CN106093214A - Detect the method for content of bisphenol A in tinned packaging material sample - Google Patents
Detect the method for content of bisphenol A in tinned packaging material sample Download PDFInfo
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- CN106093214A CN106093214A CN201610351658.6A CN201610351658A CN106093214A CN 106093214 A CN106093214 A CN 106093214A CN 201610351658 A CN201610351658 A CN 201610351658A CN 106093214 A CN106093214 A CN 106093214A
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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
- G01N2030/027—Liquid chromatography
Abstract
The present invention proposes and a kind of detects the method for content of bisphenol A in milk product tinned packaging material sample, the method includes: (1) injects distilled water in described tinned packaging material sample, and extract 2 hours under 70 degrees Celsius, to obtain the extracting solution containing bisphenol-A, wherein, described distilled water is 4.5～0.5 centimetres with the distance of tinned packaging material end face, preferably 0.5 centimetre；And (2) carry out liquid-phase chromatographic analysis to described extracting solution, determine the content of bisphenol-A in described tinned packaging material sample.Utilize the detection method of the embodiment of the present invention, it is possible to the content of bisphenol-A in simplicity, quickly, accurately and with sensitivity detection milk product plastics packaging material (especially Merlon packaging material) tinned packaging material.
Description
Technical field
The present invention relates to field of food, in particular it relates to content of bisphenol A in detection milk product tinned packaging material sample
Method.
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, divides
Son amount 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 cries again
Make Merlon, be the important derivatives of important Organic Chemicals, phenol and acetone, mainly for the production of Merlon
(PC), the multiple macromolecular material such as epoxy resin, polysulfone resin, polyphenylene oxide resin, unsaturated polyester resin.BPA is ubiquitous,
From mineral water bottle, medical apparatus and instruments to and packaging for foodstuff inside, have its figure.
Research shows, manufacture plastic containers PC material may discharge poisonous bisphenol-A, the highest release of temperature the more,
Rate of release is 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 present invention
One purpose is to propose the content of bisphenol A in a kind of milk product plastic package material-tinned packaging material of detection rapidly and accurately
Method.
In a first aspect of the present invention, the present invention proposes content of bisphenol A in a kind of detection milk product tinned packaging material sample
Method.According to embodiments of the invention, described method includes: (1) injects distilled water in described tinned packaging material sample, and in
Extract 2 hours under 70 degrees Celsius, in order to obtain the extracting solution containing bisphenol-A, wherein, described distilled water and tinned packaging material end face
Distance is 0.5～4.5 centimetre, preferably 0.5 centimetre；And (2) carry out liquid-phase chromatographic analysis to described extracting solution, determine described in listen
The content of bisphenol-A in dress packaging material sample.According to embodiments of the invention, in described sample, the content of bisphenol-A is with unit are
The quality representation of the bisphenol-A contained in sample.Utilize the detection method of the embodiment of the present invention, it is possible to easy, quickly, accurately and
The content of bisphenol-A in detection milk product plastics packaging material (especially Merlon packaging material)-tinned packaging material with sensitivity.
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 determine in tinned packaging material sample that the content of bisphenol-A is real in the following way
Existing: 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, 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 the volume that mg/ml, V represent described distilled water, and the unit of V is
Ml, A represent 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, pass through formula
QA=(Cs × V × 0.25)/(A × d) determines the content of bisphenol-A in described tinned packaging material sample, and wherein, QA represents described unit
The quality of the bisphenol-A contained in area sample, unit is mg/dm2, Cs represents the concentration of the bisphenol-A in extracting solution, and unit is
Mg/ml, V represent the volume of described distilled water, and the unit of V is the surface area that ml, A represent described sample, and the unit of A is dm2, d
Representing the thickness of described sample, unit is millimeter.Said method according to embodiments of the present invention is utilized to calculate tinned packaging material sample
The quality of bisphenol-A in unit are, represents the content of bisphenol-A in tinned packaging material sample, and the accuracy of acquired results carries further
Height, acquired results is close to the content of bisphenol-A in tinned packaging 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；Post
Temperature is room temperature；The excitation wavelength 227 of fluorescence detector, launches wavelength 313.The above-mentioned liquid chromatograph utilizing the embodiment of the present invention is examined
The testing result that the condition surveyed is obtained is stable, and detection sensitivity is high.
