CN105954436A - Method for measuring transporting quantity of para-hydroxy benzaldehyde in food contact material - Google Patents
Method for measuring transporting quantity of para-hydroxy benzaldehyde in food contact material Download PDFInfo
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- CN105954436A CN105954436A CN201610581833.0A CN201610581833A CN105954436A CN 105954436 A CN105954436 A CN 105954436A CN 201610581833 A CN201610581833 A CN 201610581833A CN 105954436 A CN105954436 A CN 105954436A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Abstract
The invention relates to a method for measuring transporting quantity of para-hydroxy benzaldehyde in a food contact material, and belongs to the technical field of analysis and detection. The method for measuring transporting quantity of para-hydroxy benzaldehyde in the food contact material is set up, quantification results are accurate and reliable, and accuracy, stability and the automation degree are high. According to stipulations of national standards in China, feed simulants are selected to simulate different foods for transporting tests, and the feed simulants comprise water, an acetic acid solution with the mass concentration of 3%, an ethanol solution with the volume fraction of 10% and isooctane which represent water-based, acidic, alcoholic and lipid foods respectively; the method is wide in coverage and high in practicability.
Description
Technical field
The present invention relates to the assay method of MEHQ migration amount in a kind of food contact material, belong to analysis detection
Technical field.
Background technology
MEHQ (No. CAS, 150-76-5) is a kind of important chemical industry and organic synthesis raw material, may be used for closing
Become dyestuff etc..Its utilization in plastic, essentially consists in the polymerization inhibitor as vinyl-type plastic monomer, ultraviolet suppression
Agent etc., also act as age resistor, antioxidant etc., can effectively postpone oxidation and the decomposition of plastic.For serving as food
The plastic of product contact, MEHQ may move to food from plastic.MEHQ is to eyes, skin
Skin, mucosa and upper respiratory tract have stimulation, and contact has infringement to eye for a long time, has strong impulse effect maybe can cause bright
Wound.2015 issue " GB 9685 national food safety standard food contact material and goods additive use standard (to levy
Seek suggestion original text) " in the range of regulation MEHQ be that polystyrene type plastic-food contacts material with maximum usage amount
Material and goods and 0.05%.
At present, for the detection of MEHQ migration amount in food contact material, there is not been reported both at home and abroad.Therefore,
Set up the quantitative detecting method of MEHQ migration amount in food contact material, it is possible to effectively to food contact material
Sanitation performance is tested, thus assesses its application risk, it is stipulated that it uses condition, and protection people's is healthy and safe.
Summary of the invention
Present invention solves the technical problem that and be: propose a kind of accurately, para hydroxybenzene first in the little food contact material of error
The assay method of ether migration amount.
In order to solve above-mentioned technical problem, the technical scheme that the present invention proposes is: to hydroxyl in a kind of food contact material
The assay method of methyl phenyl ethers anisole migration amount, it is characterised in that: comprise the following steps:
Step 1: preparing standard working solution, food simulants test solution and blank test solution, standard working solution is by hydroxyl
Water base and the oiliness isobutyltrimethylmethane. standard working solution of at least five kinds of concentration that base methyl phenyl ethers anisole is formulated；Food simulated solution is by food
Contact material and food simulants obtain by migrating experiment, try including aqueous-based food analogies test solution and oily food analogies
Liquid；Blank test solution is the food simulants not contacted with food contact material；
Step 2: use gas chromatogram-series connection triple quadrupole bar GC-MS (GC-MS/MS) molten to three kinds of step 1
Liquid carries out GC-MS/MS analysis respectively；With concentration x of MEHQ as abscissa, with the corresponding quota ion peak recorded
Area y is vertical coordinate, draws standard working solution regression curve, the linear equation y=ax+b obtained according to curve, calculates back
