CN105929076A - Method for detecting content of bisphenol A in measuring spoon samples - Google Patents
Method for detecting content of bisphenol A in measuring spoon samples Download PDFInfo
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- CN105929076A CN105929076A CN201610351576.1A CN201610351576A CN105929076A CN 105929076 A CN105929076 A CN 105929076A CN 201610351576 A CN201610351576 A CN 201610351576A CN 105929076 A CN105929076 A CN 105929076A
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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
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- G01N2030/027—Liquid chromatography
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Abstract
The invention provides a method for detecting content of bisphenol A in measuring spoon samples. The method comprises the steps that firstly, the measuring spoon samples are cut into small sample bodies, wherein the small sample bodies are spoon bodies and handle bodies, all of which are obtained respectively by cutting the two measuring spoon samples; secondly, two faces of each spoon body and two faces of each handle body are immersed into 1,00 ml of distilled water and extracted for 2 hours at the temperature of 70 DEG C, and an extracting solution containing the bisphenol A is acquired; thirdly, liquid chromatogram analysis is carried out on the extracting solution, and the content of bisphenol A in the measuring spoon samples is determined. By means of the detection method, the content of bisphenol A in dairy product plastic (especially makrolon packing materials) measuring spoons can be easily, conveniently, quickly, accurately and high-sensitively detected.
Description
Technical field
The present invention relates to field of food, in particular it relates to the method for content of bisphenol A in detection limit scoop sample product.
Background technology
Bisphenol-A, formal name used at school 2,2-bis-(4-hydroxy phenyl) propane, English name 2,2-bis (4-hydroxyphenyl) propane；
Bisphenol A, for white needle-like crystals, fusing point 156～158 DEG C, boiling point 250-252 DEG C, flash-point 79.4 DEG C, molecular weight
228, density 1.195, water insoluble, it is dissolved in acetone, is heated to when 180 DEG C decompose.Bisphenol-A is also referred to as BPA, industrial
It is called again Merlon, is the important derivatives of important Organic Chemicals, phenol and acetone, mainly for the production of poly-carbon
The multiple macromolecular materials such as acid esters (PC), epoxy resin, polysulfone resin, polyphenylene oxide resin, unsaturated polyester resin.BPA
Ubiquitous, from mineral water bottle, medical apparatus and instruments to and packaging for foodstuff inside, have its figure.
Research shows, the PC material manufacturing plastic containers may discharge poisonous bisphenol-A, and the highest release of temperature the more, is released
Put speed the fastest.Bisphenol-A can precipitate in the middle of F&B when heating, and it may upset body metabolism process, right
Infant development, immunity have an impact, the most carcinogenic.
And then, detect the content of bisphenol-A in food material the most rapidly and accurately particularly important.
Summary of the invention
It is contemplated that one of technical problem solved the most to a certain extent in correlation technique.To this end, the one of the present invention
The method that purpose is to propose the content of bisphenol A in a kind of milk product plastics measuring spoon of detection rapidly and accurately.
In a first aspect of the present invention, the present invention proposes a kind of method of content of bisphenol A in detection limit scoop sample product.According to this
Inventive embodiment, described method includes: 2 measuring spoon samples are respectively cut into spoon and handle by (1)；(2) by described spoon and
Handle two-sided all immerse 60～100ml, in preferably 100ml distilled water, and under 70 degrees Celsius extract 2 hours, in order to
Obtain the extracting solution containing bisphenol-A；And (3) carry out liquid-phase chromatographic analysis to described extracting solution, determine described measuring spoon sample
The content of bisphenol-A in product.According to embodiments of the invention, in described sample, the content of bisphenol-A is with in unit are sample
The quality representation of the bisphenol-A contained.Utilize the detection method of the embodiment of the present invention, it is possible to easy, quick, accurate and high
The content of bisphenol-A in detection milk product plastics (especially Merlon) measuring spoon delicately.
