CN104535666B - A kind of method adopting gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt - Google Patents
A kind of method adopting gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt Download PDFInfo
- Publication number
- CN104535666B CN104535666B CN201410565208.8A CN201410565208A CN104535666B CN 104535666 B CN104535666 B CN 104535666B CN 201410565208 A CN201410565208 A CN 201410565208A CN 104535666 B CN104535666 B CN 104535666B
- Authority
- CN
- China
- Prior art keywords
- phthalate
- phthalic
- solution
- concentration
- kinds
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention relates to a kind of method adopting gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt.The method sample adopts isooctane to be food simulants, soaks 1h, analyzes through gas chromatograph-mass spectrometer (GCMS) to target compound, inner mark method ration at 50 DEG C.18 kinds of phthalic esters can be effectively separated in 30min, and object is at good (the R2 & gt of 0.04 ~ 10 μ g/mL internal linear relation; 0.995), 3 mark-on levels (0.2,0.5 and 1 μ g/mL) average recovery of standard addition between 93.77 ~ 106.54%, average relative standard's deviation (RSD) is 1.40% ~ 6.59%, detection limit (LOD) is 0.02 ~ 0.32mg/kg, quantitative limit (LOQ) is 0.05 ~ 0.97mg/kg, and experimental result shows that the method is simple to operate, highly sensitive, reproducible, is applicable to the mensuration of 18 kinds of phthalic ester migration amounts in travelling belt.
Description
Technical field
The present invention relates to electronic cigarette product physical and chemical inspection technical field, be specially 18 kinds of phthalic ester migration amounts in a kind of employing gas chromatography/mass spectrometry travelling belt.
Background technology
Phthalic ester (Phthalicacidesters, PAEs) also known as phthalate ester, it is the class endocrine disruption hormone being subject to extensive concern, cell mutation can be caused, canceration and teratogenesis, be proved in toxicologic study in vitro to have and intend weak estrogen action, can cause damage to male reproductive system, cause a series of male reproduction toxicity performance such as Serum testosterone concentrations decline, the minimizing of Sperm specific enzyme quantity, genital malformation, and increase the incidence of disease of women with breast cancer.PAEs is often used as sealing articles for use in the industrial production, and softening agent and plasticiser are widely used in all kinds of chemical products such as crisper, polybag, plastic toy, medical apparatus, lubricant, cosmetics.PAEs adsorbability and compatibility are comparatively strong, and are generally be present in polymkeric substance in the mode of physisorption instead of chemical bonding usually used as the phthalic ester of plasticiser, therefore, under certain condition, easily move out and entered environment from carrier.Within 2011, Taiwan plasticiser disturbance gets more and more people's extensive concerning by the Product quality and safety that PAEs is relevant.At present, many countries start to pay close attention to PAEs and to food, move from food contact material the harm brought, and the specific transfer limitation (SpecificMigrationLimit to part PAEs in food contact material, SML) be limited, such as european union directive 2007/19/EC specifies that the specific transfer limitation of 5 kinds of PAEs is: butyl benzyl phthalate (BBP, 30mg/kg), dibutyl phthalate (DBP, 0.3mg/kg), phthalic acid (2-ethyl) own ester (DEHP, 1.5mg/kg), diisononyl phthalate (DINP, 9mg/kg), di-n-octyl phthalate (DNOP, 9mg/kg).
At present, quantifier elimination is moved to food contact material PAEs both at home and abroad and mainly concentrate on plastics and paper wrapper etc.The advantages such as travelling belt conveyor is means of production in Category I transmitting devices, has applied widely, and transport capacity is large, and circuit is flexible, stable, thus at grain, food, chemical industry, the industries such as metallurgy are used widely.Travelling belt be in travelling belt conveyor directly with the part being transmitted thing and contacting, and as potential food contact material, people not yet make correlative study to its PAEs migration amount.
Summary of the invention
In order to solve above-mentioned technical matters, the object of this invention is to provide the gas chromatography-mass spectrography assay method of 18 kinds of phthalic ester migration amounts in a kind of travelling belt.The detection method that this method provides, has pre-treatment simply effective, quantitatively accurately, reproducible, and highly sensitive and advantage that the recovery is good, for the quality safety assessment of travelling belt provides technical support.
