CN110988199B - Method for determining 2-ethylhexyl acrylate in carbonated beverage - Google Patents
Method for determining 2-ethylhexyl acrylate in carbonated beverage Download PDFInfo
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Abstract
The invention discloses a quantitative detection method of 2-ethylhexyl acrylate content in carbonated beverage, which mainly comprises the preparation of magnetic solid phase extraction material; preparing a standard working solution, a sample test solution and a blank test solution; gas chromatography-tandem triple quadrupole mass spectrometry; drawing a standard curve, calculating concentration and the like; the method has the advantages that the process is simple, the content of the 2-ethylhexyl acrylate in the carbonated beverage can be accurately measured by utilizing the sample pretreatment method and the conditions set by the chromatogram and the mass spectrum, the detection limit of the method is as low as 0.005mg/kg (5 mu g/kg), the method has good accuracy and reproducibility, and the method can be used for accurately, qualitatively and quantitatively determining.
Description
Technical Field
The invention belongs to the technical field of compound content determination, and particularly relates to a method for determining 2-ethylhexyl acrylate in a carbonated beverage.
Background
Polyacrylates are high molecular polymers with excellent heat, water and oxidation resistance properties and are therefore widely used in the fields of coatings, adhesives, leather, chemical fibers, synthetic plastics, paper industry, food contact materials and the like. The copolymer taking 2-ethylhexyl acrylate as a monomer is an acrylic ester coating which is gradually popular due to excellent color retention and physical processing performance; with the rapid development of the Chinese packaging material industry, the adhesive taking 2-ethylhexyl acrylate as a monomer is more frequently used in the beverage industry.
In the production process, in order to improve appearance and physical properties, beverage containers such as beverage bottles and beverage cans are processed using an adhesive using 2-ethylhexyl acrylate as a monomer. However, related researches show that 2-ethylhexyl acrylate has certain mutagenicity and genetic toxicity, and substances of the type can migrate in the process of contacting food, particularly easily migrate into various beverages from packaging materials and coatings, and further harm the life health of consumers. The national standard GB 9685 of China stipulates that the specific migration limit of the acrylic acid-2-ethylhexyl ester in the food contact material is 0.05 mg/kg. The harmfulness of phthalate plasticizers is well known, so that the method has high attention, related detection methods are mature, monitoring is strict, and purchasing and use can be effectively controlled; however, a complete and high-precision detection system for 2-ethylhexyl acrylate in carbonated beverages is not established, and some illegal merchants utilize the detection system to produce related food contact products by using 2-ethylhexyl acrylate instead of 2-ethylhexyl phthalate (DEHP), which is prone to cause a large food safety risk if effective supervision cannot be performed on the products in time.
At present, reports on the detection of 2-ethylhexyl acrylate in carbonated beverages are not found at home and abroad. Therefore, the method for detecting the 2-ethylhexyl acrylate in the carbonated beverage food is simple and easy to operate, has high accuracy, can effectively detect and monitor the product quality of the carbonated beverage product, and has important significance for protecting the health and safety of consumers.
The detection of a chromatography-mass spectrometry combined analysis instrument is a common compound detection method, but a detection substance is easily interfered by a matrix to influence a detection result, so that the method is very important for selecting chromatographic and mass spectrometry parameters, each compound corresponds to different chromatographic and mass spectrometry analysis conditions, and a target substance can be accurately analyzed only if correct chromatographic and mass spectrometry parameters are selected. If the parameter setting is not good, not only can a satisfactory result not be obtained, but also the interference can be caused by false positive substances, an error conclusion can be obtained, and the accuracy of an analysis result is influenced; in addition, in view of the limitations of the analytical instrument, the gas chromatography-mass spectrometer has better sensitivity, but the mass spectrometer is not very suitable for detecting the target object in the aqueous food because the mass spectrometer needs to maintain a vacuum environment.
Therefore, the method for pretreating the sample, which can quickly enrich the target substance and remove the water phase matrix, is established, and has very important social significance and practical value for quickly detecting the target substance 2-ethylhexyl acrylate in the carbonated beverage.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a quantitative detection method for the content of 2-ethylhexyl acrylate in a carbonated beverage, which has the advantages of simple determination process, high result accuracy and good reproducibility.