According to embodiments of the invention, said method can further include at least one following additional technical feature:
According to embodiments of the invention, it is determined as follows the content of bisphenol-A in described measuring spoon sample: when described sample
Thickness less than or equal to 0.25 millimeter time, determine bisphenol-A in described tinned packaging material sample by formula QA=Cs × V/A
Content, wherein, QA represents the quality of the bisphenol-A contained in described unit are sample, and unit is mg/dm2, Cs table
Showing the concentration of bisphenol-A in extracting solution, unit is the volume that mg/ml, V represent described distilled water, and the unit of V is ml,
A represents the surface area of described sample, and the unit of A is dm2；When the thickness of described sample is more than 0.25 millimeter, by public affairs
Formula QA=(Cs × V × 0.25)/(A × d) determines the content of bisphenol-A in described tinned packaging material sample, wherein, QA
Representing the quality of the bisphenol-A contained in described unit are sample, unit is mg/dm2, Cs represents the bis-phenol in extracting solution
The concentration of A, unit is the volume that mg/ml, V represent described distilled water, and the unit of V is that ml, A represent described sample
Surface area, the unit of A is dm2, d represents the thickness of described sample, and unit is millimeter.Utilize according to embodiments of the present invention
The quality of bisphenol-A in said method amount of calculation scoop sample product unit are, represents the content of bisphenol-A in measuring spoon sample, and gained is tied
The accuracy of fruit improves further, and acquired results is close to the content of bisphenol-A in measuring spoon.
According to embodiments of the invention, the condition of described liquid-phase chromatographic analysis is: the column length 250mm of chromatographic column, and internal diameter is
4.6mm, granularity is 5 μm；Flowing is mutually for the mixed solution of first alcohol and water that volume ratio is 70:30；Flow velocity is 1.0mL/min；
Column temperature is room temperature；The excitation wavelength 227 of fluorescence detector, launches wavelength 313.Utilize the above-mentioned liquid phase color of the embodiment of the present invention
The testing result that the condition of spectrum detection is obtained is stable.Detection sensitivity is high.
According to embodiments of the invention, the concentration of the bisphenol-A in described extracting solution is determined as follows: by liquid phase
Chromatography result contrasts with standard curve, and described standard curve is to carry out liquid-phase chromatographic analysis based on to standard working solution
Determining, described standard working solution is the mixed solution of bisphenol-A standard substance and water, and the concentration of described bisphenol-A standard substance is respectively
For 0.00mg/L, 0.03mg/L, 0.06mg/L, 0.15mg/L, 0.30mg/L, 0.75mg/L.Reality according to the present invention
Execute example, under above-mentioned liquid phase chromatogram condition, the detection standard working solution containing bisphenol-A standard substance, and then drafting peak area-
The standard curve of bisphenol A concentration, the correlation coefficient of gained standard curve is more than 0.999, and linear relationship is good.According to this
Bright embodiment, under above-mentioned liquid phase chromatogram condition, the peak area that in the extracting solution that detection obtains, bisphenol-A is corresponding, and then will
Obtained peak area contrasts with standard curve, and can obtain is the concentration of bisphenol-A in extracting solution.Utilize according to the present invention real
The method executing the concentration of the above-mentioned bisphenol-A determined in extracting solution of example, the accuracy of the result obtained improves further.
Specifically, in a second aspect of the present invention, the present invention proposes a kind of method of content of bisphenol A in detection limit scoop sample product.
