CN105823850A - Method for detecting content of bisphenol A in coiled material sample - Google Patents
Method for detecting content of bisphenol A in coiled material sample Download PDFInfo
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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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- G01N30/74—Optical detectors
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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
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Abstract
The invention provides a method for detecting the content of bisphenol A in a coiled material sample .The method includes the steps that 1, the coiled material sample is cut into hand samples, wherein the hand samples are three rectangular hand samples with the size of 100 mm*20 mm; 2, the two sides of each of the three hand samples are soaked in 60-100 ml of distilled water, extraction is conducted for 2 hours at the temperature of 70 DEG C, and then an extracting solution containing bisphenol A is obtained; 3, the extracting solution is subjected to liquid chromatographic analysis, and the content of bisphenol A in the coiled material sample is determined .By means of the detection method in the embodiment, the content of bisphenol A in milk product plastic packing materials (especially polycarbonate packing materials)-coiled materials can be easily, conveniently, rapidly and accurately detected at high sensitivity.
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 web sample.
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 packaging material for food 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 packaging material web of detection rapidly and accurately.
In a first aspect of the present invention, the present invention proposes and a kind of detects the method for content of bisphenol A in web sample.According to this
Inventive embodiment, described method includes: web sample is cut into sample by (1), and described sample is 100 millimeter of * 20 milli
The rectangle sample of rice；(2) the two-sided of three pieces of described samples is all immersed in 100ml distilled water, and carry under 70 degrees Celsius
Take 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 the content of bisphenol-A in described web sample.According to embodiments of the invention, in described sample the content of bisphenol-A be with
The quality representation of the bisphenol-A contained in unit are sample.Utilize the detection method of the embodiment of the present invention, it is possible to easy,
Quickly, the content of bisphenol-A in milk product plastics packaging material (especially Merlon packaging material)-coiled material accurately and is with sensitivity detected.
According to embodiments of the invention, said method can further include at least one following additional technical feature:
According to embodiments of the invention, described sample is by carrying out cutting by the rectangle sample of 100 millimeters × 60 millimeters
Arrive.According to embodiments of the invention, the rectangle sample size of 100 millimeters × 60 millimeters is true based on GB test principle
Fixed, and then by the rectangle sample of 100 millimeters × 60 millimeters being carried out the sample of cutting acquisition three pieces 100 millimeters × 20 millimeters,
In this, as the sample of extraction bisphenol-A, the accuracy of the content of bisphenol A recorded improves further, and acquired results is more nearly
The real content of bisphenol-A in testing sample.
According to embodiments of the invention, in step (2), two-sided by three pieces of described samples is all immersed in 100ml distilled water,
And extract 2 hours under 70 degrees Celsius, in order to obtain the extracting solution containing bisphenol-A.100ml distilled water can abundant submergence institute
State three pieces of samples, and then the accuracy of the content of bisphenol A recorded improves further.
According to embodiments of the invention, described determine that in web sample, the content of bisphenol-A realizes in the following way: when
When the thickness of described sample is less than or equal to 0.25 millimeter, determined in described web sample by formula QA=Cs × 100/1.2
The content of bisphenol-A, wherein, QA represents the quality of the bisphenol-A contained in described unit are sample, and unit is mg/dm2,
Cs represents the concentration of the bisphenol-A in extracting solution, and unit is mg/ml；When the thickness of described sample is more than 0.25 millimeter, logical
Crossing formula QA=(Cs × 25)/(1.2 × d) and determine the content of bisphenol-A in described web sample, wherein, QA represents
The quality of the bisphenol-A contained in described unit are sample, unit is that mg/dm2, Cs represent the bisphenol-A in extracting solution
Concentration, unit is the thickness that mg/ml, d represent described sample, and unit is millimeter.Utilize above-mentioned side according to embodiments of the present invention
Method calculates the quality of bisphenol-A in web sample unit are, represents the content of bisphenol-A, the standard of acquired results in web sample
Exactness improves further, and acquired results is closer to the content of bisphenol-A in coiled material.
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 0.9990, 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 and a kind of detects the method for content of bisphenol A in web sample.