In order to realize above-mentioned object, the object of the invention is to be achieved through the following technical solutions:
A kind of method adopting gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt, 18 kinds of described phthalic esters are repefral, diethyl phthalate, diallyl phthalate, diisobutyl phthalate, dibutyl phthalate, phthalic acid two (2-methoxyl) ethyl ester, phthalic acid two (4-methyl-2-amyl group) ester, phthalic acid two (2-ethoxy) ethyl ester, diamyl phthalate, dihexylphthalate, butyl benzyl phthalate, phthalic acid two (2-butoxy) ethyl ester, dicyclohexyl phthalate, phthalic acid (2-ethyl) own ester, diphenyl phthalate, di-n-octyl phthalate, dinonyl phthalate and diisononyl phthalate, the method comprises the following steps:
1) preparation of testing sample solution: sample cleaned by detersive, after tap water, then dries with after ultrapure water three times, for subsequent use; Immersion test: cut part representative in travelling belt sample, area is 3cm
2, with 15mL isooctane as food simulants, after adding interior mark, at 50 DEG C after soak extraction 1h, get supernatant liquid through 0.45 μm of organic phase filtering with microporous membrane, be testing sample solution;
2) preparation of standard working solution: the hybrid standard working solution with normal hexane preparation with 18 kinds of phthalic esters of concentration gradient, concentration range is 0.04 ~ 10 μ g/mL;
3) gas chromatography-mass spectrometry analysis: utilize gas chromatograph-mass spectrometer (GCMS) to carry out analysis to above-mentioned made testing sample solution and standard solution and detect, obtain related colour spectrogram; Described gas chromatography-mass spectrum condition is:
Adopt capillary chromatographic column, Stationary liquid: 5% phenyl/95% methyl polysiloxane, specification: 30m × 0.25mm × 0.25 μm;
Injector temperature: 280 DEG C;
Sample size: 1 μ L, split sampling, split ratio: 10:1;
Carrier gas: helium (purity >=99.999%), constant current mode, flow velocity: 1.0mL/min;
Heating schedule: initial temperature 60 DEG C, keeps 1min, with the speed to 220 DEG C of 20 DEG C/min, keeps 1min, then with the speed to 280 DEG C of 5 DEG C/min, keeps 8min;
Ionization mode: electron bombardment ionization source;
Ionizing energy: 70eV;
Transmission line temperature: 280 DEG C;
Ion source temperature: 230 DEG C;
Quadrupole rod temperature: 150 DEG C;
Solvent delay: 6min;
Mensuration mode: Selective ion mode surveillance style scans;
4) Specification Curve of Increasing and target compound concentration calculate: the phthalic ester hybrid standard working solution of the variable concentrations prepared is introduced gas chromatograph-mass spectrometer (GCMS), quantitative test is carried out with internal standard method, target compound and the peak area ratio of interior mark compound and the concentration of target compound are carried out linear regression analysis, obtain typical curve equation of linear regression, related coefficient need be more than or equal to 0.999; The sample of preparation is measured, records the peak area ratio of target compound and interior mark compound in sample, substitute into unary linear regression equation, calculate the concentration of phthalic ester in solution to be measured;
5) move gauge to calculate: in travelling belt sample, the migration amount of 18 kinds of phthalic esters is with following formulae discovery:
In formula:
X
i---target analytes migration amount, unit is milligrams per kilogram;
C
i---target analyte concentration in soak solution, unit is micrograms per millilitre;
C
0---target analyte concentration in blank assay, unit is micrograms per millilitre;
The volume of V---soak solution, unit is for rising;
The contact area of S---sample and food simulants, unit is square decimeter.
6---specify 1mg/kg=6mg/dm in european union directive 2002/72/EC
2;
Be final measurement result with the mean value of twice replicate determination, be accurate to 0.1mg/kg.
As preferably, be designated as Ergol in described, concentration is 1mg/mL.
As preferably, described step 2) preparation method of standard working solution is: accurately take 0.02g18 kind phthalic ester standard items, be accurate to 0.1mg, be placed in same 10mL volumetric flask, with n-hexane dissolution and constant volume, be mixed with the mixed standard solution I that each phthalic ester concentration is 2mg/mL, after diluting 100 times, be mixed with the mixed standard solution II that each phthalic ester concentration is 20 μ g/mL; Accurately pipette the mixed standard solution II of 0.02mL, 0.05mL, 0.1mL, 0.25mL, 0.5mL, 1mL, 2mL, 5mL, be placed in respective 10mL volumetric flask, then the inner mark solution that 50 μ L concentration are about 1mg/mL is accurately added, be settled to scale with normal hexane, obtain the series standard working solution that concentration range is 0.04 ~ 10 μ g/mL.