According to embodiments of the invention, the concentration of the bisphenol-A being determined as follows in described extracting solution: by liquid phase color
Analysis of spectrum result contrasts with standard curve, and described standard curve is true based on standard working solution is carried out liquid-phase chromatographic analysis
Fixed, 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
0.00mg/L、0.03mg/L、0.06mg/L、0.15mg/L、0.30mg/L、0.75mg/L.According to embodiments of the invention, upper
State under liquid phase chromatogram condition, the detection standard working solution containing bisphenol-A standard substance, and then draw the mark of peak area-bisphenol A concentration
Directrix curve, the correlation coefficient of gained standard curve is more than 0.9990, and linear relationship is good.According to embodiments of the invention, upper
State under liquid phase chromatogram condition, the peak area that in the extracting solution that detection obtains, bisphenol-A is corresponding, and then by obtained peak area and mark
Directrix curve contrasts, and can obtain is the concentration of bisphenol-A in extracting solution.According to embodiments of the present invention above-mentioned is utilized to determine extracting solution
In the method for concentration of bisphenol-A, the accuracy of the result obtained improves further.
Specifically, in a second aspect of the present invention, the present invention proposes in a kind of detection milk product tinned packaging material sample double
The method of phenol A content.According to embodiments of the invention, described method includes: (1) injects distillation in described tinned packaging material sample
Water, and extract 2 hours under 70 degrees Celsius, in order to obtain the extracting solution containing bisphenol-A, wherein, described extracting solution and tinned bag
The distance of material end face is 0.5 centimetre；(2) standard working solution is carried out liquid-phase chromatographic analysis, in order to draw the concentration-peak of bisphenol-A
The standard curve of area, in described standard working solution the concentration of bisphenol-A standard substance be 0.00mg/L, 0.03mg/L, 0.06mg/L,
0.15mg/L、0.30mg/L、0.75mg/L；(3) extracting solution containing bisphenol-A that step (2) is obtained is carried out described liquid phase
Chromatography, determines the concentration of bisphenol-A in described extracting solution, wherein, in step (2) and (3), described liquid-phase chromatographic analysis
Condition be: the column length 250mm of chromatographic column, internal diameter is 4.6mm, and granularity is 5 μm；Flowing is the methanol of 70:30 for volume ratio mutually
Mixed solution with water；Flow velocity is 1.0mL/min；Column temperature is room temperature；The excitation wavelength 227 of fluorescence detector, launches wavelength
313；And (4) are determined as follows the content of bisphenol-A in described tinned packaging material sample, wherein, the content of described bisphenol-A
It is 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
Formula is QA=Cs × V/A, and wherein, 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, and the unit of Cs is the volume that mg/ml, V represent described distilled water,
The unit of V is the surface area that ml, A represent described sample, and the unit of A is dm2；When the thickness of described sample is more than 0.25 millimeter
Time, described formula is QA=(Cs × V × 0.25)/(A × d), and wherein, QA represents the bis-phenol contained in described unit are sample
The quality of A, the unit of QA is mg/dm2, Cs represents the concentration of the bisphenol-A in described extracting solution, and the unit of Cs is mg/ml, V table
Showing the volume of described distilled water, the unit of V is the surface area that ml, A represent described sample, and the unit of A is dm2, d represents described sample
The thickness of product, the unit of d is mm.Utilize the detection method of the embodiment of the present invention, it is possible to easy, quickly, accurately and with sensitivity
The content of bisphenol-A in detection milk product plastics packaging material (especially Merlon packaging material)-tinned packaging 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 this
Bright, and be not considered as limiting the invention.Unreceipted concrete technology or condition in embodiment, according to the literary composition in this area
Offer described technology or condition or carry out according to product description.Agents useful for same or instrument unreceipted production firm person, all
For can by city available from conventional products.