Return slope of a curve a and intercept b；
Step 3: according to formula c=((yExamination-yEmpty)-b)/a calculates MEHQ concentration c in food simulants test solution,
Wherein yExaminationFor MEHQ quota ion peak area in the food simulants test solution that records, yEmptyFor in the blank test solution that records
MEHQ quota ion peak area；
Wherein, GC conditions:
(1) chromatographic column: coating is Polyethylene Glycol, polystyrene or polymethyl siloxane material, chromatogram column length is 10-
100m；Chromatographic column internal diameter is 0.20mm-0.60mm；Coating thickness is: 0.1-1.0 μm；
(2) sample size: 0.5-2.0 μ L；
(3) temperature programming condition: initial temperature 40-60 DEG C, keeps 0-4min, is warming up to the speed of 5-25 DEG C/min
160-280 DEG C, keep 0-5min；
(4) flow rate of carrier gas: 0.8-1.2mL/min；
Triple quadrupole bar tandem mass spectrum condition:
(1) ion source: electron impact ion source EI or chemical ionization source CI；
(2) ion source temperature: 230-260 DEG C；
(3) electron energy: 65-75eV；
(4) carrier gas control model: constant voltage mode, constant current mode or constant linear velocity pattern；
(5) detection mode: full scan SCAN, selection ion scan SIM or polyion reaction monitoring MRM；
(6) solvent delay: 1-6min；
(7) carrier gas: purity is the helium of 99%-99.9999%；
(8) resolution: unit, wide or widest resolution；
(9) under ion source, MEHQ is cracked, obtain fragment ion is analyzed, through corresponding ginseng
Number optimizes, and selection wherein 123.9 ＞ 109.0 and 123.9 81.0 two pairs of ions of ＞ are as the prison of MEHQ
Measured ion.
Preferably, the collision energy of described MEHQ see table:
Preferably, the preparation method step of described water base standard working solution is:
(1) MEHQ Standard Stock solutions is prepared: accurately weigh the content MEHQ more than 99.0%
Standard substance 25mg to 250mL volumetric flask, with acetone solution the constant volume of chromatographically pure rank, this Standard Stock solutions is close at 4 DEG C
Envelope lucifuge stores；
(2) pipette appropriate MEHQ Standard Stock solutions, be 3% acetic acid solution by water, mass concentration respectively
It is 10% ethanol solution constant volume with volume fraction, is configured to the standard working solution of at least five kinds of concentration；
(3) adding the water base standard working solution of 10.0mL in centrifuge tube, add 2.0mL t-butyl methyl ether, vortex shakes
4000 revs/min of centrifugations 5 minutes after swinging 5 minutes, by upper strata t-butyl methyl ether solution after 0.2 μm nylon leaching film filters
Carry out GC-MS/MS analysis.
Preferably, the preparation method step of described oiliness standard working solution isobutyltrimethylmethane. is:
(1) MEHQ Standard Stock solutions is prepared: accurately weigh the content MEHQ more than 99.0%
Standard substance 25mg to 250mL volumetric flask, with acetone solution the constant volume of chromatographically pure rank, this Standard Stock solutions is close at 4 DEG C
Envelope lucifuge stores；
(2) pipette appropriate MEHQ Standard Stock solutions, use isobutyltrimethylmethane. constant volume, be configured at least five kinds of concentration
Standard working solution, through 0.2 μm nylon leaching film filter after carry out GC-MS/MS analysis.
Beneficial effects of the present invention:
The present invention establishes the detection method of MEHQ migration amount in food contact material, and quantitative result accurately may be used
Leaning on, precision, stability and automaticity are high.Owing to food contact material may contact different types of food, it is impossible to
The mensuration of MEHQ migration amount is carried out for all food.The present invention is according to China's national standard " GB/T 23296.1-
In 2009 food contact material plastics, in restricted substances plastics, material is tested and content to food and food simulants specific transfer
The guide that assay method and food simulants exposure condition select " regulation select food simulants to simulate different food products to enter
Row migrates test, including water, 3% (mass concentration) acetic acid solution, 10% (volume fraction) ethanol solution and isobutyltrimethylmethane., represents water
Base, acidity, alcohol type and lipid food, method broad covered area, practical by force.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings the present invention is described further.
