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This standard replaces "Determination of Phthalate Esters in Food Plastic Packaging Materials" (GB/T 21928-2008) and "Determination the Migration of Phthalates in Plastic Articles Intended to Come into Contact With Foodstuffs - GC/MS" (SN/T 2037-2007).
Compared with GB/T 21928-2008 and SN/T 2037-2007, the main changes in this standard are as follows:
——the title of standard is modified to " National Food Safety Standard - Food Contact Materials and Articles - Determination of the Content and Migration of Phthalate Esters";
——the applicable scope is modified;
——the determination method is modified;
——the detection limit is modified.
Contents
1 Scope 1
2 Principle 1
3 Reagents and Materials 1
4 Instruments and Apparatus 2
5 Analysis Procedure 3
6 Expression of Analytic Result 5
7 Precision 5
8 Others 5
9 Principle 5
10 Reagents and Materials 6
11 Instruments and Apparatus 6
12 Analysis Procedure 7
13 Expression of Analytic Result 8
14 Precision 9
15 Others 9
Annex A 18 Common Phthalate Esters Plasticizers 10
Annex B Quantitive and Qualitative Selective Ions for Phthalate Esters Compounds 11
Annex C GC-MS TIC of Phthalate Esters Standard Sample Solution 12
National Food Safety Standard
Food Contact Materials and Articles-
Determination of the Content and Migration of Phthalate Esters
1 Scope
This Standard specifies method of determination of the content and migration of phthalate esters in materials in contact with foodstuffs and their products.
This Standard is applicable to determination of the content of phthalate esters in food plastic packaging materials and their products as well as the migration of phthalate esters in materials in contact with foodstuffs and their products.
Determination of Content of Phthalate Esters
2 Principle
Mill food plastic packaging material and its product, perform ultrasonic treatment with normal hexane, filter the extract, and conduct the determination by gas chromatography-mass spectrometry method (GC/MS). Adopt selected ion monitor mode (SIM), determine the chemical composition according to retention time and fragment abundance ratio, and determine the amount by external standard method.
3 Reagents and Materials
Unless otherwise specified, all reagents used in this method are chromatographically pure (or analytically pure after double distillation). The water used shall be the water that is redistilled with full-glass apparatus and stored in a glass vessel.
3.1 Reagents
3.1.1 Normal hexane (C6H14).
3.1.2 Acetone (CH3COCH3).
3.2 Phthalate esters standard products
Dimethyl phthalate (DMP), diethyl phthalate (DEP), diethyl phthalate (DAP), diisobutyl phthalate (DIBP), dibutyl phthalate (DBP), bis (2-methoxyethyl) phthalate (DMEP), bis (4-methyl-2-pentyl) phthalate (BMPP), bis(2-ethoxyethyl) phthalate (DEEP), diamyl phthalate (DPP), dihexyl phthalate (DHXP), benzyl butyl phthalate (BBP), Bis (2-n-butoxyethyl) phthalate (DBEP), dicyclohexyl phthalate (DCHP), Bis (2-ethylhexyl) phthalate (DEHP), diphenyl phthalate (DPhP), Di-n-octyl phthalate (DNOP), diisononyl phthalate (DINP), dinonyl phthalate (DNP), with purity > 95.0%.
3.3 Preparation of standard solution
3.3.1 Standard stock solutions of 18 phthalate esters (1,000 μg/mL):accurately weigh out 25mg of 18 phthalate esters standard products respectively, dissolve them with normal hexane and accurately make the volume to 25mL, and preserve them in a 4℃ refrigerator in dark condition.
3.3.2 Standard working solutions of 17 phthalate esters (10 μg/mL): accurately pipette 1 mL of all phthalate esters (except diisononyl phthalate) standard stock solutions (1,000μg/mL) respectively to 100mL volumetric flasks, add normal hexane to constant volume 100mL, and preserve them in a 4℃ refrigerator in dark condition.
3.3.3 Diisononyl phthalate standard working solution (100 μg/mL): accurately pipette 10 mL of diisononyl phthalate standard stock solution (1,000μg/mL) to a 100mL volumetric flask, add normal hexane to constant volume 100mL, and preserve them in a 4℃ refrigerator in dark condition.
