CN103308612A - Method for rapidly detecting contents of lemon yellow and sunset yellow in food - Google Patents
Method for rapidly detecting contents of lemon yellow and sunset yellow in food Download PDFInfo
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- CN103308612A CN103308612A CN2013101958371A CN201310195837A CN103308612A CN 103308612 A CN103308612 A CN 103308612A CN 2013101958371 A CN2013101958371 A CN 2013101958371A CN 201310195837 A CN201310195837 A CN 201310195837A CN 103308612 A CN103308612 A CN 103308612A
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Abstract
The invention discloses a method for rapidly detecting contents of lemon yellow and sunset yellow in a food. The method comprises the following steps of: preparing a standard solution of the lemon yellow and the sunset yellow; measuring the peak area of the standard solution of the pigments by using high performance liquid chromatography, and drawing a standard curve to obtain an equation of linear regression; filtering a liquid food sample or solid food sample solution, extracting by using an ionic liquid aqueous two-phase system composed of 1-butyl-3-methylimidzaole bromine salt and K2HPO4, and directly carrying out high performance liquid chromatography analysis on an ionic liquid after phase splitting; and respectively calculating the contents of the lemon yellow and the sunset yellow in the food according to the equation of linear regression. The method disclosed by the invention is simple in operation, free of a great deal of volatile solvents, short in separation time, good in ionic liquid phase mobility and capable of inter-dissolving with water or methanol and directly injecting for chromatography analysis. By using the method, the rapid, simple, convenient, environment-friendly, economic, qualitative and quantitative measurement can be provided for quality control departments and production enterprises.
Description
Technical field
The present invention relates to a kind of method of high-efficient liquid phase chromatogram determining content, particularly the lemon yellow in a kind of fast detecting food and the method for sunset yellow content belong to food security adjuvant detection technique field.
Background technology
Because wantonly discharge the sanitary wastewater that is rich in the elements such as carbon, nitrogen and phosphorus in natural water, these elements finally can cause the eutrophication of water body by the enrichment effect.At present, the processing for life, municipal wastewater has had a large amount of research.Wherein, the removal of phosphorus research is started late, until 20th century eight, the nineties just begin it is studied.Lemon yellow, water-soluble synthetic dyestuff, bright-coloured bright yellow.Sunset yellow has another name called yellow, orange, edible yellow No. 3 of sunset yellow, the setting sun.These two kinds of pigments can be used for the painted of food, beverage, medicine, cosmetics, feed, tobacco, toy, packaging material for food etc. safely.Have the researcher to find that there is certain insecurity in such food coloring or produces illeffects human body, although the harmfulness of edible synthesized coloring matter final conclusion not still, they are without any nutritive value, to health also without any help.In recent years, a lot of illegal retailers are profit-push, add excessive food coloring in the food or carry out the illegal act such as yellow croaker frauds with pigment, for this kind situation, various countries hygiene department is all with the behavior of use edible synthesized coloring matter in the formal Specification food production of laws and regulations.Because 1-butyl-the water-soluble and methyl alcohol of 3-methylimidazole bromine salt energy is therefore ion liquid abstraction can directly carry out stratographic analysis mutually;
The subject matter that affects at present the pigment additive mensuration in the food is the interference that has multiple pigment and other related substanceses in the sample, addition is less in some food samples simultaneously, also need sample is carried out measuring after the enrichment, so the preenrichment technology is usually used in the compartment analysis of synthetic food color.
Tend to use volatile organic compounds in the preprocessing process of traditional analytic sample, exist simultaneously bioaccumulation efficiency low, poor selectivity is easily introduced the impurity of matrix, and sample is difficult to obtain the problems such as purifying, and solvent itself can cause secondary pollution again simultaneously.Therefore study novel, green replace solvents---ionic liquid, inquire into character, the mechanism and use of its extract and separate pigment, no matter be for ensuring food safety or reduce volatile organic matter and pollute, very important meaning being arranged.