Fig. 1 is MEHQ GC-MS total ion current figure in embodiment 1
Detailed description of the invention
Embodiment 1
Instrument and reagent:
Instrument: gas chromatogram-series connection triple quadrupole bar GC-MS (GC-MS/MS), centrifuge, vortex oscillation instrument.
Reagent: MEHQ standard substance (purity >=98%), deionized water, acetic acid (analytical pure), dehydrated alcohol, different
Octane (chromatographically pure), t-butyl methyl ether (chromatographically pure).
In a kind of food contact material, the assay method of MEHQ migration amount comprises the following steps:
Step 1, prepare standard working solution, food simulants test solution and blank test solution.Standard working solution is by hydroxyl
Water base and the oiliness standard working solution (isobutyltrimethylmethane .) of at least five kinds of concentration that base methyl phenyl ethers anisole is formulated；Described food simulants
Test solution by food contact material and food simulants according to " limited thing in GB/T 23296.1-2009 food contact material plastics
In matter plastics, material is tested to food and food simulants specific transfer and is exposed bar with content assaying method and food simulants
The guide that part selects " by migrating experiment acquisition, including aqueous-based food analogies test solution and oily food analogies test solution；Described
Blank test solution is the food simulants test solution not contacted with food contact material.
The preparation method of aqueous-based food analogies standard working solution is particularly as follows: (1) prepares the storage of MEHQ standard
Standby solution: accurately weigh content MEHQ standard substance 25mg (being accurate to 0.1mg) more than 99.0% to 250mL capacity
Bottle, with acetone solution the constant volume of chromatographically pure rank, this Standard Stock solutions stores 4 DEG C of lower seal lucifuges；(2) pipette in right amount
MEHQ Standard Stock solutions, respectively with water, 3% (mass concentration) acetic acid solution and 10% (volume fraction) ethanol
Solution constant volume, is configured to the standard working solution of at least five kinds of concentration；(3) in centrifuge tube, the work of 10.0mL water base standard is added
Solution, adds 2.0mL t-butyl methyl ether, and vortex oscillation is centrifugation 5 minutes (4000 revs/min) after 5 minutes, by upper strata uncle
Butyl methyl ether solution carries out GC-MS/MS analysis after 0.2 μm nylon leaching film filters.
The preparation method of oiliness standard working solution (isobutyltrimethylmethane .) is particularly as follows: (1) prepares MEHQ standard inventory
Solution: accurately weigh content MEHQ standard substance 25mg (being accurate to 0.1mg) more than 99.0% to 250mL capacity
Bottle, with acetone solution the constant volume of chromatographically pure rank, this Standard Stock solutions stores 4 DEG C of lower seal lucifuges；(2) pipette in right amount
MEHQ Standard Stock solutions, use isobutyltrimethylmethane. constant volume, be configured to the standard working solution of at least five kinds of concentration, pass through
0.2 μm nylon leaching film carries out GC-MS/MS analysis after filtering.
The preparation method of aqueous-based food analogies test solution particularly as follows: (1) by food contact material respectively with water, 3% (quality
Concentration) acetic acid solution and 10% (volume fraction) ethanol solution be according to " in GB/T 23296.1-2009 food contact material plastics
In restricted substances plastics, material is tested and content assaying method and food simulants to food and food simulants specific transfer
The guide that exposure condition selects " carry out migrating experiment, it is thus achieved that aqueous-based food analogies test solution；(2) aqueous-based food mould is accurately pipetted
Thing test solution 10.0mL is in 25mL centrifuge tube for plan, adds 2.00mL t-butyl methyl ether, and vortex oscillation is centrifugation 5 points after 5 minutes
Clock (4000 revs/min), carries out GC-MS/MS analysis by upper strata t-butyl methyl ether solution after 0.2 μm nylon leaching film filters.
