GB 5009.205-2024 National food safety standard - Determination of toxic equivalent quantity of dioxins and their analogues in foods
National food safety standard - Determination of toxic equivalent quantity of dioxins and their analogues in foods
1 Scope
This standard specifies the determination methods for the content and toxic equivalent quantity (TEQ) of 17 types of 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) (collectively referred to as “PCDD/Fs”) and 12 types of dioxin-like polychlorinated biphenyls (DL-PCBs) in foods (see Table A.1 of Annex A).
“Method I: Isotope dilution - Gas chromatography - Magnetic sector high resolution mass spectrometry” is applicable to the determination of 17 PCDD/Fs and 12 DL-PCBs and their TEQ in foods.
“Method II: Isotope dilution - Gas chromatography - Triple quadrupole mass spectrometry” is applicable to the determination of 17 PCDD/Fs and 12 DL-PCBs and their TEQ in meat and meat products, aquatic animals and their products, milk and dairy products, eggs and egg products and oils.
Method I: Isotope dilution - Gas chromatography - Magnetic sector high resolution mass spectrometry
2 Principle
After extraction, purification and concentration, the specimen is determined by gas chromatography-magnetic sector high resolution mass spectrometer (GC-HRMS) and quantified by stable isotope dilution method. The TEQ of PCDD/Fs and DL-PCBs in the specimen are calculated by multiplying the toxic equivalency factor (TEF) of each target compound with the measured content and accumulating.
3 Reagents and materials
3.1 Reagents
Unless otherwise stated, reagents used in this method are all analytically pure, and water is of Grade 1 as specified in GB/T 6682.
3.1.13 Diatomite for extraction: with bulk density of 18.0 g/100 mL ~ 36.0 g/100 mL (such as EXtrelut NT or equivalent products).
3.1.14 Gel chromatographic packing: polystyrene gel, 38 μm ~ 75 μm (e.g. Bio-Beads S-X3 or equivalent products).
3.1.15 Silica gel: 75 μm ~ 250 μm.
3.1.16 Alkaline aluminium oxide: 63 μm ~ 200 μm (e.g. EcoChromTM MP Alumina B-Super I or equivalent products).
3.1.17 Florisil: 150 μm ~ 250 μm.
3.1.18 Activated carbon: 150 μm to 180 μm (e.g. Carbopack C, Supelco 10258 or equivalent products).
3.1.19 Diatomite for purification: 26 μm (e.g. Celite 545 AW, Supelco 20199-U or equivalent products).
3.2 Reagent preparation
3.2.1 Activated silica gel: Wash the silica gel with methanol and then dichloromethane, and bake at 600°C for at least 12 h after the solvent is evaporated. Freshly prepare before use.
3.2.2 Acidified silica gel (mass fraction: 44%): Weigh 112.0 g of activated silica gel in a 250 mL rotary flask with stopper and grinding mouth, add 88.0 g of concentrated sulfuric acid, seal it and place it on a shaking table to oscillate until the silica gel is in an even flow state. Freshly prepare before use.
3.2.3 Alkalized silica gel (mass fraction: 33%): Weigh 100.0 g of activated silica gel in a 250 mL rotary flask with stopper and grinding mouth, add 49.0 g of 1 mol/L sodium hydroxide solution, seal it and place it on a shaking table to oscillate until the silica gel is in an even flow state. Freshly prepare before use.
3.2.4 Silver nitrate silica gel: Weigh 10.0 g of silver nitrate in a 250 mL rotary flask with stopper and grinding mouth, add 40 mL of water to dissolve it, then slowly add 90.0 g of activated silica gel, seal it and place it on a shaking table to oscillate until the silica gel is in an even flow state. Freshly prepare before use.
3.2.5 Alkaline aluminium oxide: Activate alkaline aluminium oxide at 600°C for 24 h. Freshly prepare before use.
3.2.6 Aqueous florisil (mass fraction: 1%): Take a quantity of florisil into Soxhlet extractor, extract it with n-hexane and dichloromethane (by volume ratio of 1:1) for 24 h; weigh 99.0 g after the solvent dries, add 1.0 mL of water, and mix it evenly in a closed container (such as a glass flask with stopper or a glass triangular flask with stopper). Freshly prepare before use.
3.2.7 Mixed activated carbon: Weigh 9.0 g of activated carbon and 41.0 g of diatomite for purification, mix them evenly in a closed container (such as glass flask with stopper or glass triangle flask with stopper), and then activate them at 130°C for 6 h. Freshly prepare before use.
3.2.8 Anhydrous sodium sulfate: Take anhydrous sodium sulfate and burn it at 660°C for 6 h. Freshly prepare before use.
3.3 Standard solution
3.3.1 Standard solution for resolution test: solution containing natural PCDD/Fs. See Table B.1 of Annex B for the specific compounds and concentrations.