Summary of the invention
Technical matters to be solved by this invention is for the deficiencies in the prior art, provide a kind of fast, accurately, the intuitively lemon yellow in the fast detecting food of quantitative and qualitative analysis and the method for sunset yellow content.
Technical matters to be solved by this invention is to realize by following technical scheme.The present invention is lemon yellow in a kind of fast detecting food and the method for sunset yellow content, and be characterized in: the step of the method is as follows:
(1) making of working curve: adopt the stepwise dilution method that lemon yellow and the sunset yellow standard solution that concentration is 500mg/mL is mixed with lemon yellow and the sunset yellow standard solution of a series of solution concentrations in 0.05 μ g/mL～50.0 μ g/mL scopes; With the peak area of each concentration standard solution more than the high-performance liquid chromatogram determination, the drawing standard curve obtains equation of linear regression;
(2) sample preparation: food samples is fluid sample or solid sample, adopts respectively following methods to process:
Fluid sample: get sample that the 2.0mL suction filtration crosses in the 10mL centrifuge tube, add 0.3mL1-butyl-3-methylimidazole bromine salt, be settled to 4mL, add 3.4gK
2HPO
4, vibration is to fully dissolving, and the centrifugal 2～3min of 3000r/min forms aqueous two-phase, gets mutually 20 μ L of ionic liquid, directly advances look capable analysis of spectrum;
Solid sample: take by weighing the 2.0-5.0g solid food,, use the 10-20mL dissolved in distilled water, get this solution of 3.0mL to 10mL tool plug centrifuge tube, add 0.3mL1-butyl-3-methylimidazole bromine salt, be diluted to 4mL, add 3.4g K
2HPO
4, vibration is to fully dissolving, and the centrifugal 2～3min of 3000r/min forms aqueous two-phase, gets mutually 20 μ L of ionic liquid, directly advances look capable analysis of spectrum;
(3) the fluid sample solution in the step (2) or solid sample solution are carried out efficient liquid phase chromatographic analysis;
High-efficient liquid phase chromatogram condition: chromatographic column: Zorbax ODS, internal diameter 4.6mm * column length 150mm * particle diameter 5 μ m; Column temperature: 30 ℃; Ultraviolet detects wavelength: it is 410 nm that lemon yellow detects wavelength, and it is 480nm that sunset yellow detects wavelength; Flow velocity: 1.0mL/min; Mobile phase: add the 2mL acetic acid solutions in the 0.02mol/L ammonium acetate solution and become the acetic acid of pH=4.5-ammonium acetate buffer A; B is methyl alcohol; Mobile phase B is by 15% even variation to 40% in gradient: 0～5min, and Mobile phase B is by 40% even variation to 98% in 5～10min, and Mobile phase B is by 98% even variation to 15% in 10～15min; The sample solution sample volume is 20 μ L;
(4) according to the equation of linear regression of step (1), calculate respectively the content of lemon yellow and sunset yellow in the food.
Compared with prior art, advantage of the present invention is mainly reflected in:
1, the inventive method uses ionic liquid/salt two phase aqueous extraction system as the pre-treating method of example enrichment, and this method has the advantages such as the phase-splitting time is short, viscosity is low, extraction process is difficult for emulsification, ionic liquid can be recycled.
2, lemon yellow and sunset yellow in the inventive method ionic liquid aqueous two-phase extraction-food by HPLC, simple to operate, need not use a large amount of volatile solvents, disengaging time is short, ionic liquid phase good fluidity, can dissolve each other with water or methyl alcohol, but direct injected is carried out stratographic analysis, can be quality testing department and manufacturing enterprise quick, easy, environmental protection, economic lemon yellow and sunset yellow quantitative and qualitative analysis mensuration are provided.
Embodiment
Below by example the present invention is further described, but protection scope of the present invention is not limited to this.
