red dyes are disabled in a kind of eye shadow or muffin, includes the following steps:
(1) make triangle carrier: triangle carrier is to be cut out using Whatman Grade 31ET Chr type chromatographic paper
At the triangle scraps of paper；
(2) it is loaded: few drops of ethyl alcohol is added dropwise by the cotton parts complete wetting of the swab stick in swab stick front end with dropper, use institute
It states swab stick and dips eye shadow or muffin sample to be tested, and be uniformly applied on the triangle carrier；
(3) make detection device: detection device includes metal crocodile clip, metal frame, high voltage power supply and ion trap mass spectrometer,
Metal crocodile clip is fixed in metal frame, is fixed on metal crocodile clip in the middle part of the bottom edge of triangle carrier, metal crocodile clip
Rear end is connected with high voltage power supply, and triangle carrier is placed at the injection port front end of ion trap mass spectrometer；
(4) it detects: the mixed solution of methylene chloride, ethyl alcohol and formic acid being added dropwise on triangle carrier, using high voltage power supply
4.0kV voltage is applied to metal crocodile clip, mixed solution carries out the disabling Sudan red dyes to be measured in eye shadow or muffin sample
It extracts, and then is migrated on triangle carrier to its tip direction, finally form spraying, ion trap mass spectrometer use at tip
Positive ion mode detection.
Mixed solution is made of methylene chloride, ethyl alcohol and the formic acid that volume ratio is 40:60:0.3, and dosage is 20 μ L；It smears
Mode are as follows: few drops of ethyl alcohol are added dropwise in swab stick front end with dropper and soak cotton parts, eye shadow to be tested is dipped with the swab stick
Or muffin sample, eye shadow or muffin sample are uniformly smeared into a thin layer on the surface of triangle carrier, triangle carrier is etc.
Lumbar triangle shape, a length of 0.5cm in bottom edge, a height of 0.75cm, apex angle are 30 °.
Existing ion trap mass spectrometer can meet needs of the invention, such as: (the match of LTQ XL type ion trap mass spectrometer
Silent ThermoFisher Scientific Company).To meet the purpose for being convenient for carrying and transporting, and quickly detect, preferably small portable ion
Trap mass spectrograph, such as: 12 type small portable rectangle linear ion trap mass spectrometer (Qing Pu scientific & technical corporation) of Mini.
The distance between tip and the injection port front end of ion trap mass spectrometer of triangle carrier are 5mm.
Disabling Sudan red dyes to be measured are Sudan red 1, Sudan II, Sudan red III and Sudan IV, disabling the Sudan to be measured
The test condition of red dye is as shown in table 1:
1 test condition of table
Two, detection parameters:
Through detecting, precursor ion, product ion and the detection of above-mentioned 4 kinds of disablings Sudan red dyes in eye shadow or muffin sample
As shown in table 2, the second order ms figure detected is as shown in Figure 1: for limit
Precursor ion, product ion and the detection limit of 24 kinds of table disabling Sudan red dyes
Three, the preparation of positive eye shadow or muffin sample
It weighs through detection without containing 4 kinds of Sudan red 1, Sudan II, Sudan red III and Sudan IV disabling tonyred dyes
The eye shadow or muffin sample 1g of material, are placed in a surface plate, are added molten for the dichloromethane-ethanol mixing of 40:60 with volume ratio
The concentration that liquid is prepared is the disabling Sudan red dyes mixed standard solution 2mL of 0.5mg/mL, is mixed evenly, is put with glass bar
It is placed in draught cupboard to solvent and volatilizees completely completely, then stirred evenly dried eye shadow or muffin matrix with glass bar,
Obtain containing Sudan red 1, Sudan II, Sudan red III and 4 kinds of Sudan IV disabling Sudan red dyes positive eye shadow or
Muffin sample, for subsequent processes exploitation and condition optimizing.
Four, condition optimizing explanation
A series of test effect of solvents as migration and spraying solvent: n-hexane, tetrahydro furan has been investigated in research respectively
It mutters, ethyl acetate, chloroform, methylene chloride, acetone, acetonitrile, isopropanol, ethyl alcohol, first alcohol and water.In spray voltage 4.0kV condition
Under, the experimental results showed that, the effect of methylene chloride and ethyl alcohol is best.Methylene chloride and ethyl alcohol different proportion item are further investigated
The test effect of part, the results showed that when the volume ratio of methylene chloride and ethyl alcohol is 40:60, signal strength highest.In addition, just
Under ion detection mode, adding certain density formic acid facilitates promotion signal intensity, has investigated formic acid concn by 0.1% variation
To 2.0%, wherein when formic acid concn is 0.3%, signal strength highest.
In addition to the optimization to migration and spraying solvent, the test effect using different paper bases is also compared, comprising: cellulose
Chromatographic paper (1 Chr of Whatman Grade, Whatman Grade 3MM Chr, Whatman Grade 4 Chr, Whatman
Grade 31ET Chr) and ion exchange paper (Whatman Grade SG81).To sum up pass through series of optimum, it is final to determine in fact
Test condition are as follows: Whatman Grade 31ET Chr chromatographic paper, migration and spraying solvent are methylene chloride: ethyl alcohol: formic acid (volume
Than 40:60:0.3), spray voltage 4.0kV.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (4)
1. disabling the rapid detection method of Sudan red dyes in a kind of eye shadow or muffin, characterized by the following steps:
(1) make triangle carrier: the triangle carrier is to be cut out using Whatman Grade 31ET Chr type chromatographic paper
At the triangle scraps of paper；The triangle carrier is isosceles triangle, and a length of 0.5cm in bottom edge, a height of 0.75cm, apex angle are 30 °；
(2) it is loaded: few drops of ethyl alcohol is added dropwise by the cotton parts complete wetting of the swab stick, with the cotton in swab stick front end with dropper
Stick dips eye shadow or muffin sample to be tested, and is uniformly applied on the triangle carrier；
(3) make detection device: the detection device includes metal crocodile clip, metal frame, high voltage power supply and ion trap mass spectrometer,
The metal crocodile clip is fixed in the metal frame, is fixed on the metal crocodile clip in the middle part of the bottom edge of the triangle carrier
On, the rear end of the metal crocodile clip is connected with the high voltage power supply, and the triangle carrier is placed on the ion trap mass spectrometry
At the injection port front end of instrument；The tip of the triangle carrier and the distance between the injection port front end of the ion trap mass spectrometer
For 5mm；
(4) it detects: the mixed solution of methylene chloride, ethyl alcohol and formic acid being added dropwise on the triangle carrier, using the high pressure
Power supply applies 4.0kV voltage to the metal crocodile clip, and the mixed solution is to the taboo to be measured in the eye shadow or muffin sample
It is extracted with Sudan red dyes, and then is migrated on the triangle carrier to its tip direction, finally formed at tip
Spraying, the ion trap mass spectrometer is detected using positive ion mode；The disabling Sudan red dyes to be measured are Sudan red 1, the Sudan
Red II, Sudan red III and Sudan IV；
The test condition of the disabling Sudan red dyes to be measured is as shown in table 1:
1 test condition of table
The mixed solution is made of methylene chloride, ethyl alcohol and the formic acid that volume ratio is 40:60:0.3, and dosage is 20 μ L；
The method also includes containing disabling Sudan red dyes positive eye shadow or muffin sample preparation method, specifically include as
Lower step: it weighs through detection without containing Sudan red 1,4 kinds of Sudan II, Sudan red III and Sudan IV disabling Sudan red dyes
Eye shadow or muffin sample 1g, be placed in a surface plate, being added with volume ratio is the dichloromethane-ethanol mixed solution of 40:60
The concentration of preparation is the disabling Sudan red dyes mixed standard solution 2mL of 0.5mg/mL, is mixed evenly with glass bar, is placed
It volatilizees completely in draught cupboard to solvent, then is stirred evenly dried eye shadow or muffin matrix completely with glass bar, i.e.,
The positive eye shadow or powder that Sudan red dyes are disabled containing Sudan red 1, Sudan II, Sudan red III and 4 kinds of Sudan IV is made
Cake sample.
2. disabling the rapid detection method of Sudan red dyes in eye shadow according to claim 1 or muffin, it is characterised in that:
The smearing mode are as follows: the eye shadow or muffin sample are uniformly smeared into a thin layer on the surface of the triangle carrier.
3. disabling the rapid detection method of Sudan red dyes in eye shadow according to claim 1 or muffin, it is characterised in that:
The ion trap mass spectrometer is small portable ion trap mass spectrometer.
4. disabling the rapid detection method of Sudan red dyes in eye shadow according to claim 3 or muffin, it is characterised in that:
The small portable ion trap mass spectrometer is 12 type small portable rectangle linear ion trap mass spectrometer of Mini.
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| CN201610024215.6A CN105588871B (en) | 2016-01-14 | 2016-01-14 | The rapid detection method of Sudan red dyes is disabled in a kind of eye shadow or muffin |
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| CN201610024215.6A CN105588871B (en) | 2016-01-14 | 2016-01-14 | The rapid detection method of Sudan red dyes is disabled in a kind of eye shadow or muffin |
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| CN107543857B (en) * | 2017-03-22 | 2020-07-07 | 中国检验检疫科学研究院 | Rapid screening method for 14 sensitizing carcinogenic dyes in toy |
| CN107085069A (en) * | 2017-05-12 | 2017-08-22 | 辽宁大学 | A kind of thin-layer sample application method for being used to prepare thin-layer chromatography |
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