The present invention establishes the gas chromatography-mass spectrography assay method of 18 kinds of phthalic ester migration amounts in a kind of travelling belt, has the following advantages:
1. the present invention establishes a kind of 18 kinds of phthalic ester migration quantitative analysis methods in Simultaneously test travelling belt first, operates quick, simple, and has filled up the blank of phthalic ester migration quantitative determination in current travelling belt.
2. the material directly contacted with travelling belt is fat food or the product such as grain, food, plastics mainly, adopt isooctane be in food simulants Imitation conveyance band PAEs to the migration situation of contact material, strictly can investigate the security of travelling belt, also can take into account the easy of subsequent sample pretreatment process, method is simple.
3. the inventive method three mark-on levels (0.2,0.5 and 1 μ g/mL) average recovery of standard addition between 93.77 ~ 106.54%, average relative standard's deviation (RSD) is 1.40% ~ 6.59%, detection limit (LOD) is 0.02 ~ 0.32mg/kg, quantitative limit (LOQ) is 0.05 ~ 0.97mg/kg, this shows that the method is highly sensitive, repeatability and the recovery good.
Accompanying drawing explanation
Fig. 1 is 18 kinds of phthalic esters and interior target standard solution SIM chromatogram.
Fig. 2 is actual sample chromatogram.
Embodiment
The present invention is further described by following instantiation, but does not limit the present invention.
Embodiment 1
1. instrument and reagent
Instrument: gas chromatograph-mass spectrometer (GCMS) (U.S. Agilent7890A-5975C type); AE163 electronic balance (sensibility reciprocal: 0.0001g, Mettler company of Switzerland); Biochemical cultivation case (essence is grand).
Reagent: 18 kinds of phthalic esters and interior mark standard items: repefral (DMP), diethyl phthalate (DEP), diallyl phthalate (DAP), diisobutyl phthalate (DIBP), dibutyl phthalate (DBP), phthalic acid two (2-methoxyl) ethyl ester (DMEP), phthalic acid two (4-methyl-2-amyl group) ester (BMPP), phthalic acid two (2-ethoxy) ethyl ester (DEEP), diamyl phthalate (DPP), dihexylphthalate (DHXP), butyl benzyl phthalate (BBP), phthalic acid two (2-butoxy) ethyl ester (DBEP), dicyclohexyl phthalate (DCHP), phthalic acid (2-ethyl) own ester (DEHP), diphenyl phthalate (BP), di-n-octyl phthalate (DNOP), dinonyl phthalate (DNP), diisononyl phthalate (DINP), Ergol (BB, interior mark, IS), ChemService company of the purity >98.0% U.S., normal hexane, isooctane (chromatographically pure, DuksanPureChemicals company of Korea S), experimental water is the made ultrapure water of Milli-Q pure water system.
2. the preparation of standard working solution
Accurately take 0.02g (being accurate to 0.1mg) 18 kinds of phthalic ester standard items, be placed in same 10mL volumetric flask, with n-hexane dissolution and constant volume, be mixed with the mixed standard solution I that each phthalic ester concentration is 2mg/mL, after diluting 100 times, be mixed with the mixed standard solution II that each phthalic ester concentration is 20 μ g/mL.Accurately pipette the mixed standard solution II of 0.02mL, 0.05mL, 0.1mL, 0.25mL, 0.5mL, 1mL, 2mL, 5mL, be placed in respective 10mL volumetric flask, then the inner mark solution that 50 μ L concentration are about 1mg/mL is accurately added, be settled to scale with normal hexane, obtain the series standard working solution that concentration range is 0.04 ~ 10 μ g/mL.
3. sample pre-treatments:
Sample pretreatment: sample cleaned by detersive, after tap water, then dries with after ultrapure water three times, for subsequent use; Immersion test: cut part representative in travelling belt sample, area is 3cm
2(total contact area is about 7.5cm
2), with 15mL isooctane as food simulants, after adding interior mark, at 50 DEG C after soak extraction 1h, get supernatant and directly carry out GS/MS analysis.