The technical scheme of the invention is as follows: a quantitative determination method for the content of 2-ethylhexyl acrylate in a carbonated beverage specifically comprises the following steps:
(1) preparing a magnetic solid phase extraction material: dissolving ferric trichloride hexahydrate in ethylene glycol at room temperature, adding anhydrous sodium acetate and polyethylene glycol 600, adding a carbon nitride nano material, stirring to enable the carbon nitride nano material to be uniformly suspended in an iron solution, putting the suspension into a high-pressure reaction kettle for hydrothermal reaction, and collecting formed Fe by using a magnet after the reaction is finished3O4@C3N4Pouring out the reaction liquid from the magnetic solid-phase material, and washing the magnetic solid-phase material with distilled water for later use;
(2) preparing a standard working solution, a sample test solution and a blank test solution:
Preparation of standard working solution:
a. preparation of 2-ethylhexyl acrylate standard stock solutions: accurately weighing 10mg of acrylic acid-2-ethylhexyl ester standard substance with the content of more than 99.0% into a 100mL volumetric flask, accurately measuring the content to 0.1mg, dissolving the standard substance by using n-hexane with pesticide residue level, fixing the volume, and sealing and storing the standard substance at 4 ℃ in a dark place;
b. preparation of 2-ethylhexyl acrylate standard use solutions: respectively transferring 50 mu L, 100 mu L, 200 mu L, 500 mu L and 1000 mu L of 2-ethylhexyl acrylate standard stock solution into 5 100mL volumetric flasks, using pesticide residue grade n-hexane for constant volume, and preparing standard working solutions with the concentrations of 50 mu g/L, 100 mu g/L, 200 mu g/L, 500 mu g/L and 1000 mu g/L to be tested;
preparing a sample test solution:
weighing 20-30g carbonated beverage sample into a 50mL glass centrifuge tube, adding 50-100mg magnetic solid phase extraction material Fe3O4@C3N4After vortex oscillation for 2-5min, using magnet to attract Fe outside the glass centrifuge tube3O4@C3N4Material, pouring off the carbonated beverage solution; adding 2.0-3.0mL of n-hexane solvent into a centrifuge tube, performing vortex oscillation for 5-15s, and performing ultrasonic extraction for 5-10 min; placing a magnet outside a centrifuge tube to absorb the magnetic solid phase material, taking 1-2mL of supernatant, filtering the supernatant through a 0.45-micrometer organic filter membrane, and placing the supernatant in a sample injection vial to be tested;
Preparing a blank test solution: replacing the carbonated beverage used in the second step with ultrapure water with equal quality, and keeping the other operations consistent with the second step;
(3) respectively carrying out gas chromatography-tandem triple quadrupole mass spectrometry on the three solutions prepared in the step 2 by adopting a gas chromatography-tandem triple quadrupole mass spectrometer; taking the concentration x of the 2-ethylhexyl acrylate in the standard working solution as an abscissa and the corresponding measured peak area y of the daughter ion as an ordinate, drawing a regression curve of the standard working solution, and calculating the slope a and the intercept b of the regression curve according to a linear equation y which is obtained by the curve and is ax + b;
the gas chromatography-tandem triple quadrupole mass spectrometer detection instrument measurement parameters are set as follows:
gas chromatography conditions:
capillary chromatographic column: the length of the chromatographic column is 30-60 m; the inner diameter of the chromatographic column is 0.25-0.50 mm; the thickness of the chromatographic column coating film is 0.25-0.4 mu m;
temperature programming conditions: the initial temperature is 30-90 ℃, the temperature is kept for 2-6min, the temperature is raised to 200 ℃ and 325 ℃ at the speed of 20-40 ℃/min, and the temperature is kept for 1-10 min;
sample introduction amount: 1.0-5.0 μ L;
carrier gas flow rate: 0.5-2.0 mL/min;
tandem triple quadrupole mass spectrometry conditions:
an ion source: electron impact ion source (EI) or atmospheric pressure chemical ionization source (CI);
Electron energy: 60-75 eV;
③ ion source temperature: 150 ℃ and 250 ℃;
and fourthly, a detection mode: selecting ion Scanning (SIM) or multiple ion reaction detection (MRM);
solvent delay: 2-8 min;
carrier gas: helium gas with a purity of 99.999%;
seventh, flow of sheath gas: 6-9L/min;
and collision gas: nitrogen with purity of 99-99.995%;
ninthly, resolution ratio: narrow or wide;
(4) according to the formula c ═ y-b]A, calculating the concentration c of the sample test solution and the concentration c of the blank test solution0Wherein the y-value corresponds to the measured quantitative ion peak area of 2-ethylhexyl acrylate in the carbonated beverage sample or blank;
(5) the content of 2-ethylhexyl acrylate in the carbonated beverage is X ═ c-c0) (10), wherein X is the content of 2-ethylhexyl acrylate in the carbonated beverage in μ g/kg; c is the concentration of the carbonated beverage sample test solution, c0The concentration of the blank test solution is expressed in the unit of mu g/L.