According to embodiments of the invention, described method includes: 2 measuring spoon samples are respectively cut into spoon and handle by (1)；(2) by institute
State spoon and handle two-sided all immerse in 100ml distilled water, and extract 2 hours under 70 degrees Celsius；(3) standard is worked
Liquid carries out liquid-phase chromatographic analysis, in order to draw the standard curve of the concentration-peak area of bisphenol-A, bis-phenol in described standard working solution
The concentration of A standard substance is respectively 0.00mg/L, 0.03mg/L, 0.06mg/L, 0.15mg/L, 0.30mg/L, 0.75mg/L；
(4) extracting solution containing bisphenol-A that step (2) is obtained is carried out described liquid-phase chromatographic analysis, determine described extracting solution
In the concentration of bisphenol-A, wherein, in step (3) and (4), the condition of described liquid-phase chromatographic analysis is: chromatographic column
Column length 250mm, internal diameter is 4.6mm, and granularity is 5 μm；Flowing mixing for first alcohol and water that volume ratio is 70:30 mutually
Close solution；Flow velocity is 1.0mL/min；Column temperature is room temperature；The excitation wavelength 227 of fluorescence detector, launches wavelength 313；With
And (5) are determined as follows the content of bisphenol-A in described measuring spoon sample, wherein, the content of described bisphenol-A be with
The quality representation of the bisphenol-A contained in unit are sample, when the thickness of described sample is less than 0.25 millimeter, described public affairs
Formula is QA=Cs × V/A, and wherein, QA represents the quality of the bisphenol-A contained in described unit are sample, the unit of QA
For mg/dm2, Cs represents the concentration of the bisphenol-A in described extracting solution, and the unit of Cs is that mg/ml, V represent described distillation
The volume of water, the unit of V is the surface area that ml, A represent described sample, and the unit of A is dm2；Thickness when described sample
When degree is more than 0.25 millimeter, described formula is QA=(Cs × V × 0.25)/(A × d), and wherein, QA represents described list
Plane amasss the quality of the bisphenol-A contained in sample, and the unit of QA is mg/dm2, Cs represents the bis-phenol in described extracting solution
The concentration of A, the unit of Cs is the volume that mg/ml, V represent described distilled water, and the unit of V is that ml, A represent described
The surface area of sample, the unit of A is dm2, d represents the thickness of described sample, and the unit of d is mm.Utilize the present invention real
Execute the detection method of example, it is possible to easy, detection milk product plastics (especially Merlon) quickly, accurately and with sensitivity
The content of bisphenol-A in measuring spoon.
Accompanying drawing explanation
Fig. 1 is canonical plotting according to embodiments of the present invention.
Detailed description of the invention
Embodiments of the invention are described below in detail.The embodiments described below is exemplary, is only used for explaining the present invention,
And be not considered as limiting the invention.Unreceipted concrete technology or condition in embodiment, according to the document in this area
Described technology or condition or carry out according to product description.Agents useful for same or instrument unreceipted production firm person, be
Can by city available from conventional products.
It should be noted that the method for content of bisphenol A in the detection limit scoop sample product that proposed of the embodiment of the present invention
It is particularly well-suited to the detection to the sample of 6 grams of milk powder spoons of 3 grams of milk powder spoons.The method application that the embodiment of the present invention is proposed
The detection of content of bisphenol A in 3 grams of milk powder spoons to 6 grams milk powder spoon sample, the accuracy recording result is high, close to sample
The real content of middle bisphenol-A.
Embodiment 1
Will be described in detail the detection of the content of bisphenol-A in milk product plastics (especially Merlon) measuring spoon in the present embodiment
Method, step and material.
1 reagent and material
1.1 bisphenol-A standard substance, purity is more than 99.0%.
1.2 Chromatographic Pure Methanol.
1.3 bisphenol-A standard reserving solutions (375mg/L): compound method is as follows, accurately weigh 37.5mg bisphenol-A (accurately
To 0.1mg) in 100mL volumetric flask, by methanol constant volume, matching while using.
1.4 bisphenol-As standard intermediate liquid (37.5mg/L): compound method is as follows, take 10mL bisphenol-A standard reserving solution
In 100mL volumetric flask, use methanol constant volume.
1.5 bisphenol-A standard working solution: compound method is as follows, draw respectively accurately with micropipettor 0 μ L, 20
μ L, 40 μ L, 100 μ L, 200 μ L, 500 μ L bisphenol-A standard intermediate liquids in the volumetric flask of 6 25mL,
Use water constant volume, obtain bisphenol A concentration in water be respectively 0.00mg/L, 0.03mg/L, 0.06mg/L, 0.15mg/L,
The standard working solution of 0.30mg/L, 0.75mg/L.
2 instrument and equipments
2.1 high performance liquid chromatographs, join fluorescence detector.
2.2 analytical balance.
2.3 micropipettors: 10 μ L, 50 μ L, 1000 μ L.