4. gas chromatography-mass spectrum condition
Chromatographic column: capillary chromatographic column, Stationary liquid: 5% phenyl/95% methyl polysiloxane, specification: 30m × 0.25mm × 0.25 μm; Injector temperature: 280 DEG C; Sample size: 1 μ L, split sampling (split ratio: 10:1); Carrier gas: helium (purity >=99.999%), constant current mode, flow velocity: 1.0mL/min; Heating schedule: initial temperature 60 DEG C, keeps 1min, with the speed to 220 DEG C of 20 DEG C/min, keeps 1min, then with the speed to 280 DEG C of 5 DEG C/min, keeps 8min; Ionization mode: electron bombardment ionization source (EI); Ionizing energy: 70eV; Transmission line temperature: 280 DEG C; Ion source temperature: 230 DEG C; Quadrupole rod temperature: 150 DEG C; Solvent delay: 6min; Mensuration mode: Selective ion mode surveillance style (SIM) scans.
For guaranteeing the sensitivity of analytical approach and reducing matrix interference, have employed Selective ion mode scan pattern (SIM), and select interference minimum, responding relatively strong ion is quantitative and qualitative analysis ion, and the quantitative and qualitative ion of 18 kinds of phthalic esters and internal standard compound is as shown in table 1.
Table 118 kind of phthalic ester and the quantitative and qualitative ion table of internal standard compound
5. Specification Curve of Increasing and target compound content calculate: the phthalic ester hybrid standard working solution of the variable concentrations prepared is introduced gas chromatograph-mass spectrometer (GCMS), quantitative test is carried out with internal standard method, target compound and the peak area ratio of interior mark compound and the concentration of target compound are carried out linear regression analysis, obtain typical curve equation of linear regression, related coefficient need be more than or equal to 0.999.The sample of preparation is measured, records the peak area ratio of target compound and interior mark compound in sample, substitute into unary linear regression equation, calculate the content of phthalic ester in solution to be measured.
6. move gauge to calculate: in travelling belt sample, the migration amount of 18 kinds of phthalic esters is with following formulae discovery:
In formula:
X
i---target analytes migration amount, unit is milligrams per kilogram (mg/kg);
C
i---target analyte concentration in soak solution, unit is micrograms per millilitre (μ g/mL);
C
0---target analyte concentration in blank assay, unit is micrograms per millilitre (μ g/mL);
The volume of V---soak solution, unit is for rising (L);
The contact area of S---sample and food simulants, unit is square decimeter (dm2).
6---specify 1mg/kg=6mg/dm2 in european union directive 2002/72/EC.
Be final measurement result with the mean value of twice replicate determination, be accurate to 0.1mg/kg.4. standard working curve and result calculate
7. the range of linearity of method, detection limit and quantitative limit
The standard working solution of preparation 18 kinds of phthalic esters, regretional analysis is carried out with internal standard compound and its respective concentration of chromatographic peak area comparison after GC-MS analyzes, draw typical curve and regression equation, related coefficient, calibration curve, as shown in table 1, and be detection limit when utilizing signal to noise ratio (S/N ratio) to be 3, be quantitative limit when signal to noise ratio (S/N ratio) is 10.As shown in Table 1, the chromatographic condition adopted makes 18 kinds of phthalate compounds and interior mark all be separated well, and all there is good correlativity (R2>0.9950), detect and be limited to 0.02-0.32mg/kg, be quantitatively limited to 0.05-0.97mg/kg.
Linear equation, detection limit and the quantitative limit of table 118 kind of phthalic ester
8. the recovery of method and precision
This method is adopted to carry out recovery of standard addition experiment, get 3 parts, travelling belt sample, respectively according to low (about 0.2 μ g/mL), in (about 0.5 μ g/mL), high (about 1 μ g/mL) three kinds of levels add 18 kinds of phthalic ester standard items, each Pitch-based sphere replication 5 samples, and by adding scalar and the mark-on measured quantity calculating recovery, the results are shown in Table 2.As known from Table 2, the average recovery of standard addition of 18 kinds of phthalic esters is between 93.77 ~ 106.54%, and average relative standard's deviation (RSD) is 1.40%-6.59%, shows that this method accuracy is high, reproducible, is applicable to quantitatively.