Embodiment 1, the lemon yellow in a kind of fast detecting food and the method for sunset yellow content, and the step of the method is as follows:
(1) making of working curve: adopt the stepwise dilution method that lemon yellow and the sunset yellow standard solution that concentration is 500mg/mL is mixed with lemon yellow and the sunset yellow standard solution of a series of solution concentrations in 0.05 μ g/mL～50.0 μ g/mL scopes; With the peak area of each concentration standard solution more than the high-performance liquid chromatogram determination, the drawing standard curve obtains equation of linear regression, and measurement result sees Table 1.
Table 1 method parameter
| Analyte | Percentage extraction | Equation of linear regression | The range of linearity (μ g/mL) | Detection limit (μ g/mL) | Relative standard deviation |
| Sunset yellow | 98.91% | Y=707.74x(μg/mL)+56.03(480nm) | 0.05-50.0 | 0.011 | 0.80 |
| Lemon yellow | 99.24% | Y=264.46x(μg/mL)+21.24(410nm) | 0.05-50.0 | 0.002 | 0.31 |
(2) sample preparation: food samples is fluid sample or solid sample, adopts respectively following methods to process:
Fluid sample: get sample that the 2.0mL suction filtration crosses in the 10mL centrifuge tube, add 0.3mL1-butyl-3-methylimidazole bromine salt, be settled to 4mL, add 3.1-4.0g K
2HPO
4, vibration is to fully dissolving, and the centrifugal 2-3min of 2000-3000r/min forms aqueous two-phase, gets mutually 20 μ L of ionic liquid, directly advances look capable analysis of spectrum;
Solid sample: take by weighing the 2.0-5.0g solid food,, use the 10-20mL dissolved in distilled water, get this solution of 3.0mL to 10mL tool plug centrifuge tube, add 0.3mL1-butyl-3-methylimidazole bromine salt, be diluted to 4mL, add 3.1-4.0g K
2HPO
4, vibration is to fully dissolving, and the centrifugal 2-3min of 2000-3000r/min forms aqueous two-phase, gets mutually 20 μ L of ionic liquid, directly advances look capable analysis of spectrum; (3) the fluid sample solution in the step (2) or solid sample solution are carried out efficient liquid phase chromatographic analysis;
(3) high-efficient liquid phase chromatogram condition: chromatographic column: Zorbax ODS, internal diameter 4.6mm * column length 150mm * particle diameter 5 μ m; Column temperature: 30 ℃; Ultraviolet detects wavelength: it is 410 nm that lemon yellow detects wavelength, and it is 480nm that sunset yellow detects wavelength; Flow velocity: 1.0mL/min; Mobile phase: add the 2mL acetic acid solutions in the 0.02mol/L ammonium acetate solution and become the acetic acid of pH=4.5-ammonium acetate buffer A; B is methyl alcohol; Mobile phase B is by 15% even variation to 40% in gradient: 0～5min, and Mobile phase B is by 40% even variation to 98% in 5～10min, and Mobile phase B is by 98% even variation to 15% in 10～15min; The sample solution sample volume is 20 μ L;
(4) according to the equation of linear regression of step (1), calculate respectively the content of lemon yellow and sunset yellow in the food.
Embodiment 2, the method for the content of tartrazine in a kind of fast detecting large yellow croaker, and the step of the method is as follows:
1, working curve is made: method is with method in example 1 step 1.
2, sample preparation:
The large yellow croaker entity of lemon yellow dyeing is cleaned, added distilled water and carry out ultrasonic extraction once, extraction time is 10-30 minute, and extracting temperature is 30 ℃; Extract and finish namely to get the large yellow croaker test solution by directly injecting sample injection bottle behind the 0.45 μ m filtering with microporous membrane;
Get 3.00ml large yellow croaker test liquid in 10mL tool plug centrifuge tube, add 0.3mL 1-butyl-3-methylimidazole bromine salt, to the 4mL scale, add 3.5g K with distilled water diluting
2HPO
4, vibration is to fully dissolving, and the centrifugal 2-3min of 2000-3000r/min forms aqueous two-phase, gets mutually 20 μ L of ionic liquid, directly advances look capable analysis of spectrum; , according to the working curve that table 1 obtains, calculate that content of tartrazine is respectively 1.42 μ g/mL in the dyeing large yellow croaker extract.