3 detection methods
The preparation of 3.1 water base analogies test solutions
2 amount of plastic scoop sample product are cut or are cut into two parts: a part is spoon, and a part is handle, 2 measuring spoons
As 1 part of sample, this 1 part of sample is put in 150ml triangular flask, add the distilled water of 100ml, in 70 DEG C of water
Extracting 2 hours in bath, the sample liquid of extraction is to be measured.
3.2 chromatographic determinations (HPLC)
Chromatographic column: the column length of post is 250mm, internal diameter is 4.6mm, and granularity is 5 μm, or the analytical column that performance is similar；
Flowing phase: methanol: water=70:30；
Flow velocity: 1.0mL/min；
Column temperature: room temperature；
Fluorescence detector: excitation wavelength 227, launches wavelength 313.
3.3 draw HPLC standard curve
According to the condition determination of 3.2, standard working solution 1.5 is measured, with the concentration of bisphenol-A as abscissa,
With corresponding peak area as vertical coordinate, drawing standard curve, gained standard curve is as it is shown in figure 1, linear equation is
Y=1614196X-81016.The correlation coefficient of this standard curve is more than 0.9990, and linear relationship is good, and then can make
Sample correction is carried out with the standard curve of external standard method.
3.4 results calculate
3.4.1 thickness of sample≤0.25mmQA=Cs × V/A
Wherein, QA: the bisphenol-A quality contained in unit are material, unit is mg/dm2；
Cs: the concentration of the material in release to water base extractant, is calculated by HPLC standard curve, and unit is mg/ml；
V: the volume of water base extractant, unit is ml, is 100ml herein；
The surface area of A: sample, unit is dm2；
3.4.2 thickness of sample 0.25mmQA=(Cs × V × 0.25)/(A × d)
Wherein, QA: the bisphenol-A quality contained in unit are material, unit is mg/dm2；
C: the concentration of the material in release to water base extractant, is calculated by HPLC standard curve, and unit is mg/ml；
V: the volume of water base extractant, unit is ml, is 100ml herein；
The surface area of A: sample, unit is dm2；
The thickness of d: testing sample, unit is mm.
3.4.3 sample area calculates
The surface area of measuring spoon is divided into two parts, and a part is spoon, and a part is bar, two-part surface area separate computations, spoon
Can approximate and calculate by circular cone, bar approximation is pressed rectangle and is calculated.For spoon, reducible for circular cone, deduct with the surface area of big circular cone
The surface area of conicle, conical surface amasss computing formula=3.14 × r × L, and wherein r is radius, and L is that bus is long.
As a example by 3 grams of milk powder spoons on the market and 6 grams of milk powder spoons, the wherein measuring spoon mouth external diameter of 3 grams of milk powder spoons: 2.7cm, amount
Spoon end external diameter 2.2cm, spoon emits high 2.26cm, and handle is long: 8.8cm, handle width: 0.8cm；Outside the measuring spoon mouth of 6 grams of milk powder spoons
Footpath: 3.0cm, external diameter 2.8cm at the bottom of measuring spoon, emit a height of 2.9cm, a length of 9.6cm of handle, a width of 0.8cm of handle.Measuring spoon is also
Originally after being circular cone, great circle cone nut line length 6.8cm, diameter 2.7cm, the long 4.6cm of conicle bus, diameter 2cm, the face of spoon
Long-pending=3.14 × 2.7/2 × 6.8-3.14 × 2/2 × 4.6=14.38cm；For bar, a length of 8.9cm, a width of 0.8cm, area is
14.24cm2.Two parts area adds up to 28.62cm2.It is required for being immersed in water extraction because measuring spoon is two-sided, therefore surface area is pressed
Two-sided calculating, is 28.62 × 2=57.24dm2, it is 0.57dm2
So bisphenol-A quality Q A contained in unit are material in this kind of size quantity scoop sample product can be counted in the following way
Obtain: when packaging material thickness≤0.25mm QA=Cs × 100/0.57；
As packaging material thickness 0.25mm QA=(Cs × 25)/(0.57 × d).