The recovery of standard addition of table 218 kind of phthalic ester and average relative standard deviation
Claims (3)
1. the method adopting gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt, 18 kinds of described phthalic esters are repefral, diethyl phthalate, diallyl phthalate, diisobutyl phthalate, dibutyl phthalate, phthalic acid two (2-methoxyl) ethyl ester, phthalic acid two (4-methyl-2-amyl group) ester, phthalic acid two (2-ethoxy) ethyl ester, diamyl phthalate, dihexylphthalate, butyl benzyl phthalate, phthalic acid two (2-butoxy) ethyl ester, dicyclohexyl phthalate, phthalic acid (2-ethyl) own ester, diphenyl phthalate, di-n-octyl phthalate, dinonyl phthalate and diisononyl phthalate, it is characterized in that the method comprises the following steps:
1) preparation of testing sample solution: sample cleaned by detersive, after tap water, then dries with after ultrapure water three times, for subsequent use; Immersion test: cut part representative in travelling belt sample, area is 3cm
2, with 15mL isooctane as food simulants, after adding interior mark, at 50 DEG C after soak extraction 1h, get supernatant liquid through 0.45 μm of organic phase filtering with microporous membrane, be testing sample solution;
2) preparation of standard working solution: the hybrid standard working solution with normal hexane preparation with 18 kinds of phthalic esters of concentration gradient, concentration range is 0.04 ~ 10 μ g/mL;
3) gas chromatography-mass spectrometry analysis: utilize gas chromatograph-mass spectrometer (GCMS) to carry out analysis to above-mentioned made testing sample solution and standard solution and detect, obtain related colour spectrogram; Described gas chromatography-mass spectrum condition is:
Adopt capillary chromatographic column, Stationary liquid: 5% phenyl/95% methyl polysiloxane, specification: 30m × 0.25mm × 0.25 μm; Injector temperature: 280 DEG C;
Sample size: 1 μ L, split sampling, split ratio: 10:1;
Carrier gas: helium, purity >=99.999%, constant current mode, flow velocity: 1.0mL/min;
Heating schedule: initial temperature 60 DEG C, keeps 1min, with the speed to 220 DEG C of 20 DEG C/min, keeps 1min, then with the speed to 280 DEG C of 5 DEG C/min, keeps 8min;
Ionization mode: electron bombardment ionization source;
Ionizing energy: 70eV;
Transmission line temperature: 280 DEG C;
Ion source temperature: 230 DEG C;
Quadrupole rod temperature: 150 DEG C;
Solvent delay: 6min;
Mensuration mode: Selective ion mode surveillance style scans;
4) Specification Curve of Increasing and target compound concentration calculate: the phthalic ester hybrid standard working solution of the variable concentrations prepared is introduced gas chromatograph-mass spectrometer (GCMS), quantitative test is carried out with internal standard method, target compound and the peak area ratio of interior mark compound and the concentration of target compound are carried out linear regression analysis, obtain typical curve equation of linear regression, related coefficient need be more than or equal to 0.999; The sample of preparation is measured, records the peak area ratio of target compound and interior mark compound in sample, substitute into unary linear regression equation, calculate the concentration of phthalic ester in solution to be measured;
5) move gauge to calculate: in travelling belt sample, the migration amount of 18 kinds of phthalic esters is with following formulae discovery:
In formula:
X
i---target analytes migration amount, unit is milligrams per kilogram;
C
i---target analyte concentration in soak solution, unit is micrograms per millilitre;
C
0---target analyte concentration in blank assay, unit is micrograms per millilitre;
The volume of V---soak solution, unit is for rising;
The contact area of S---sample and food simulants, unit is square decimeter;
6---specify 1mg/kg=6mg/dm in european union directive 2002/72/EC
2;
Be final measurement result with the mean value of twice replicate determination, be accurate to 0.1mg/kg.
2. the assay method according to claims 1, is characterized in that: be inside designated as Ergol, and concentration is 1mg/mL.