According to embodiments of the invention, described method includes: web sample is cut into sample by (1), and described sample is 100 millimeters
* the rectangle sample of 60 millimeters；(2) described sample cutting into three pieces of samples, described sample is 100 millimeters * 20 millimeters
Rectangle sample；(3) the two-sided of described three fast samples is all immersed in 100ml distilled water, and under 70 degrees Celsius, extract 2
Hour；(4) 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, wherein, 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；(5) by containing that step (3) is obtained
The extracting solution of bisphenol-A carries out described liquid-phase chromatographic analysis, determines the concentration of bisphenol-A in described extracting solution；And (6)
Being determined as follows the content of bisphenol-A in described web sample, wherein, the content of described bisphenol-A is with unit are
The quality representation of the bisphenol-A contained in sample, when the thickness of described sample is less than or equal to 0.25 millimeter, described formula
For QA=Cs × 100/1.2, wherein, QA represents the quality of the bisphenol-A contained in described unit are sample, the list of QA
Position is the concentration that mg/dm2, Cs represent the bisphenol-A in described extracting solution, and the unit of Cs is mg/ml；When described sample
When thickness is more than 0.25 millimeter, described formula is QA=(Cs × 25)/(1.2 × 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 thickness that mg/ml, d represent described sample, and the unit of d is mm.The present invention is utilized to implement
The detection method of example, it is possible to simplicity, quickly, accurately and with sensitivity detection milk product plastics packaging material (especially Merlon
Packaging material) content of bisphenol-A in-coiled material.
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 web sample that detects that the embodiment of the present invention is proposed is particularly well-suited to
Net content/specification is that (the packed packaging material of flexible package is producing the packed web sample of the flexible package of 400g or 400g (16*25g)
For package before processing, so be called coiled material at this) detection.The method that the embodiment of the present invention is proposed is applied to net content/rule
Lattice are the coiled material that the flexible package of 400g or 400g (16*25g) is packed, and the accuracy recording result improves, more further
The real content of bisphenol-A in sample.
Embodiment 1
Will be described in detail containing of bisphenol-A in milk product plastics packaging material (especially Merlon packaging material)-coiled material in the present embodiment
Detection method, step and the material of amount.
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 and (are accurate to
0.1mg) in 100mL volumetric flask, by methanol constant volume, matching while using.
1.4 bisphenol-A standard intermediate liquids ((37.5mg/L): compound method is as follows, take 10mL bisphenol-A standard reserving solution in
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, 0.30
The standard working solution of mg/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
It is 0.6dm that web sample cutter are cut into 100mm × 60mm area2Sample, then this sample is cut
Become the sample of three pieces of 100mm × 20mm.The above-mentioned sample cut is put in 150ml triangular flask, adds 100ml
Distilled water, in 70 DEG C of water-baths extract 2 hours, 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 use
The standard curve of external standard method carries out sample correction.
3.4 results calculate
3.4.1 packaging material thickness≤0.25mm, QA=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 area of A: sample, unit is dm2；
3.4.2 packaging material thickness 0.25mm, QA=(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 area of A: sample, unit is dm2；
The thickness of d: testing sample, unit is mm.
3.4.3 sample area calculates
Surface area=the length of coiled material × wide=10cm × 6cm=60cm2=0.6dm2.All need because coiled material is two-sided to be immersed in water extraction,
Therefore surface area is by two-sided calculating, is 0.6 × 2=1.2dm2。
So bisphenol-A quality Q A contained in unit are material in web sample can be calculated in the following way: when
Packaging material thickness≤0.25mm QA=Cs × 100/1.2；
As packaging material thickness 0.25mm QA=(Cs × 25)/(1.2 × 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
Coiled material mark-on sample, carries out response rate experiment detection, and 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 85%～105%, illustrates method described in embodiment 1
Accuracy 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 energy of method described in embodiment 1 is described
Enough needs meeting 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 coiled material that the bisphenol-A mark liquid that test coiled material is 0.06mg/L of selection processed.Migrate experiment knot
Fruit is as shown in table 3:
Table 3
By table 3 data it will be seen that in the case of coiled material surface is long-pending necessarily, determine that water base amount is more at 60-100mL
Scientific and reasonable, and inventor is in discovery in process of the test, and the coiled material sample of three pieces of 100mm × 20mm puts into 150ml
In triangular flask, the distilled water adding 100ml is more applicable, it is possible to by three pieces of whole submergences of sample to be measured, and then be preferably added to
The volume of distilled water is 100ml.