It should be noted that content of bisphenol A in the detection milk product tinned packaging material sample that proposed of the embodiment of the present invention
Method is particularly well-suited to the detection that specification is 900g or 180g milk product tinned packaging material sample.The side that the embodiment of the present invention is proposed
Method is applied to the detection that specification is 900g or 180g milk product tinned packaging material content of bisphenol A, and the accuracy recording result is further
Improve, be closer to the real content of bisphenol-A in sample.
Embodiment 1
Will be described in detail in milk product plastics packaging material (especially Merlon packaging material)-tinned packaging material double in the present embodiment
The detection method of the content of phenol A, 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 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 microsyringe 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 in water double
Phenol A concentration is respectively the standard work of 0.00mg/L, 0.03mg/L, 0.06mg/L, 0.15mg/L, 0.30mg/L, 0.75mg/L
Liquid.
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
In tinned packaging material, add distilled water, the height distance that adds water end face 0.5cm, extract 2 hours in 70 DEG C of water-baths,
The sample liquid extracted 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 is vertical coordinate, draws standard curve, and 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 external standard method
Standard curve carry out sample correction.
3.4 results calculate
3.4.1 packaging material thickness≤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 area of A: sample, unit is dm2；
3.4.2 packaging material thickness 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 area of A: sample, unit is dm2；
The thickness of d: testing sample, unit is mm.
3.4.3 surface area of sample calculates
The most existing tinned packaging material is divided into two kinds of 900g and 180g, and is cylindrical, so the table of tinned packaging material
Area can be by calculated as below, surface area=3.14r2Wherein, r is radius to+2 × 3.14 × r × h, and h is high,
Tinned packaging material (900g): high 16.5cm, radius 6.4cm is due to the height distance end face 0.5cm that adds water, then actual high
Degree is 16cm, and then surface area is 771.69cm2, i.e. 7.72dm2, add water volume and be about 2000ml.
Tinned packaging material (180g): high 11cm, radius 3.75cm, due to the height distance end face 0.5cm that adds water, then actual height
For 10.5cm, and then area is 291.43cm2, i.e. 2.91dm2, add water volume and be about 450ml.
So bisphenol-A quality Q A contained in unit are material in the most existing tinned packaging material sample can be by such as
Under type is calculated:
For tinned packaging material (900g), when packaging material thickness≤0.25mm QA=Cs × 2000/7.72；
As packaging material thickness 0.25mm QA=(Cs × 500)/(7.72 × d).
For tinned packaging material (180g), when packaging material thickness≤0.25mm QA=Cs × 450/2.91；
As packaging material thickness 0.25mm QA=(Cs × 112.5)/(2.91 × 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-hydroxyl
Base phenyl) the mensuration high performance liquid chromatography of propane (bisgallic acid A) " in regulation to detection limit, by the method described by embodiment 1
Detection limit be set to 0.03mg/L, prepare the listening of three Concentraton gradient of 0.06mg/L, 0.15mg/L, 0.3mg/L the most respectively
Dress packaging 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, in table, the response rate of mark-on sample is all between 76.7%～98.6%, and embodiment 1 is described
The accuracy of described method can meet the needs of detection.
Embodiment 3 Precision Experiment
Compound concentration is mark-on sample Parallel testing 6 times, testing result such as table 2 and the table respectively of 0.15mg/L, 0.3mg/L
Shown in 3.
Table 2
Table 3
From table 2 and table 3, the standard deviation RSD% of parallel laboratory test is less than 10%, method described in embodiment 1 is described
Precision 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 to food and food
The guide that the test of product analogies specific transfer and content assaying method and food simulants exposure condition select " in restricted substances
Analysis, generally represent with limited component limitation QMA, i.e. with in every 6 square decimeters of plastic table areas containing the maximum of this material
Milligram 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 logical
Cross adjustment surface area-to-volume ratio carry out analysis mode thing and then obtain more preferably material concentration.This test have employed full immersion
Method carries out migration test to the sample with otch.Requirement in testing according to specific transfer, test result is with " mg/dm2" table
Show.
