CN104535666A - A method of measuring migration amounts of eighteen phthalic acid esters in a conveyor belt by adopting a gas chromatography-mass spectrometry instrument - Google Patents
A method of measuring migration amounts of eighteen phthalic acid esters in a conveyor belt by adopting a gas chromatography-mass spectrometry instrument Download PDFInfo
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Abstract
The invention relates to a method of measuring migration amounts of eighteen phthalic acid esters in a conveyor belt by adopting a gas chromatography-mass spectrometry instrument. The method includes following steps of: 1) preparing a sample solution to be measured, 2) preparing a standard working solution, 3) performing gas chromatography-mass spectrometry analysis, 4) mapping a standard curve and calculating concentrations of target compounds, and 5) calculating the migration amounts. The method is advantageous in that: 1) the method is rapid in operation, simple and feasible and fills in gasps of migration amount measurement of phthalic acid esters in conveyor belts at present; 2) the method not only strictly inspects safety of the conveyor belt, but also pays attention to simplification of subsequent sample pretreatment processes, and the method is simple and feasible; and 3) the method is high in sensitivity, good in repeatability and good in recovery rate.
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 (Phthalic acid esters, 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 of part PAEs in food contact material is limited the quantity (Specific Migration Limit, 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 adopt gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt determine method, 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 3 cm
2, with 15 mL isooctane as food simulants, after adding interior mark, at 50 DEG C after soak extraction 1 h, 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: 1.0 mL/min;
Heating schedule: initial temperature 60 DEG C, keeps 1 min, with the speed to 220 DEG C of 20 DEG C/min, keeps 1 min, then with the speed to 280 DEG C of 5 DEG C/min, keeps 8 min;
Ionization mode: electron bombardment ionization source;
Ionizing energy: 70 eV;
Transmission line temperature: 280 DEG C;
Ion source temperature: 230 DEG C;
Quadrupole rod temperature: 150 DEG C;
Solvent delay: 6 min;
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 1 mg/kg=6 mg/dm in european union directive 2002/72/EC
2;
Be final measurement result with the mean value of twice replicate determination, be accurate to 0.1 mg/kg.
As preferably, be designated as Ergol in described, concentration is 1 mg/mL.
As preferably, described step 2) preparation method of standard working solution is: accurately take 0.02 g18 kind phthalic ester standard items, be accurate to 0.1 mg, be placed in same 10 mL volumetric flasks, with n-hexane dissolution and constant volume, be mixed with the mixed standard solution I that each phthalic ester concentration is 2 mg/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 0.02 mL, 0.05 mL, 0.1 mL, 0.25 mL, 0.5 mL, 1 mL, 2 mL, 5 mL, be placed in 10 respective mL volumetric flasks, then the inner mark solution that 50 μ L concentration are about 1 mg/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 ~ 0.32 mg/kg, quantitative limit (LOQ) is 0.05 ~ 0.97 mg/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. Agilent 7890A-5975C type); AE163 electronic balance (sensibility reciprocal: 0.0001 g, 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), Chem Service company of the purity >98.0% U.S., normal hexane, isooctane (chromatographically pure, Duksan Pure Chemicals 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 0.02 g(and be accurate to 0.1 mg) 18 kinds of phthalic ester standard items, be placed in same 10 mL volumetric flasks, with n-hexane dissolution and constant volume, be mixed with the mixed standard solution I that each phthalic ester concentration is 2 mg/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 0.02 mL, 0.05 mL, 0.1 mL, 0.25 mL, 0.5 mL, 1 mL, 2 mL, 5 mL, be placed in 10 respective mL volumetric flasks, then the inner mark solution that 50 μ L concentration are about 1 mg/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 3 cm
2(total contact area is about 7.5 cm
2), with 15 mL isooctane as food simulants, after adding interior mark, at 50 DEG C after soak extraction 1 h, 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: 30 mm × 0.25 μm, m × 0.25; 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: 1.0 mL/min; Heating schedule: initial temperature 60 DEG C, keeps 1 min, with the speed to 220 DEG C of 20 DEG C/min, keeps 1 min, then with the speed to 280 DEG C of 5 DEG C/min, keeps 8 min; Ionization mode: electron bombardment ionization source (EI); Ionizing energy: 70 eV; Transmission line temperature: 280 DEG C; Ion source temperature: 230 DEG C; Quadrupole rod temperature: 150 DEG C; Solvent delay: 6 min; 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 1 18 kinds of phthalic esters 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 1 mg/kg=6 mg/dm2 in european union directive 2002/72/EC.
Be final measurement result with the mean value of twice replicate determination, be accurate to 0.1 mg/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 2, 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 2, 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 0.02-0.32 mg/kg, be quantitatively limited to 0.05-0.97 mg/kg.
Linear equation, detection limit and the quantitative limit of table 2 18 kinds of phthalic esters
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 3.As known from Table 3, 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 3 18 kinds of phthalic esters and average relative standard deviation
Claims (3)
1. one kind adopt gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt determine method, 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 3 cm
2, with 15 mL isooctane as food simulants, after adding interior mark, at 50 DEG C after soak extraction 1 h, 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: 1.0 mL/min;
Heating schedule: initial temperature 60 DEG C, keeps 1 min, with the speed to 220 DEG C of 20 DEG C/min, keeps 1 min, then with the speed to 280 DEG C of 5 DEG C/min, keeps 8 min;
Ionization mode: electron bombardment ionization source;
Ionizing energy: 70 eV;
Transmission line temperature: 280 DEG C;
Ion source temperature: 230 DEG C;
Quadrupole rod temperature: 150 DEG C;
Solvent delay: 6 min;
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 1 mg/kg=6 mg/dm in european union directive 2002/72/EC
2;
Be final measurement result with the mean value of twice replicate determination, be accurate to 0.1 mg/kg.
2. the assay method according to claims 1, is characterized in that: be inside designated as Ergol, and concentration is 1 mg/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 0.02 g18 kind phthalic ester standard items, be accurate to 0.1 mg, be placed in same 10 mL volumetric flasks, with n-hexane dissolution and constant volume, be mixed with the mixed standard solution I that each phthalic ester concentration is 2 mg/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 0.02 mL, 0.05 mL, 0.1 mL, 0.25 mL, 0.5 mL, 1 mL, 2 mL, 5 mL, be placed in 10 respective mL volumetric flasks, then the inner mark solution that 50 μ L concentration are about 1 mg/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.
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