In the step 1, the concentration range of ferric trichloride in the ethylene glycol solution is 0.1-2.0 mol/L.
In the step 1, the molar ratio of the anhydrous sodium acetate to the ferric trichloride is 2-10: 1.
in the step 1, the molar ratio of the polyethylene glycol 600 to the ferric trichloride is 0.01-0.5: 1.
in step 1, g-C3N4The mass ratio of the iron trichloride to the iron trichloride is 0.1-0.5: 1.
In the step 1, the temperature of the hydrothermal reaction is 150-250 ℃, and the reaction time is 5-24 h.
The beneficial effects of the invention are:
the invention establishes the method for detecting the content of the 2-ethylhexyl acrylate in the carbonated beverage for the first time, the sample test solution can be directly subjected to sample injection test after being enriched by a magnetic solid phase material and separated from a water phase, extracted by normal hexane and filtered by a filter membrane, the complex pretreatment step is not needed, the target to be detected can be efficiently enriched, and the detection limit of the method is reduced; in addition, the method can accurately measure the content of the 2-ethylhexyl acrylate in the carbonated beverage by utilizing the set conditions of the chromatogram and the mass spectrum, the detection limit of the method is as low as 0.005mg/kg, and the method has good accuracy and repeatability and can accurately determine the nature and quantity.
Drawings
FIG. 1 shows collision energy of 2-ethylhexyl acrylate;
FIG. 2 shows the added recovery and precision statistics of 2-ethylhexyl acrylate content;
FIG. 3 is a typical chromatogram of 2-ethylhexyl acrylate;
FIG. 4 is a mass spectrum of a kojic MRM of 2-ethylhexyl acrylate.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.
EXAMPLE one method for measuring 2-ethylhexyl acrylate content in carbonated beverages
1. Preparing a magnetic solid phase extraction material: 2.7g FeCl3·6H2O (10mmol) was dissolved in 50mL of ethylene glycol, followed by the addition of 4.1g of sodium acetate (50mmol) and 1.2g of polyethylene glycolAlcohol 600(0.2mmol), dissolved with stirring; then adding carbon nitride nano material (g-C)3N4The substance can be prepared by high-temperature calcination of urea or melamine by a mature method, and is shown in the literature: nat. mater, 2009,8, 76-80; angew. chem.int.Ed.,2012,51,68), stirring to make it uniformly suspended in iron solution, placing the suspension into high-pressure reaction still (equipped with teflon tank), screwing down the reaction still and making hydrothermal reaction at 220 deg.C for 15 hr, after the reaction is finished, using magnet to collect the formed Fe3O4@C3N4The materials are washed by distilled water for standby.