In the present embodiment, the tinned packaging material of the test of selection (180g) is listening of processing of the bisphenol-A mark liquid of 0.15mg/L
Dress packaging material, the tinned packaging material that the bisphenol-A mark liquid that tinned packaging material (900g) is 0.30mg/L of selection processed.Migrate experimental result
As shown in table 3:
Table 3:
By data above it will be seen that in the case of tinned packaging material (180g) surface area is certain, determine that water base amount exists
300-450mL, distance packaging material end face 4.5 centimetres～0.5 centimetre is the most scientific and reasonable；At tinned packaging material (900g) surface area one
In the case of Ding, determine that water base amount, at 1500-2000mL, is that more science is closed apart from packaging material end face 4.5 centimetres～0.5 centimetre
Reason；But find in process of the test, at tinned packaging material (180g) and tinned packaging material (900g), add the steaming of 450ml and 2000mL
Distilled water is more applicable, greatly reduces the risk factor brought owing to liquid level is on the low side, product material is uneven, and then for listening
Dress packaging material (180g) is preferably added to 450ml distilled water, is preferably added to 2000ml distilled water, distilled water for tinned packaging material (900g)
It it is 0.5 centimetre with the distance of packaging material end face.
In the description of this specification, reference term " embodiment ", " some embodiments ", " example ", " specifically show
Example " or the description of " some examples " etc. means to combine this embodiment or example describes specific features, structure, material or spy
Point is contained at least one embodiment or the example of the present invention.In this manual, to the schematic representation of above-mentioned term not
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, the skill of this area
The feature of the different embodiments described in this specification or example and different embodiment or example can be tied by art personnel
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 example
Property, it is impossible to being interpreted as limitation of the present invention, those of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, revises, replaces and modification.
Claims (5)
1. one kind is detected the method for content of bisphenol A in milk product tinned packaging material sample, it is characterised in that including:
(1) in described tinned packaging material sample, inject distilled water, and extract 2 hours under 70 degrees Celsius, in order to obtain containing double
The extracting solution of phenol A, wherein, described distilled water is 0.5～4.5 centimetre with the distance of tinned packaging material end face, preferably 0.5 centimetre；With
And
(2) described extracting solution is carried out liquid-phase chromatographic analysis, determine the content of bisphenol-A in described tinned packaging material sample.
Method the most according to claim 1, it is characterised in that be determined as follows in described tinned packaging material sample double
The content of phenol 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 in extracting solution
The concentration of bisphenol-A, V represents the volume of described distilled water, and A represents the surface area of described sample；
When described sample thickness more than 0.25 millimeter time, by formula QA=(Cs × V × 0.25)/(A × d) determine described in listen
The content of bisphenol-A in dress packaging material 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, and d represents described sample
Thickness.
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 by as follows
Mode 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
0.00mg/L、0.03mg/L、0.06mg/L、0.15mg/L、0.30mg/L、0.75mg/L。
5. one kind is detected the method for content of bisphenol A in tinned packaging material sample, it is characterised in that including:
(1) in described tinned packaging material sample, inject distilled water, and extract 2 hours under 70 degrees Celsius, in order to obtain containing double
The extracting solution of phenol A, wherein, described extracting solution is 0.5 centimetre with the distance of tinned packaging material end face；
(2) 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, described
In 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；
(3) extracting solution containing bisphenol-A that step (1) is obtained is carried out described liquid-phase chromatographic analysis, determine described extracting solution
In the concentration of bisphenol-A, wherein, in step (2) and (3), 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
(4) be determined as follows the content of bisphenol-A in described tinned packaging material 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 formula is QA=Cs × V/A, and wherein, QA represents described unit
The quality of the bisphenol-A contained in area sample, 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, and the unit of V is the surface area that ml, A represent described sample, the list of A
Position is dm2；
When the thickness of described sample is more than 0.25 millimeter, described formula is QA=(Cs × V × 0.25)/(A × d), wherein, QA
Representing the quality of the bisphenol-A contained in described unit are sample, the unit of QA is mg/dm2, Cs represents in described extracting solution
The concentration of bisphenol-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 sample
Surface area, the unit of A is dm2, d represents the thickness of described sample, and the unit of d is mm.
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| 陈娟 等: "玩具中苯酚和双酚A的高效液相色谱-荧光检测方法研究", 《分析科学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109975466A (en) * | 2017-12-28 | 2019-07-05 | 厦门市产品质量监督检验院 | The detection method of bisphenol-A in a kind of shopping receipt |
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