3.3.4 Series standard working solutions of phthalate esters: accurately pipette an appropriate amount of phthalate esters standard working solution, use normal hexane to prepare standard mixed working solutions of 17 phthalate esters with concentrations 0.02mg/L, 0.05mg/L, 0.10mg/L, 0.20mg/L, 0.50mg/L and 1.00mg/L, as well as monostandard working solutions of diisononyl phthalate (DINP) with concentrations 0.5mg/L, 1.0mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L and 20.0mg/L.
4 Instruments and Apparatus
4.1 Gas chromatograph - mass spectrometer (GC-MS).
4.2 Analytic balance: sensitivity 0.0001g and 0.01g.
4.3 Ultrasonic generator.
4.4 Glassware.
Note: the glassware washed is flushed with aquabidestillata for three times, and soaked in dimethylketone for 1h; then baked at 200℃ for 2h and cooled to the ambient temperature for standby use.
5 Analysis Procedure
5.1 Specimen preparation
Take 5g of typical sample, cut the specimen (excluding preservative film) to fragments with single diameter ≤0.2cm, cut the preservative film to fragments with diameter ≤0.3cm, mix them up; accurately weigh of 0.2g ~ 0.5g specimens (accurate to 0.000,1g) and place them into a triangular flask with stopper; add 20mL normal hexane, perform ultrasonic treatment for 30min; and perform ultrasonic treatment for the residual with 20mL normal hexane; combine the filtrates into a 50 mL volumetric flask, add normal hexane to the scale; perform proper dilution depending on content of phthalate ester in the specimen, and mix it up; filter it with 0.45μm organic phase glass membrane filter, and analyze with gas chromatography-mass spectrometer (GC-MS).
5.2 Blank test
Treat the reagent (used in the test) as specified in 5.1, and perform GC-MS analysis.
5.3 Reference conditions of instrument and apparatus
5.3.1 Reference condition of gas chromatography
a) Chromatographic column: 5% benzyl- methyl polyorganosiloxane quartz capillary column or analytical column with similar performance; specification: column length 30.0m, inner diameter 0.25mm, and membrane thickness 0.25μm;
b) Injection port temperature: 260℃;
c) Temperature programming: set the initial column temperature 60℃, and keep 1 min; raise the temperature at a speed of 20℃/min to 220℃ and keep 1min; raise the temperature at a speed of 5℃/min to 250℃ and keep 1 min; raise the temperature at a speed of 20℃/min to 290℃ and keep 7.5 min;
d) Carrier gas: helium gas (purity ≥ 99.999%), flow rate: 1mL/min;
e) Sample injection mode: splitless mode;
f) Sample injection quantity: 1 μL.
5.3.2 Reference condition of mass spectrogram
a) Color-spectrum and mass-spectrum interfacing temperature: 280℃;
b) Ion source temperature: 230℃;
c) Electro-ionization mode: electron impact ion source (EI);
d) Monitor mode: selected ion monitor mode (SIM); for monitored ions, see Annex B;
e) Ionizing energy: 70eV;
f) Dissolvent delay: 7 min.
5.4 Drawing of standard curve
Respectively inject series standard working solutions gas chromatography-mass spectrometer, test the peak areas of quantitive ions of corresponding phthalate ester compound, and draw the standard curve with concentration of standard working solution as horizontal coordinate and peak area of phthalate ester compound quantitive ion as longitudinal coordinate.
5.5 Determination on specimen solution
Inject the specimen solution into gas chromatography-mass spectrometer, and obtain the peak area of phthalate ester compound quantitive ion respectively; get the concentrations of phthalate ester compounds in the liquids (to be tested) by looking up the standard curve.
1 Scope
2 Principle
3 Reagents and Materials
4 Instruments and Apparatus
5 Analysis Procedure
6 Expression of Analytic Result
7 Precision
8 Others
9 Principle
10 Reagents and Materials
11 Instruments and Apparatus
12 Analysis Procedure
13 Expression of Analytic Result
14 Precision
15 Others
Annex A 18 Common Phthalate Esters Plasticizers
Annex B Quantitive and Qualitative Selective Ions for Phthalate Esters Compounds
Annex C GC-MS TIC of Phthalate Esters Standard Sample Solution