Embodiment 3, the lemon yellow in a kind of fast detecting orange flavor soda and the method for sunset yellow content, and the step of the method is as follows:
1, working curve is made: method is with method in example 1 step 1.
2, sample preparation
Get 3.00mL board orange flavour beverage in 10mL tool plug centrifuge tube, Ultrasonic Heating 10min removes CO
2, adding 0.3mL, 1-butyl-3-methylimidazole bromine salt to the 4mL scale, adds 3.5g K with distilled water diluting
2HPO
4Vibration is to fully dissolving, the centrifugal 2-3min of 2000-3000r/min, form aqueous two-phase, get mutually 20 μ L of ionic liquid, directly advance look capable analysis of spectrum, according to the working curve that table 1 obtains, calculate that the content of lemon yellow and sunset yellow is respectively 1.46 μ g/g and 17.68 μ g/g in certain board orange flavour beverage.
Embodiment 4, the lemon yellow in a kind of fast detecting orange flavor peppermint candy and the method for sunset yellow content, and the step of the method is as follows:
1, working curve is made: method is with method in example 1 step 1.
2, sample preparation
Get the 5.000g peppermint candy, behind the 10mL dissolved in distilled water, pipette this solution 3.0mL in 10mL tool plug centrifuge tube, add 0.3mL 1-butyl-3-methylimidazole bromine salt, to scale, add 3.5g K with distilled water diluting
2HPO
4, vibration is to fully dissolving, the centrifugal 2-3min of 2000-3000r/min, form aqueous two-phase, get mutually 20 μ L of ionic liquid, directly advance look capable analysis of spectrum, according to the working curve that obtains in the step 1, calculate that the content of sunset yellow is respectively ug/g0.059 μ g/g in the peppermint candy, sunset yellow does not detect.
Claims (1)
1. the lemon yellow in the fast detecting food and the method for sunset yellow content, it is characterized in that: the step of the method is as follows:
(1) making of working curve: adopt the stepwise dilution method that lemon yellow and the sunset yellow standard solution that concentration is 500mg/mL is mixed with lemon yellow and the sunset yellow standard solution of a series of solution concentrations in 0.05 μ g/mL～50.0 μ g/mL scopes; With the peak area of each concentration standard solution more than the high-performance liquid chromatogram determination, the drawing standard curve obtains equation of linear regression;
(2) sample preparation: food samples is fluid sample or solid sample, adopts respectively following methods to process:
Fluid sample: get sample that the 2.0mL suction filtration crosses in the 10mL centrifuge tube, add 0.3mL1-butyl-3-methylimidazole bromine salt, be settled to 4mL, add 3.6g K
2HPO
4, vibration is to fully dissolving, and the centrifugal 2～3min of 3000r/min forms aqueous two-phase, gets mutually 20 μ L of ionic liquid, directly carries out stratographic analysis;
Solid sample: take by weighing the 2.0-5.0g solid food, use the 10-20mL dissolved in distilled water, get this solution of 3.0mL to 10mL tool plug centrifuge tube, add 0.3mL1-butyl-3-methylimidazole bromine salt, be diluted to 4mL, add 3.4g K
2HPO
4; Vibration is to fully dissolving, and the centrifugal 2～3min of 3000r/min forms aqueous two-phase, gets mutually 20 μ L of ionic liquid, directly advances look capable analysis of spectrum;
(3) the fluid sample solution in the step (2) or solid sample solution are carried out efficient liquid phase chromatographic analysis;
High-efficient liquid phase chromatogram condition: chromatographic column: Zorbax ODS, internal diameter 4.6mm * column length 150mm * particle diameter 5 μ m; Column temperature: 30 ℃; Ultraviolet detects wavelength: it is 410 nm that lemon yellow detects wavelength, and it is 480nm that sunset yellow detects wavelength; Flow velocity: 1.0mL/min; Mobile phase: add the 2mL acetic acid solutions in the 0.02mol/L ammonium acetate solution and become the acetic acid of pH=4.5-ammonium acetate buffer A; B is methyl alcohol; Mobile phase B is by 15% even variation to 40% in gradient: 0～5min, and Mobile phase B is by 40% even variation to 98% in 5～10min, and Mobile phase B is by 98% even variation to 15% in 10～15min; The sample solution sample volume is 20 μ L;
(4) according to the equation of linear regression of step (1), calculate respectively the content of lemon yellow and sunset yellow in the food.