2. Preparing a standard working solution, a sample test solution and a blank test solution:
preparation of standard working solution:
a. preparation of 2-ethylhexyl acrylate standard stock solutions: accurately weighing a 2-ethylhexyl acrylate standard substance with the content of more than 99.0 percent into a volumetric flask of 10mg to 100mL, accurately measuring the content to 0.1mg, dissolving the standard substance by using n-hexane with pesticide residue level and fixing the volume, storing the stock solution at 4 ℃ in a sealed and light-proof manner, wherein the content of the 2-ethylhexyl acrylate in the solution is 100 mg/L;
b. Preparation of 2-ethylhexyl acrylate standard use solutions: respectively transferring 50 mu L, 100 mu L, 200 mu L, 500 mu L and 1000 mu L of 2-ethylhexyl acrylate standard stock solution into 5 100mL volumetric flasks, using pesticide residue grade n-hexane for constant volume, preparing standard working solutions with the concentrations of 50 mu g/L, 100 mu g/L, 200 mu g/L, 500 mu g/L and 1000 mu g/L respectively, and testing;
preparing a sample test solution:
20g of carbonated beverage sample is weighed into a 50mL glass centrifuge tube, and 100mg of magnetic solid phase extraction material Fe is added into the centrifuge tube3O4@C3N4After vortex oscillation for 5min, the Fe is attracted outside the glass centrifuge tube by a magnet3O4@C3N4Material, pouring off the carbonated beverage solution; adding 2.0mL of n-hexane solvent into a centrifuge tube, performing vortex oscillation for 10s, and performing ultrasonic extraction for 5 min; placing a magnet outside a glass centrifuge tube to absorb the magnetic solid phase material, taking 1mL of supernatant, filtering the supernatant through a 0.45 mu m organic filter membrane, and placing the supernatant in a sample injection vial to be tested;
preparing a blank test solution: 20g of carbonated beverage used in the second step is replaced by 20g of ultrapure water, and other operations are the same as those in the second step;
3. respectively carrying out gas chromatography-tandem triple quadrupole mass spectrometry on the three solutions prepared in the step 2 by adopting a gas chromatography-tandem triple quadrupole mass spectrometer; taking the concentration x of the 2-ethylhexyl acrylate in the standard working solution as an abscissa and the corresponding measured peak area y of the daughter ion as an ordinate, drawing a regression curve of the standard working solution, and calculating the slope a and the intercept b of the regression curve according to a linear equation y which is obtained by the curve and is ax + b;
The instrument conditions for this measurement were set as follows:
gas chromatography conditions:
1) capillary chromatographic column: coating material, polymethylsiloxane coating; the length of the chromatographic column is 30 m; the inner diameter of the chromatographic column is 0.25 mm; the thickness of the chromatographic column coating film is 0.25 μm;
2) temperature programming conditions: the initial temperature is 50 ℃, the temperature is kept for 3min, the temperature is increased to 250 ℃ at the speed of 20 ℃/min, and the temperature is kept for 5 min;
3) sample introduction amount: 1.0 μ L;
4) flow rate of carrier gas: 1.0 mL/min.
Tandem triple quadrupole mass spectrometry conditions:
1) an Electron Impact (EI) ion source;
2) electron energy: 70 eV;
3) ion source temperature: 230 ℃;
4) the detection mode is as follows: multiple ion reaction detection (MRM);
5) solvent retardation: 4.5 min;
6) carrier gas: helium gas with a purity of 99.999%;
7) the flow rate of the sheath gas: 6L/min;
8) collision gas: nitrogen gas of purity 99.995%;
9) resolution ratio: narrow peak width;
the collision energy is shown in fig. 1, in this embodiment, a first-order spectrum analysis is performed on 2-ethylhexyl acrylate under an electron bombardment ion source to obtain a first-order cleavage peak of 2-ethylhexyl acrylate, then collision induced Cleavage (CID) is performed, mass spectrum fragments are analyzed, and under an optimized second-order mass spectrum condition, interference of acrylate homologues is combined, 112- >55 and 112- >41 are selected as monitoring ions, wherein 112- >55 is a quantitative ion, and the collision energy of 112- >55 is 20 eV; 112- - >41 is a qualitative ion, and the collision energy of 112- - >41 is 30 eV.
4. Calculating the concentration c of 2-ethylhexyl acrylate in the sample test solution and the blank concentration c according to the formula (y-b)/a0(ii) a Wherein y is the area of the quantitative ion peak of acrylic acid-2-ethylhexyl ester in the test solution.