Embodiment 2 response rate is tested
According to GB/T 23296.16-2009 " in food contact material macromolecular material food simulants 2,2-bis-(4-hydroxy benzenes
Base) the mensuration high performance liquid chromatography of propane (bisgallic acid A) " in regulation to detection limit, by the side described by embodiment 1
The detection limit of method is set to 0.03mg/L, prepares three Concentraton gradient of 0.06mg/L, 0.15mg/L, 0.3mg/L the most respectively
Measuring spoon mark-on sample, carry out the response rate experiment detection, testing result is as shown in table 1.
Table 1
As can be seen from Table 1, the response rate of three kinds of mark-on samples, all between 79.2～102.0%, illustrates described in embodiment 1
The accuracy of method can meet the needs of detection.
Embodiment 3 Precision Experiment
Compound concentration is mark-on sample Parallel testing 6 times respectively of 0.15mg/L, and testing result is as shown in table 2.
Table 2
As shown in Table 2, the standard deviation RSD% of parallel laboratory test is less than 10%, and the precision of method described in embodiment 1 is described
Disclosure satisfy that the needs of detection.
Embodiment 4 migrates experiment
According to GB/T 23296.1-2009, " in food contact material plastics, in restricted substances plastics, material is simulated to food and food
The guide that the test of thing specific transfer and content assaying method and food simulants exposure condition select " in the analysis of restricted substances,
Generally represent with limited component limitation QMA, i.e. so that every 6 square decimeters of plastic table areas to contain the maximum milligram of this material
Number (mg/6dm2) represent.
In migration test, it is adaptable to the analysis method of test substance is difficult to reach enough detection limits, and then needs by adjusting
Whole surface area-to-volume ratio is carried out analysis mode thing and then obtains more preferably material concentration.This test have employed full immersion method pair
Sample with otch carries out migration test.Requirement in testing according to specific transfer, test result is with " mg/dm2" represent.
In the present embodiment, the measuring spoon that the bisphenol-A mark liquid that test measuring spoon is 0.06mg/L of selection processed.Migrate experiment knot
Fruit is as shown in table 3:
Table 3
By data above it will be seen that in the case of measuring spoon surface area is certain, determine that water base amount is relatively at 60-100mL
For scientific and reasonable, finding in process of the test, the distilled water of 2 measuring spoon sample immersion 100ml is more applicable.
In the description of this specification, reference term " embodiment ", " some embodiments ", " example ", " concrete example ",
Or specific features, structure, material or the feature that the description of " some examples " etc. means to combine this embodiment or example describes
It is contained at least one embodiment or the example of the present invention.In this manual, need not to the schematic representation of above-mentioned term
Identical embodiment or example must be directed to.And, the specific features of description, structure, material or feature can be in office
One or more embodiments or example combine in an appropriate manner.Additionally, in the case of the most conflicting, this area
The feature of the different embodiments described in this specification or example and different embodiment or example can be tied by technical staff
Close and combination.
Although above it has been shown and described that embodiments of the invention, it is to be understood that above-described embodiment is exemplary,
Being not considered as limiting the invention, those of ordinary skill in the art within the scope of the invention can be to above-described embodiment
It is changed, revises, replaces and modification.
Claims (5)
1. the method for content of bisphenol A in detection limit scoop sample product, it is characterised in that including:
(1) 2 measuring spoon samples are respectively cut into spoon and handle；
(2) described spoon and the two-sided of handle are all immersed 60～100ml, in preferably 100ml distilled water, and under 70 degrees Celsius
Extract 2 hours, in order to obtain the extracting solution containing bisphenol-A；And
(3) described extracting solution is carried out liquid-phase chromatographic analysis, determine the content of bisphenol-A in described measuring spoon sample.
Method the most according to claim 1, it is characterised in that be determined as follows bis-phenol in described measuring spoon sample
The content of A:
When the thickness of described sample is less than or equal to 0.25 millimeter, determine described tinned packaging material by formula QA=Cs × V/A
The content of bisphenol-A in sample, wherein, the quality of the bisphenol-A contained in QA representation unit area sample, Cs represents extraction
The concentration of the bisphenol-A in liquid, V represents the volume of described distilled water, and A represents the surface area of described sample；
When the thickness of described sample is more than 0.25 millimeter, determined by formula QA=(Cs × V × 0.25)/(A × d)
The content of bisphenol-A in described tinned packaging material sample, wherein, the quality of the bisphenol-A contained in QA representation unit area sample,
Cs represents the concentration of the bisphenol-A in extracting solution, and V represents the volume of described distilled water, and A represents the surface area of described sample,
D represents the thickness of described sample.