3. the assay method according to claims 1, it is characterized in that: step 2) preparation method of standard working solution is: accurately take 0.02g18 kind phthalic ester standard items, be accurate to 0.1mg, be placed in same 10mL volumetric flask, with n-hexane dissolution and constant volume, be mixed with the mixed standard solution I that each phthalic ester concentration is 2mg/mL, after diluting 100 times, be mixed with the mixed standard solution II that each phthalic ester concentration is 20 μ g/mL; Accurately pipette the mixed standard solution II of 0.02mL, 0.05mL, 0.1mL, 0.25mL, 0.5mL, 1mL, 2mL, 5mL, be placed in respective 10mL volumetric flask, then the inner mark solution that 50 μ L concentration are about 1mg/mL is accurately added, be settled to scale with normal hexane, obtain the series standard working solution that concentration range is 0.04 ~ 10 μ g/mL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410565208.8A CN104535666B (en) | 2015-02-11 | 2015-02-11 | A kind of method adopting gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410565208.8A CN104535666B (en) | 2015-02-11 | 2015-02-11 | A kind of method adopting gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104535666A CN104535666A (en) | 2015-04-22 |
| CN104535666B true CN104535666B (en) | 2016-01-27 |
Family
ID=52851236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410565208.8A Active CN104535666B (en) | 2015-02-11 | 2015-02-11 | A kind of method adopting gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104535666B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105021755B (en) * | 2015-07-03 | 2016-11-09 | 中华人民共和国台州出入境检验检疫局 | Liquid Chromatography/Mass Spectrometry 7 kinds of benzene polyacid of detection and derivative specific transfer metering method thereof |
| CN105954436A (en) * | 2016-07-21 | 2016-09-21 | 常州工学院 | Method for measuring transporting quantity of para-hydroxy benzaldehyde in food contact material |
| CN106404934A (en) * | 2016-08-25 | 2017-02-15 | 宁波检验检疫科学技术研究院 | Method for detecting phthalic acid di-n-propyl ester in washing product |
| CN108226085A (en) * | 2018-01-09 | 2018-06-29 | 广州伯朗氏检测技术有限公司 | The method that Fourier transform Attenuated Total Reflect ion Infrared Spectroscopy measures dimethicone the amount of migration in pre-encapsulated injector sub-assembly |
| CN111624282A (en) * | 2020-07-03 | 2020-09-04 | 成都市食品药品检验研究院 | Method for detecting phthalate substances in self-heating hot pot packaging inner box |
| CN113466396B (en) * | 2021-06-23 | 2024-09-17 | 山东省产品质量检验研究院 | Method for detecting migration quantity of plasticizer in skin contact material |
| CN113504333B (en) * | 2021-08-20 | 2023-03-14 | 上海烟草集团有限责任公司 | Method for detecting organic matter migration amount in paper packaging material |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101493440A (en) * | 2008-08-06 | 2009-07-29 | 通标标准技术服务（天津）有限公司 | Method for measuring migration volume of phthalic ester and di(2-ethylhexyl) adipate in fatty foodstuff contact material |
| CN102183591A (en) * | 2011-02-10 | 2011-09-14 | 云南烟草科学研究院 | Test method for analyzing migration condition of chemical constituents in cigarette tipping paper |
| CN102539555A (en) * | 2011-12-16 | 2012-07-04 | 暨南大学 | Method for measuring migration amount of harmful substances in printing ink |
| CN102914614A (en) * | 2012-11-07 | 2013-02-06 | 云南烟草科学研究院 | Method for screening saliva stimulant influencing transfer volume of phthalate in paper cup mouth touching material |
| CN102928537A (en) * | 2012-11-07 | 2013-02-13 | 云南烟草科学研究院 | Method for screening phthalate migration volume impact factors in material of mouth touch portion of paper cup |
| CN103424489A (en) * | 2013-08-22 | 2013-12-04 | 常州进出口工业及消费品安全检测中心 | Method for measuring diallyl phthalate migration in food contact materials |
| CN103913518A (en) * | 2012-12-31 | 2014-07-09 | 天士力制药集团股份有限公司 | Method for detecting content of plasticizer in white spirit and application thereof in detection of migration rate of plasticizer |
-
2015
- 2015-02-11 CN CN201410565208.8A patent/CN104535666B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101493440A (en) * | 2008-08-06 | 2009-07-29 | 通标标准技术服务（天津）有限公司 | Method for measuring migration volume of phthalic ester and di(2-ethylhexyl) adipate in fatty foodstuff contact material |
| CN102183591A (en) * | 2011-02-10 | 2011-09-14 | 云南烟草科学研究院 | Test method for analyzing migration condition of chemical constituents in cigarette tipping paper |
| CN102539555A (en) * | 2011-12-16 | 2012-07-04 | 暨南大学 | Method for measuring migration amount of harmful substances in printing ink |