5. The content of 2-ethylhexyl acrylate in the carbonated beverage is X ═ c-c0) (10), wherein X is the content of 2-ethylhexyl acrylate in the carbonated beverage in μ g/kg; c is the carbonated beverage sample concentration, c0The blank concentration is given in μ g/L.
And (3) performing a repeatability test, namely preparing two parts of food simulant test solution in parallel, then performing the operations of the step 3 and the step 4, and if the absolute difference of the two independent test results does not exceed 20 percent of the arithmetic mean value, the test is accurate.
Example two, the precision and recovery rate of the method were measured by the addition method
The method of adding recovery rate is adopted, 2-ethylhexyl acrylate is added to 5.0 mug/kg, 50 mug/kg and 1000 mug/kg of carbonic acid beverage samples without 2-ethylhexyl acrylate respectively, then sample pretreatment and measurement are carried out, each level is measured in parallel for 8 times, the calculation of recovery rate and precision is carried out, and the results of the recovery rate and precision test are shown in figure 2.
As can be seen from FIG. 2, the recovery and precision of the process are good. The recovery rate of the method for measuring various simulators is 85-115 percent; the precision is below 10%, the quantification is accurate and reliable, and the reproducibility is good.
The method of the invention comprises the selection of experimental conditions to be set only for the determination of the 2-ethylhexyl acrylate content in carbonated beverages. The detection method has the detection low limit of 0.005mg/kg (5 mu g/kg) which is far less than the requirement of 0.05mg/kg of the standard limit, so that the detection method can effectively detect and monitor the 2-ethylhexyl acrylate in the carbonated beverage products.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. However, the above description is only an example of the present invention, the technical features of the present invention are not limited thereto, and any other embodiments that can be obtained by those skilled in the art without departing from the technical solution of the present invention should be covered by the claims of the present invention.
Claims (6)
1. A quantitative determination method for the content of 2-ethylhexyl acrylate in carbonated beverages is characterized by comprising the following specific steps:
(1) preparing a magnetic solid phase extraction material: dissolving ferric trichloride hexahydrate in ethylene glycol at room temperature, adding anhydrous sodium acetate and polyethylene glycol 600, adding a carbon nitride nano material, stirring to enable the carbon nitride nano material to be uniformly suspended in an iron solution, putting the suspension into a high-pressure reaction kettle for hydrothermal reaction, and collecting formed Fe by using a magnet after the reaction is finished 3O4@C3N4Pouring out the reaction liquid from the magnetic solid-phase material, and washing the magnetic solid-phase material with distilled water for later use;
(2) preparing a standard working solution, a sample test solution and a blank test solution:
preparation of standard working solution:
a. preparation of 2-ethylhexyl acrylate standard stock solutions: accurately weighing 10mg of acrylic acid-2-ethylhexyl ester standard substance with the content of more than 99.0% into a 100mL volumetric flask, accurately measuring the content to 0.1mg, dissolving the standard substance by using n-hexane with pesticide residue level, fixing the volume, and sealing and storing the standard substance at 4 ℃ in a dark place;
b. preparation of 2-ethylhexyl acrylate standard use solutions: respectively transferring 50 mu L, 100 mu L, 200 mu L, 500 mu L and 1000 mu L of 2-ethylhexyl acrylate standard stock solution into 5 100mL volumetric flasks, using pesticide residue grade n-hexane for constant volume, and preparing standard working solutions with the concentrations of 50 mu g/L, 100 mu g/L, 200 mu g/L, 500 mu g/L and 1000 mu g/L to be tested;
preparing a sample test solution:
weighing 20-30g carbonated beverage sample to 50mL glassAdding 50-100mg of magnetic solid phase extraction material Fe into a glass centrifuge tube3O4@C3N4After vortex oscillation for 2-5min, using magnet to attract Fe outside the glass centrifuge tube3O4@C3N4Material, pouring off the carbonated beverage solution; adding 2.0-3.0mL of n-hexane solvent into a glass centrifuge tube, performing vortex oscillation for 5-15s, and performing ultrasonic extraction for 5-10 min; placing a magnet outside a centrifuge tube to absorb the magnetic solid phase material, taking 1-2mL of supernatant, filtering the supernatant through a 0.45-micrometer organic filter membrane, and placing the supernatant in a sample injection vial to be tested;
Preparing a blank test solution: replacing the carbonated beverage used in the second step with ultrapure water with equal quality, and keeping the other operations consistent with the second step;
(3) respectively carrying out gas chromatography-tandem triple quadrupole mass spectrometry on the three solutions prepared in the step 2 by adopting a gas chromatography-tandem triple quadrupole mass spectrometer; taking the concentration x of the 2-ethylhexyl acrylate in the standard working solution as an abscissa and the corresponding measured peak area y of the daughter ion as an ordinate, drawing a regression curve of the standard working solution, and calculating the slope a and the intercept b of the regression curve according to a linear equation y which is obtained by the curve and is ax + b;
the gas chromatography-tandem triple quadrupole mass spectrometer detection instrument measurement parameters are set as follows:
gas chromatography conditions:
capillary chromatographic column: coating material, polymethylsiloxane coating; the length of the chromatographic column is 30-60 m; the inner diameter of the chromatographic column is 0.25-0.50 mm; the thickness of the chromatographic column coating film is 0.25-0.4 mu m;
temperature programming conditions: the initial temperature is 30-90 ℃, the temperature is kept for 2-6min, the temperature is raised to 200 ℃ and 325 ℃ at the speed of 20-40 ℃/min, and the temperature is kept for 1-10 min;
sample introduction amount: 1.0-5.0 μ L;
carrier gas flow rate: 0.5-2.0 mL/min;
tandem triple quadrupole mass spectrometry conditions:
An ion source: electron bombardment ion sources or atmospheric pressure chemical ionization sources;
electron energy: 60-75 eV;
③ ion source temperature: 150 ℃ and 250 ℃;
and fourthly, a detection mode: selecting ion scanning or multi-ion reaction detection;
solvent delay: 2-8 min;
carrier gas: helium gas with a purity of 99.999%;
seventh, flow of sheath gas: 6-9L/min;
and collision gas: nitrogen with purity of 99-99.995%;
ninthly, resolution ratio: narrow or wide;
(4) according to the formula c ═ y-b]A, calculating the concentration c of the sample test solution and the concentration c of the blank test solution0Wherein the y-value corresponds to the measured quantitative ion peak area of 2-ethylhexyl acrylate in the carbonated beverage sample or blank;
(5) the content of 2-ethylhexyl acrylate in the carbonated beverage is X ═ c-c0) (10), wherein X is the content of 2-ethylhexyl acrylate in the carbonated beverage in μ g/kg; c is the concentration of the carbonated beverage sample test solution, c0The concentration of the blank test solution is expressed in the unit of mu g/L.
2. The method for quantitatively determining the content of 2-ethylhexyl acrylate in a carbonated beverage as claimed in claim 1, wherein in step 1, the concentration of ferric chloride in the ethylene glycol solution is in the range of 0.1 to 2.0 mol/L.
3. The method for quantitatively detecting the content of 2-ethylhexyl acrylate in a carbonated beverage as claimed in claim 1, wherein in step 1, the molar ratio of anhydrous sodium acetate to ferric chloride is 2-10: 1.
4. The method for quantitatively detecting the content of 2-ethylhexyl acrylate in a carbonated beverage as claimed in claim 1, wherein in step 1, the molar ratio of polyethylene glycol 600 to ferric chloride is 0.01 to 0.5: 1.
5. the method for quantitatively determining the content of 2-ethylhexyl acrylate in a carbonated beverage as claimed in claim 1, wherein in step 1，g-C3N4The mass ratio of the ferric trichloride to the ferric trichloride is 0.1-0.5: 1.
6. the method for quantitatively detecting the content of 2-ethylhexyl acrylate in carbonated beverage as claimed in claim 1, wherein the hydrothermal reaction is carried out at 150 ℃ and 250 ℃ for 5-24h in step 1.
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| CN102175799A (en) * | 2010-12-28 | 2011-09-07 | 西安航天三沃化学有限公司 | Method for testing contents of residual monomers in acrylate pressure sensitive adhesive by virtue of gas chromatography |
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