Method the most according to claim 1, it is characterised in that the condition of described liquid-phase chromatographic analysis is:
The column length 250mm of chromatographic column, internal diameter is 4.6mm, and granularity is 5 μm；
Flowing is mutually for the mixed solution of first alcohol and water that volume ratio is 70:30；
Flow velocity is 1.0mL/min；
Column temperature is room temperature；
The excitation wavelength 227 of fluorescence detector, launches wavelength 313.
Method the most according to claim 3, it is characterised in that the concentration of the bisphenol-A in described extracting solution is to pass through
Following manner determines:
Liquid-phase chromatographic analysis result being contrasted with standard curve, described standard curve is to carry out liquid based on to standard working solution
Analysis of hplc determines, containing bisphenol-A standard substance in described standard working solution, the concentration of described bisphenol-A standard substance is respectively
For 0.00mg/L, 0.03mg/L, 0.06mg/L, 0.15mg/L, 0.30mg/L, 0.75mg/L.
5. the method for content of bisphenol A in detection limit scoop sample product, it is characterised in that including:
(1) 2 measuring spoon samples are respectively cut into spoon and handle；
(2) described spoon and the two-sided of handle are all immersed in 100ml distilled water, and extract 2 hours under 70 degrees Celsius；
(3) standard working solution is carried out liquid-phase chromatographic analysis, in order to draw the standard curve of the concentration-peak area of bisphenol-A,
In described standard working solution the concentration of bisphenol-A standard substance be respectively 0.00mg/L, 0.03mg/L, 0.06mg/L, 0.15mg/L,
0.30mg/L、0.75mg/L；
(4) extracting solution containing bisphenol-A that step (2) is obtained is carried out described liquid-phase chromatographic analysis, determine described in carry
Take the concentration of bisphenol-A in liquid,
Wherein, in step (3) and (4), the condition of described liquid-phase chromatographic analysis is:
The column length 250mm of chromatographic column, internal diameter is 4.6mm, and granularity is 5 μm；
Flowing is mutually for the mixed solution of first alcohol and water that volume ratio is 70:30；
Flow velocity is 1.0mL/min；
Column temperature is room temperature；
The excitation wavelength 227 of fluorescence detector, launches wavelength 313；And
(5) being determined as follows the content of bisphenol-A in described measuring spoon sample, wherein, the content of described bisphenol-A is
With the quality representation of bisphenol-A that contains in unit are sample,
When the thickness of described sample is less than 0.25 millimeter, described formula is QA=Cs × V/A, and wherein, QA represents described
The quality of the bisphenol-A contained in unit are sample, the unit of QA is mg/dm2, it is double that Cs represents in described extracting solution
The concentration of phenol A, the unit of Cs is the volume that mg/ml, V represent described distilled water, and the unit of V is that ml, A represent institute
Stating the surface area of sample, the unit of A is dm2；
When the thickness of described sample is more than 0.25 millimeter, described formula is QA=(Cs × V × 0.25)/(A × d), its
In, QA represents the quality of the bisphenol-A contained in described unit are sample, and the unit of QA is mg/dm2, Cs represents
The concentration of the bisphenol-A in described extracting solution, the unit of Cs is the volume that mg/ml, V represent described distilled water, the unit of V
Represent the surface area of described sample for ml, A, the unit of A is dm2, d represents the thickness of described sample, and the unit of d is
mm。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107144499A (en) * | 2017-05-16 | 2017-09-08 | 东莞出入境检验检疫局检验检疫综合技术中心 | The research method of bisphenol-A Transport in simulated body fluid in ABS plastic toy |
| CN108037223A (en) * | 2017-12-13 | 2018-05-15 | 中山永恒检测科技有限公司 | The detection method of bisphenol-A in a kind of paint |
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