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Cited By (7)
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| CN106370494A (en) * | 2016-10-12 | 2017-02-01 | 林圣灼 | Method for extracting and separating coumarin by utilizing [BuPy(Butyl Pyridine)] PF6 |
| CN106645603A (en) * | 2017-01-13 | 2017-05-10 | 广西民族大学 | Method for synchronously detecting content of food additives and heavy metals in food in inverse HPLC-ICP-MS method |
| CN108760926A (en) * | 2018-06-06 | 2018-11-06 | 松原市食品药品检验所 | A kind of detection method for examining lemon yellow dyeing cattail pollen |
| CN109752474A (en) * | 2019-03-04 | 2019-05-14 | 福建中烟工业有限责任公司 | A method of acid green 50 and/or fast green FCF in the detection quick-fried pearl of cigarette |
| CN110161028A (en) * | 2019-06-14 | 2019-08-23 | 西北师范大学 | Utilize the method for the perchlorate in DLLME and scanner digital image analysis measurement food |
| CN111983010A (en) * | 2020-08-30 | 2020-11-24 | 广东利诚检测技术有限公司 | Method for detecting sunset yellow in bread based on out-of-phase equal-difference three-way induced potential |
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2013
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Non-Patent Citations (6)
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106370494A (en) * | 2016-10-12 | 2017-02-01 | 林圣灼 | Method for extracting and separating coumarin by utilizing [BuPy(Butyl Pyridine)] PF6 |
| CN106645603A (en) * | 2017-01-13 | 2017-05-10 | 广西民族大学 | Method for synchronously detecting content of food additives and heavy metals in food in inverse HPLC-ICP-MS method |
| CN108760926A (en) * | 2018-06-06 | 2018-11-06 | 松原市食品药品检验所 | A kind of detection method for examining lemon yellow dyeing cattail pollen |
| CN109752474A (en) * | 2019-03-04 | 2019-05-14 | 福建中烟工业有限责任公司 | A method of acid green 50 and/or fast green FCF in the detection quick-fried pearl of cigarette |
| CN109752474B (en) * | 2019-03-04 | 2022-04-22 | 福建中烟工业有限责任公司 | Method for detecting acid green 50 and/or fast green FCF in cigarette blasting beads |
| CN110161028A (en) * | 2019-06-14 | 2019-08-23 | 西北师范大学 | Utilize the method for the perchlorate in DLLME and scanner digital image analysis measurement food |
| CN111983010A (en) * | 2020-08-30 | 2020-11-24 | 广东利诚检测技术有限公司 | Method for detecting sunset yellow in bread based on out-of-phase equal-difference three-way induced potential |
| CN111983010B (en) * | 2020-08-30 | 2022-04-08 | 广东利诚检测技术有限公司 | Method for detecting sunset yellow in bread based on out-of-phase equal-difference three-way induced potential |
| CN113533609A (en) * | 2021-07-06 | 2021-10-22 | 河北大学 | Method for simply analyzing migration volume of common bisphenol substances in plastic product |
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