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 (7)
1. one kind is detected the method for content of bisphenol A in web sample, it is characterised in that including:
(1) web sample is cut into sample, described sample be 100 millimeters × 20 millimeters rectangle sample；
(2) the two-sided of three pieces of described samples is all immersed in 60～100ml distilled water, and extracts 2 hours under 70 degrees Celsius,
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 web sample.
Method the most according to claim 1, it is characterised in that described sample is by by 100 millimeters × 60 millimeters
Rectangle sample carry out cutting and obtain.
Method the most according to claim 1, it is characterised in that in step (2), double by three pieces of described samples
Face is all immersed in 100ml distilled water, and extracts 2 hours under 70 degrees Celsius, in order to obtain the extracting solution containing bisphenol-A.
Method the most according to claim 1, it is characterised in that described determine that in web sample, the content of bisphenol-A is logical
Cross what following manner realized:
When the thickness of described sample is less than or equal to 0.25 millimeter, determine described coiled material sample by formula QA=Cs × 100/1.2
The content of bisphenol-A in product, wherein, QA represents the quality of the bisphenol-A contained in described unit are sample, and Cs represents and carries
Take the concentration of bisphenol-A in liquid；
When the thickness of described sample is more than 0.25 millimeter, determined described by formula QA=(Cs × 25)/(1.2 × d)
The content of bisphenol-A in web sample, wherein, QA represents the quality of the bisphenol-A contained in described unit are sample,
Cs represents the concentration of the bisphenol-A in extracting solution, and 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 5, it is characterised in that the concentration of the bisphenol-A in described extracting solution is by such as
Under type 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.
7. one kind is detected the method for content of bisphenol A in web sample, it is characterised in that including:
(1) web sample cutting into sample, described sample is the rectangle sample of 100 millimeters * 60 millimeters；
(2) described sample cutting into three pieces of samples, described sample is the rectangle sample of 100 millimeters * 20 millimeters；
(3) the two-sided of described three fast samples is all immersed in 100ml distilled water, and extract 2 hours under 70 degrees Celsius；
(4) 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, wherein, 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；
(5) extracting solution containing bisphenol-A that step (3) is obtained is carried out described liquid-phase chromatographic analysis, determine described in carry
Take the concentration of bisphenol-A in liquid；And
(6) be determined as follows the content of bisphenol-A in described web 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 or equal to 0.25 millimeter, described formula is QA=Cs × 100/1.2, wherein, QA
Representing the quality of the bisphenol-A contained in described unit are sample, the unit of QA is mg/dm2, Cs represents described extraction
The concentration of the bisphenol-A in liquid, the unit of Cs is mg/ml；
When the thickness of described sample is more than 0.25 millimeter, described formula is QA=(Cs × 25)/(1.2 × d), wherein,
QA represents the quality of the bisphenol-A contained in described unit are sample, and the unit of QA is mg/dm2, Cs represent described in carry
Taking the concentration of bisphenol-A in liquid, the unit of Cs is the thickness that mg/ml, d represent described sample, and the unit of d is mm.
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| 中国国家标准化管理委员会等: "GB/T 23296.1-2009 食品接触材料 塑料中受限物质 塑料中物质向食品及食品模拟物特定迁移试验和含量测定方法以及食品模拟物暴露条件选择的指南", 《中华人民共和国国家标准 GB/T 23296.1-2009》 * |
| 中国国家标准化管理委员会等: "GB/T 23296.16-2009 食品接触材料 高分子材料 食品模拟物中2,2-二（4-羟基苯基）丙烷（双酚A）的测定 高效液相色谱法", 《中华人民共和国国家标准 GB/T 23296.16-2009》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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