| CN102914614A (en) * | 2012-11-07 | 2013-02-06 | 云南烟草科学研究院 | Method for screening saliva stimulant influencing transfer volume of phthalate in paper cup mouth touching material |
| CN102928537A (en) * | 2012-11-07 | 2013-02-13 | 云南烟草科学研究院 | Method for screening phthalate migration volume impact factors in material of mouth touch portion of paper cup |
| CN103913518A (en) * | 2012-12-31 | 2014-07-09 | 天士力制药集团股份有限公司 | Method for detecting content of plasticizer in white spirit and application thereof in detection of migration rate of plasticizer |
| CN103424489A (en) * | 2013-08-22 | 2013-12-04 | 常州进出口工业及消费品安全检测中心 | Method for measuring diallyl phthalate migration in food contact materials |
Non-Patent Citations (4)
| Title |
|---|
| Petersen, J. H.;Jensen, L. K.Phthalates and food-contact materials: enforcing the 2008 European Union plastics legislation.《FOOD ADDITIVES AND CONTAMINANTS》.2010,第27卷(第11期),1608-1616. * |
| 与食品接触的塑料成型品中邻苯二甲酸酯类增塑剂迁移量的测定;孙利, 陈志锋， 雍伟, 储晓刚;《中国卫生检验杂志》;20080331;第18卷(第3期);393-396 * |
| 快餐和早点包装中邻苯二甲酸酯类塑化剂迁移风险的研究;祝惠惠，罗世鹏，刘君峰，商贵芹，陈明;《食品安全质量检测学报》;20141130;第5卷(第11期);3571-3575 * |
| 气相色谱-质谱法同时测定橡塑材料中18种邻苯二甲酸酯类增塑剂;何芃;《塑料工业》;20100930;第38卷(第9期);60-64 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104535666A (en) | 2015-04-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104535666B (en) | A kind of method adopting gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt | |
| CN112345651B (en) | Method for determining content of halogenated acid in chloral hydrate or preparation thereof | |
| Fries | Determination of benzothiazole in untreated wastewater using polar-phase stir bar sorptive extraction and gas chromatography–mass spectrometry | |
| Kucharska et al. | Development of a broad spectrum method for measuring flame retardants-overcoming the challenges of non-invasive human biomonitoring studies | |
| Vichi et al. | Determination of volatile thiols in lipid matrix by simultaneous derivatization/extraction and liquid chromatography–high resolution mass spectrometric analysis. Application to virgin olive oil | |
| Fan et al. | Determination of the migration of 20 phthalate esters in fatty food packaged with different materials by solid-phase extraction and UHPLC–MS/MS | |
| CN104359998B (en) | A kind of gas chromatography tandem mass spectrometry detects the method for methyl mesylate | |
| Dong et al. | Matrix effects in detection of phthalate esters from wheat by a modified QuEChERS method with GC/MS | |
| CN103308640A (en) | Gas chromatography-mass spectrometry combined detection method for 17 phthalate compounds in printing ink | |
| CN109991349A (en) | The detection method of benzene-like compounds content in food contact material | |
| Xie et al. | An efficient method for determining the acid value in edible oils by solvent-assisted headspace gas chromatography | |
| CN103926354B (en) | Gas chromatography-mass spectrometry determination method for six phthalates in hot melt adhesive | |
| CN103091418B (en) | Method for detecting plasticizing agent | |
| Ly-Verdu et al. | A passive sampling-based analytical strategy for the determination of volatile organic compounds in the air of working areas | |
| CN103926352B (en) | Extraction standard correction-gas chromatography-mass spectrography the assay method of 12 kinds of phthalic esters in a kind of hot melt adhesive | |
| CN111272900B (en) | Gas chromatography analysis method for detecting content of 3-chloro-2, 2-dimethyl-1-propanol | |
| Fan et al. | Method development for the simultaneous analysis of trans, trans-muconic acid, 1, 2-dihydroxybenzene, S-phenylmercapturic acid and S-benzylmercapturic acid in human urine by liquid chromatography/tandem mass spectrometry | |
| CN105628815A (en) | Method for determining trace ethyl carbamate in fermented food | |
| Liao et al. | Rapid measurement of Phthalic acid Ester environmental hormones using ion mobility spectrometry | |
| CN109856283B (en) | Analysis method of butyl ester components in water-based adhesive for cigarette packaging | |
| CN102095815A (en) | Method for determining musk xylene in washing products | |
| CN107356698B (en) | 2- picoline and method for quantitatively determining while N-serve in a kind of sample | |
| CN103293265A (en) | Gas chromatography-mass spectrometry combined detection method for 17 phthalate compounds in stay wire for cigarettes | |
| Pandohee et al. | Evaluation of new micro solid-phase extraction cartridges for on-column derivatisation reactions | |
| CN110988189A (en) | Method for rapidly determining phthalate plasticizer in beverage |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |