CN104374754A - Method for detecting content of lemon yellow in beverage sample - Google Patents
Method for detecting content of lemon yellow in beverage sample Download PDFInfo
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- CN104374754A CN104374754A CN201410427037.2A CN201410427037A CN104374754A CN 104374754 A CN104374754 A CN 104374754A CN 201410427037 A CN201410427037 A CN 201410427037A CN 104374754 A CN104374754 A CN 104374754A
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Abstract
The invention discloses a method for detecting the content of lemon yellow in a beverage sample. By excitation of isatin p-phenylene diamine dischiff base with 386nm wavelength, a maximum fluorescence emission peak is shown at 483nm, after addition of nano graphene oxide suspension liquid into an isatin p-phenylene diamine dischiff base solution, the fluorescence intensity decreases linearly, after addition of the lemon yellow in the isatin p-phenylene diamine dischiff base solution, the isatin p-phenylene diamine dischiff base fluorescence intensity enhances, the fluorescence intensity change shows that the nano graphene oxide (rGO) and the lemon yellow (Tz) can be used as an isatin p-phenylene diamine dischiff base fluorescent molecule switch group, and a method for rapidly detecting the content of the lemon yellow by an isatin p-phenylene diamine dischiff base-graphene oxide fluorescent sensor is established. The experimental results show that when the lemon yellow concentration is in the range of 8.58ng / L to 327ng / L, the fluorescent intensity (F) has a good linear relationship with the lemon yellow solution concentration, the calculated linear regression equation is F = 0.4454CTz-2.9562, R = 0.991, and the detection limit is 0.34ng / L. The method has good precision and accuracy.
Description
Technical field
The present invention relates to a kind of method detecting content of tartrazine based on isatin Bis-Schiff Bases-graphene oxide fluorescent optical sensor fast, particularly detect the method for content of tartrazine in drink sample.
Background technology
Lemon yellow (Tz) is a kind of azo acid dye of Prof. Du Yucang, have another name called tartrazines, main application can be used as the colorant of beverage, food, medicine and daily cosmetics, China allows the secondary colour used to have amaranth, famille rose, sunset yellow, lemon yellow and indigo in food service industry, and it is color etc. on the surface that they can be used for beverage, jelly, ice cream, can and cake.This type of synthetic dyestuff can improve the sensory properties of food, but use amount must meet country's " food additives use hygienic standard ".The food that the synthetic food colors such as excessive Tatrazine exceed standard, can produce certain injury to health.In order to ensure the health diet of people, what develop that easy, to detect harmful food additives fast and effectively content seems very in time is important.The method of detection lemon yellow conventional at present has high performance liquid chromatography (HPLC), spectrophotometric method, polarography and microtrabeculae method, electrochemical process, fluorescence spectrum analysing method etc.
Graphene oxide (graphene oxide, rGO) surface uniform be dispersed with a large amount of carboxyls and hydroxyl, graphene oxide (rGO) is a kind of novel nano material, and the physical chemistry of its uniqueness and optical property, the application in fluorescent optical sensor is very extensive.
Based on graphene oxide to the fluorophor (conjugated system) containing generation fluorescence in the quenching effect of fluorescence and isatin Bis-Schiff Bases structural molecule, and schiff bases, adsorption and desorption effect between lemon yellow and graphene oxide can be changed mutually, the photoluminescent property of the present invention to isatin Bis-Schiff Bases conducts in-depth research, inquire into the possibility that isatin Bis-Schiff Bases and graphene oxide build fluorescent optical sensor, establish the method detecting content of tartrazine based on isatin Bis-Schiff Bases-graphene oxide fluorescent optical sensor fast accordingly.
Summary of the invention
The object of the present invention is to provide a kind of method detecting content of tartrazine in drink sample.
The present invention detects the principle of content of tartrazine: graphene oxide is a kind of very effective fluorescence quenching to organic compound.Excite with 386nm wavelength, maximum fluorescence emission peak has been there is in isatin contracting p-phenylenediamine (PPD) Bis-Schiff Bases at 483nm place, find after add a certain amount of nano graphene oxide suspending liquid in isatin contracting p-phenylenediamine (PPD) Bis-Schiff Bases, its fluorescence intensity straight line declines, this is because graphene oxide has caused by fluorescent quenching effect, after adding a certain amount of lemon yellow to above-mentioned solution, the fluorescence intensity of isatin contracting p-phenylenediamine (PPD) Bis-Schiff Bases strengthens again, this is because the suction-operated of lemon yellow and nano graphene oxide (rGO) is greater than adsorption between isatin contracting p-phenylenediamine (PPD) Bis-Schiff Bases and (rGO), isatin contracting p-phenylenediamine (PPD) Bis-Schiff Bases is got off by from nano graphene oxide (rGO) surface desorption, this also illustrates that nano graphene oxide (rGO) and lemon yellow (Tz) can as the role in fluorescent molecule switch groups of isatin contracting p-phenylenediamine (PPD) Bis-Schiff Bases simultaneously, establish the new method that isatin Bis-Schiff Bases-graphene oxide fluorescent optical sensor detects content of tartrazine fast accordingly.
The present invention is investigated the selectivity that isatin Bis-Schiff Bases-graphene oxide fluorescent optical sensor measures lemon yellow, select adjuvant common in food, for 151.41ng/mL lemon yellow, relative error controls to test ± 5%, and result shows: glucose, Sodium Benzoate, sucrose, fructose, citric acid, sodium citrate, the KI of 100 times; The Cacl of 10 times
2, Nacl, NaH
2pO
4; The carboxymethyl cellulose of 1 times; Do not disturb the test of lemon yellow concentration, result shows that isatin Bis-Schiff Bases-graphene oxide fluorescent optical sensor has good selectivity to lemon yellow.
Concrete steps are:
(1) accurately take 0.0122g isatin contracting p-phenylenediamine (PPD) Bis-Schiff Bases and be dissolved in 10mLN, in dinethylformamide (DMF) solvent, with ultrapure water dilution, be configured to the solution of 122ng/mL.
(2) accurately take 0.0532g nano graphene oxide (rGO) be dissolved in 5mL ultrapure water after constant volume in 10mL volumetric flask, obtain the nano graphene oxide stock suspensions that concentration is 5.32mg/mL, In Shade preservation is stand-by, and the used time is diluted to the solution of variable concentrations.
(3) by the concentration of step (2) gained be 5.32mg/mL nano graphene oxide stock suspensions dilution be mixed with the nano graphene oxide suspending liquid that concentration is 2.66 μ g/mL.
(4) in a 10mL tool plug test tube, add the nano graphene oxide suspending liquid that 2mL step (1) gained solution and 2mL step (3) gained concentration are 2.66 μ g/mL, fully shake up, obtain mixed solution.
(5) in step (4) gained mixed solution, add the lemon yellow solution that 2mL concentration is 8.58ng/L ~ 327ng/L respectively, after mixing, respectively get this solution appropriate in 10mm cuvette, at ambient temperature, control slit width and be 5.0, excitation wavelength and emission wavelength lambda ex/ λ em=386nm/483nm, measure its fluorescence intensity (F) respectively, when result shows that lemon yellow concentration is within the scope of 8.58ng/L ~ 327ng/L, fluorescence intensity (F) has good linear relationship with the concentration of lemon yellow solution, its equation of linear regression calculated is F=0.4454C
tz-2.9562, R=0.991, detect and be limited to 0.34ng/L.
(6) CO in removing beverage is boiled in heating
2accurately measure this beverage 5.00mL, be settled to 50mL with ultrapure water, then this solution is joined in step (4) gained mixed solution, get this mixed solution appropriate in 10mm cuvette, at ambient temperature, control slit width and be 5.0, excitation wavelength and emission wavelength lambda ex/ λ em=386nm/483nm, measure its fluorescence intensity (F), substitute into the equation of linear regression in step (5), calculate the concentration of lemon yellow and the content of lemon yellow in drink sample.
Preci-sion and accuracy of the present invention is all better.
Accompanying drawing explanation
Fig. 1 is working curve diagram of the present invention.
Embodiment
Embodiment:
(1) accurately take 0.0122g isatin contracting p-phenylenediamine (PPD) Bis-Schiff Bases and be dissolved in 10mLN, in dinethylformamide (DMF) solvent, with ultrapure water dilution, be configured to the solution of 122ng/mL.
(2) accurately take 0.0532g nano graphene oxide (rGO) be dissolved in 5mL ultrapure water after constant volume in 10mL volumetric flask, obtain the nano graphene oxide stock suspensions that concentration is 5.32mg/mL, In Shade preservation is stand-by, and the used time is diluted to the solution of variable concentrations.
(3) by the concentration of step (2) gained be 5.32mg/mL nano graphene oxide stock suspensions dilution be mixed with the nano graphene oxide suspending liquid that concentration is 2.66 μ g/mL.
(4) in a 10mL tool plug test tube, add the nano graphene oxide suspending liquid that 2mL step (1) gained solution and 2mL step (3) gained concentration are 2.66 μ g/mL, fully shake up, obtain mixed solution.