The preparation method of oily food analogies test solution (isobutyltrimethylmethane .) particularly as follows: by food contact material and isobutyltrimethylmethane. according to
" in GB/T 23296.1-2009 food contact material plastics, in restricted substances plastics, material is specific to food and food simulants
The guide that migration test and content assaying method and food simulants exposure condition select " carry out migrating experiment, it is thus achieved that oiliness
Food simulants test solution (isobutyltrimethylmethane .), carries out GC-MS/MS analysis after 0.2 μm nylon leaching film filters.
Blank test solution be respectively do not contact with food contact material water, 3% (mass concentration) acetic acid solution, 10% (body
Fraction) ethanol solution and isobutyltrimethylmethane..
Step 2, respectively three kinds of solution of step 1 are carried out GC-MS/MS mensuration: with para hydroxybenzene in standard working solution
Concentration x of methyl ether is abscissa, with the corresponding quota ion peak area y recorded as vertical coordinate, draws standard working solution and returns
Return curve, obtain linear equation y=ax+b according to curve matching, calculate slope a and intercept b of regression curve；
Wherein, GC-MS/MS instrument parameter is as follows:
GC conditions:
(1) chromatographic column: coating is polymethyl siloxane material (5% phenyl 95% polydimethylsiloxane), column length
Degree is 30m；Chromatographic column internal diameter is 0.25mm；Coating thickness is: 0.25 μm；
(2) sample size: 1.0 μ L；
(3) temperature programming condition: initial temperature 60 DEG C, is warming up to 200 DEG C with the speed of 10 DEG C/min, keeps 2min；
(4) flow rate of carrier gas: 1.0mL/min.
Triple quadrupole bar tandem mass spectrum condition:
(1) ion source: electron impact ion source (EI)；
(2) ion source temperature: 250 DEG C；
(3) electron energy: 70eV；
(4) carrier gas control model: constant current mode；
(5) detection mode: polyion reaction monitoring (MRM)；
(6) solvent delay: 4min；
(7) carrier gas: purity is the helium of 99.9992%；
(8) resolution: unit resolution.
Under ion source, MEHQ is cracked, obtain fragment ion is analyzed, through corresponding ginseng
Number optimizes, and present invention selection wherein 123.9 ＞ 109.0 and 123.9 81.0 two pairs of ions of ＞ are as para hydroxybenzene first
The monitoring ion of ether, collision energy such as table 1 below:
The collision energy of table 1 MEHQ
Step 3, according to formula c=((yExamination-yEmpty)-b)/a calculates MEHQ concentration c in food simulants test solution,
Wherein yExaminationFor MEHQ quota ion peak area in the food simulants test solution that records, yEmptyFor in the blank test solution that records
MEHQ quota ion peak area.
Repeated experiment: food simulants test solution and the blank the most parallel preparation of test solution two parts, then carries out step 2 and 3, if
The absolute difference of twice independent test result is less than the 15% of its arithmetic average, then test is accurately.
Additive process is finally used to detect precision and the response rate of this method:
Use additive process, add respectively hydroxyl in the food simulants without MEHQ namely blank test solution
Methyl phenyl ethers anisole is to carry out sample pre-treatments also by the step of the present invention after tri-levels of 0.05mg/kg, 0.50mg/kg, 5.00mg/kg
Measure, repeat each level to add and measure 6 times, and carry out the response rate and precision calculating, the response rate and precision test
The results detailed in Table 2.
Table 2 MEHQ is TIANZHU XINGNAO Capsul and precision in blank test solution
As can be seen from Table 2, the response rate and the precision of this method are good.Varieties of food items analogies mensuration is returned by method
Yield reaches 86.2%～102.2%；Precision is less than 8%, and accurately and reliably, precision is high for quantitative result.
Embodiment 2
In a kind of food contact material, the assay method of MEHQ migration amount is with embodiment 1, and difference is:
GC conditions:
(1) chromatographic column: coating is polymethyl siloxane material (5% phenyl 95% poly dimethyl arlydene siloxanes), color
Spectrum column length is 60m；Chromatographic column internal diameter is 0.20mm；Coating thickness is: 0.20 μm；
(2) sample size: 0.8 μ L；
(3) temperature programming condition: initial temperature 60 DEG C, is warming up to 240 DEG C with the speed of 20 DEG C/min；
(4) flow rate of carrier gas: 0.8mL/min.
Triple quadrupole bar tandem mass spectrum condition:
(1) ion source: electron impact ion source (EI)；
(2) ion source temperature: 250 DEG C；
(3) electron energy: 70eV；
(4) carrier gas control model: constant current mode；
(5) detection mode: polyion reaction monitoring (MRM)；
(6) solvent delay: 4min；
(7) carrier gas: purity is the helium of 99.9992%；
(8) resolution: unit resolution.
Under ion source, MEHQ is cracked, obtain fragment ion is analyzed, through corresponding ginseng
Number optimizes, and present invention selection wherein 123.9 ＞ 109.0 and 123.9 81.0 two pairs of ions of ＞ are as para hydroxybenzene first
The monitoring ion of ether, collision energy such as table 1 below:
The collision energy of table 1 MEHQ
Embodiment 3
In a kind of food contact material, the assay method of MEHQ migration amount is with embodiment 1, and difference is:
GC conditions:
(1) chromatographic column: coating is polydimethyl siloxane material, chromatogram column length is 15m；Chromatographic column internal diameter is
0.32mm；Coating thickness is: 1 μm；
(2) sample size: 2.0 μ L；
(3) temperature programming condition: initial temperature 60 DEG C, is warming up to 180 DEG C with the speed of 5 DEG C/min, keeps 2min；
(4) flow rate of carrier gas: 2.0mL/min.
Triple quadrupole bar tandem mass spectrum condition:
(1) ion source: electron impact ion source (EI)；
(2) ion source temperature: 250 DEG C；
(3) electron energy: 70eV；
(4) carrier gas control model: constant current mode；
(5) detection mode: polyion reaction monitoring (MRM)；
(6) solvent delay: 4min；
(7) carrier gas: purity is the helium of 99.9992%；
(8) resolution: unit resolution.
Under ion source, MEHQ is cracked, obtain fragment ion is analyzed, through corresponding ginseng
Number optimizes, and present invention selection wherein 123.9 ＞ 109.0 and 123.9 81.0 two pairs of ions of ＞ are as para hydroxybenzene first
The monitoring ion of ether, collision energy such as table 1 below:
The collision energy of table 1 MEHQ
The concrete technical scheme being not limited to described in above-described embodiment of the present invention, the technology that all employing equivalents are formed
Scheme is the protection domain of application claims.
Claims (4)
1. the assay method of MEHQ migration amount in a food contact material, it is characterised in that: comprise the following steps:
Step 1: preparing standard working solution, food simulants test solution and blank test solution, standard working solution is by para hydroxybenzene
Water base and the oiliness isobutyltrimethylmethane. standard working solution of at least five kinds of concentration that methyl ether is formulated；Food simulated solution is by Food Contact
Material and food simulants obtain by migrating experiment, including aqueous-based food analogies test solution and oily food analogies test solution；
Blank test solution is the food simulants not contacted with food contact material；
Step 2: use gas chromatogram-series connection triple quadrupole bar GC-MS GC-MS/MS three kinds of solution difference to step 1
Carry out GC-MS/MS analysis；With concentration x of MEHQ as abscissa, with the corresponding quota ion peak area y recorded
For vertical coordinate, draw standard working solution regression curve, the linear equation y=ax+b obtained according to curve, calculate recurrence song
The slope a of line and intercept b；
Step 3: according to formula c=((yExamination-yEmpty)-b)/a calculates MEHQ concentration c in food simulants test solution, wherein
yExaminationFor MEHQ quota ion peak area in the food simulants test solution that records, yEmptyFor in the blank test solution that records to hydroxyl
Base methyl phenyl ethers anisole quota ion peak area；
Wherein, GC conditions:
(1) chromatographic column: coating is Polyethylene Glycol, polystyrene or polymethyl siloxane material, chromatogram column length is 10-100m；
Chromatographic column internal diameter is 0.20mm-0.60mm；Coating thickness is: 0.1-1.0 μm；
(2) sample size: 0.5-2.0 μ L；
(3) temperature programming condition: initial temperature 40-60 DEG C, keeps 0-4min, is warming up to 160-with the speed of 5-25 DEG C/min
280 DEG C, keep 0-5min；
(4) flow rate of carrier gas: 0.8-1.2mL/min；
Triple quadrupole bar tandem mass spectrum condition:
(1) ion source: electron impact ion source EI or chemical ionization source CI；
(2) ion source temperature: 230-260 DEG C；
(3) electron energy: 65-75eV；
(4) carrier gas control model: constant voltage mode, constant current mode or constant linear velocity pattern；
(5) detection mode: full scan SCAN, selection ion scan SIM or polyion reaction monitoring MRM；
(6) solvent delay: 1-6min；
(7) carrier gas: purity is the helium of 99%-99.9999%；
(8) resolution: unit, wide or widest resolution；
(9) under ion source, MEHQ is cracked, obtain fragment ion is analyzed, excellent through corresponding parameter
Change, select wherein 123.9 ＞ 109.0 and 123.9 81.0 two pairs of ions of ＞ as MEHQ monitoring from
Son.
The assay method of MEHQ migration amount in food contact material the most according to claim 1, its feature exists
In: the collision energy of described MEHQ see table:
The assay method of MEHQ migration amount in food contact material the most according to claim 1, its feature exists
In: the preparation method step of described water base standard working solution is:
(1) MEHQ Standard Stock solutions is prepared: accurately weigh the content MEHQ standard more than 99.0%
Product 25mg to 250mL volumetric flask, with acetone solution the constant volume of chromatographically pure rank, this Standard Stock solutions is kept away at 4 DEG C of lower seals
Light stores；
(2) pipette appropriate MEHQ Standard Stock solutions, be 3% acetic acid solution and body by water, mass concentration respectively
Fraction is 10% ethanol solution constant volume, is configured to the standard working solution of at least five kinds of concentration；
(3) in centrifuge tube, add the water base standard working solution of 10.0mL, add 2.0mL t-butyl methyl ether, vortex oscillation 5 points
4000 revs/min of centrifugations 5 minutes after clock, are carried out upper strata t-butyl methyl ether solution after 0.2 μm nylon leaching film filters
GC-MS/MS analyzes.
The assay method of MEHQ migration amount in food contact material the most according to claim 1, its feature exists
In: the preparation method step of described oiliness standard working solution isobutyltrimethylmethane. is:
(1) MEHQ Standard Stock solutions is prepared: accurately weigh the content MEHQ standard more than 99.0%
Product 25mg to 250mL volumetric flask, with acetone solution the constant volume of chromatographically pure rank, this Standard Stock solutions is kept away at 4 DEG C of lower seals
Light stores；
(2) pipette appropriate MEHQ Standard Stock solutions, use isobutyltrimethylmethane. constant volume, be configured to the mark of at least five kinds of concentration
Quasi-working solution, carries out GC-MS/MS analysis after 0.2 μm nylon leaching film filters.
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| CN114606269A (en) * | 2022-03-17 | 2022-06-10 | 国家食品安全风险评估中心 | High-throughput detection method for genetic toxicity of food contact material migration and application |
| CN116359398A (en) * | 2023-04-26 | 2023-06-30 | 南通百川新材料有限公司 | Method for measuring content of p-hydroxyanisole in acrylic ester product |
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| CN114606269A (en) * | 2022-03-17 | 2022-06-10 | 国家食品安全风险评估中心 | High-throughput detection method for genetic toxicity of food contact material migration and application |
| CN114606269B (en) * | 2022-03-17 | 2024-02-23 | 国家食品安全风险评估中心 | High-throughput detection method for genetic toxicity of food contact material migration object and application |
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