(5) in step (4) gained mixed solution, add the lemon yellow solution that 2mL concentration is 8.58ng/L ~ 327ng/L respectively, after mixing, respectively get this solution appropriate in 10mm cuvette, at ambient temperature, control slit width and be 5.0, excitation wavelength and emission wavelength lambda ex/ λ em=386nm/483nm, measure its fluorescence intensity (F) respectively, when result shows that lemon yellow concentration is within the scope of 8.58ng/L ~ 327ng/L, fluorescence intensity (F) has good linear relationship (see figure 1) with the concentration of lemon yellow solution, its equation of linear regression calculated is F=0.4454C
tz-2.9562, R=0.991, detect and be limited to 0.34ng/L.
(6) beverage of four kinds of different brands is selected to carry out sample analysis.Respectively the beverage heating of four kinds of different brands is boiled removing CO
2accurately measure each beverage 5.00mL respectively, be settled to 50mL with ultrapure water respectively, then add the mixed solution of step (4) gained respectively, after mixing, at ambient temperature, control slit width and be 5.0, excitation wavelength and emission wavelength lambda ex/ λ em=386nm/483nm, measure the maximum fluorescence emission peak value of 50mL solution respectively, substitute into step (5) gained equation of linear regression, calculate the content of lemon yellow in the concentration of lemon yellow and drink sample in table 1.
Respectively to adding 200-400 μ g standard lemon yellow solution in each 50.00mL of beverage of four kinds of different brands, carry out recovery testu, result shows that in these four kinds of beverages, content of tartrazine meets food additives hygienic standard, the results are shown in Table 1.Relative standard deviation RSD is at 2.07%-4.66%, and recovery of standard addition, between 90.50% ~ 98.97%, shows that the preci-sion and accuracy of this method is better.
Table 1: the test result of content of tartrazine in beverage
Claims (1)
1. detect a method for content of tartrazine in drink sample, it is characterized in that concrete steps are:
(1) accurately take 0.0122g isatin contracting p-phenylenediamine (PPD) Bis-Schiff Bases and be dissolved in 10mLN, in dinethylformamide solvent, with ultrapure water dilution, be configured to the solution of 122ng/mL;
(2) accurately take 0.0532g nano graphene oxide be dissolved in 5mL ultrapure water after constant volume in 10mL volumetric flask, obtaining concentration is the nano graphene oxide stock suspensions of 5.32mg/mL, and In Shade preservation is stand-by, and the used time is diluted to the solution of variable concentrations;
(3) by the concentration of step (2) gained be 5.32mg/mL nano graphene oxide stock suspensions dilution be mixed with the nano graphene oxide suspending liquid that concentration is 2.66 μ g/mL;
(4) in a 10mL tool plug test tube, add the nano graphene oxide suspending liquid that 2mL step (1) gained solution and 2mL step (3) gained concentration are 2.66 μ g/mL, fully shake up, obtain mixed solution;
(5) in step (4) gained mixed solution, add the lemon yellow solution that 2mL concentration is 8.58ng/L ~ 327ng/L respectively, after mixing, respectively get this solution appropriate in 10mm cuvette, at ambient temperature, control slit width and be 5.0, excitation wavelength and emission wavelength lambda ex/ λ em=386nm/483nm, measure its fluorescence intensity F respectively, when result shows that lemon yellow concentration is within the scope of 8.58ng/L ~ 327ng/L, the concentration of fluorescence intensity F and lemon yellow solution has good linear relationship, its equation of linear regression calculated is F=0.4454C
tz-2.9562, R=0.991, detect and be limited to 0.34ng/L,
(6) CO in removing beverage is boiled in heating
2accurately measure this beverage 5.00mL, be settled to 50mL with ultrapure water, then this solution is joined in step (4) gained mixed solution, get this mixed solution appropriate in 10mm cuvette, at ambient temperature, control slit width and be 5.0, excitation wavelength and emission wavelength lambda ex/ λ em=386nm/483nm, measure its fluorescence intensity F, substitute into the equation of linear regression in step (5), calculate the concentration of lemon yellow and the content of lemon yellow in drink sample.
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Cited By (2)
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| CN105651753A (en) * | 2016-03-01 | 2016-06-08 | 上海应用技术学院 | Graphene oxide fluorescent sensor and preparation method and application thereof |
| CN106290341A (en) * | 2016-09-14 | 2017-01-04 | 郑州欧柯奇仪器制造有限公司 | Tea polyphenols method for quick in tea beverage |
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