3.3.2 Standard solution for PCDD/Fs isotope labeled quantitative internal standard: solution containing 15 types of 13C12-PCDD/Fs. See Table B.2 for the specific compounds and concentrations.
Foreword i 1 Scope 2 Principle 3 Reagents and materials 4 Instruments and apparatus 5 Analytical procedures 6 Expression of analysis results 7 Precision 8 Detection limit 9 Others 10 Principle 11 Reagents and materials 12 Instruments and apparatus 13 Analytical steps 14 Expression of analysis results 15 Precision 16 Quantitative limit of the method 17 Others Annex A 17 types of 2,3,7,8-substituted PCDD/Fs and 12 types of DL-PCBs with names, CAS numbers, IUPAC numbers, and WHO specified toxic equivalent factors (TEF) Annex B Standard solution Annex C Technical requirements for determination methods Annex D Separation and purification process of automatic sample purification system Annex E Chromatogram of standard solution
Standard
GB 5009.205-2024 National food safety standard-Determination of toxic equivalent of dioxins and their analogues in food (English Version)
Standard No.
GB 5009.205-2024
Status
valid
Language
English
File Format
PDF
Word Count
21000 words
Price(USD)
630.0
Implemented on
2024-8-8
Delivery
via email in 1 business day
Detail of GB 5009.205-2024
Standard No.
GB 5009.205-2024
English Name
National food safety standard-Determination of toxic equivalent of dioxins and their analogues in food
Chinese Name
食品安全国家标准食品 中二噁英及其类似物毒性当量的测定
Chinese Classification
X09
Professional Classification
GB
ICS Classification
Issued by
National Health Commission and State Administration for Market Regulation
GB 5009.205-2024 National food safety standard - Determination of toxic equivalent quantity of dioxins and their analogues in foods
National food safety standard - Determination of toxic equivalent quantity of dioxins and their analogues in foods
1 Scope
This standard specifies the determination methods for the content and toxic equivalent quantity (TEQ) of 17 types of 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) (collectively referred to as “PCDD/Fs”) and 12 types of dioxin-like polychlorinated biphenyls (DL-PCBs) in foods (see Table A.1 of Annex A).
“Method I: Isotope dilution - Gas chromatography - Magnetic sector high resolution mass spectrometry” is applicable to the determination of 17 PCDD/Fs and 12 DL-PCBs and their TEQ in foods.
“Method II: Isotope dilution - Gas chromatography - Triple quadrupole mass spectrometry” is applicable to the determination of 17 PCDD/Fs and 12 DL-PCBs and their TEQ in meat and meat products, aquatic animals and their products, milk and dairy products, eggs and egg products and oils.
Method I: Isotope dilution - Gas chromatography - Magnetic sector high resolution mass spectrometry
2 Principle
After extraction, purification and concentration, the specimen is determined by gas chromatography-magnetic sector high resolution mass spectrometer (GC-HRMS) and quantified by stable isotope dilution method. The TEQ of PCDD/Fs and DL-PCBs in the specimen are calculated by multiplying the toxic equivalency factor (TEF) of each target compound with the measured content and accumulating.
3 Reagents and materials
3.1 Reagents
Unless otherwise stated, reagents used in this method are all analytically pure, and water is of Grade 1 as specified in GB/T 6682.
3.1.1 Acetone (C3H6O): pesticide residue grade.
3.1.2 n-hexane (C6H14): pesticide residue grade.
3.1.3 Toluene (C7H8): pesticide residue grade.
3.1.4 Cyclohexane (C6H12): pesticide residue grade.
3.1.5 Dichloromethane (CH2Cl2): pesticide residue grade.
3.1.6 Methanol (CH3OH): chromatographic grade.
3.1.7 n-nonane (C9H20): ≥99%.
3.1.8 Ethyl acetate (CH3COOCH2CH3): pesticide residue grade.
3.1.9 Anhydrous sodium sulfate (Na2SO4): guaranteed reagent.
3.1.10 Concentrated sulfuric acid (H2SO4): guaranteed reagent.
3.1.11 Sodium hydroxide (NaOH): guaranteed reagent.
3.1.12 Silver nitrate (AgNO3): guaranteed reagent.
3.1.13 Diatomite for extraction: with bulk density of 18.0 g/100 mL ~ 36.0 g/100 mL (such as EXtrelut NT or equivalent products).
3.1.14 Gel chromatographic packing: polystyrene gel, 38 μm ~ 75 μm (e.g. Bio-Beads S-X3 or equivalent products).
3.1.15 Silica gel: 75 μm ~ 250 μm.
3.1.16 Alkaline aluminium oxide: 63 μm ~ 200 μm (e.g. EcoChromTM MP Alumina B-Super I or equivalent products).
3.1.17 Florisil: 150 μm ~ 250 μm.
3.1.18 Activated carbon: 150 μm to 180 μm (e.g. Carbopack C, Supelco 10258 or equivalent products).
3.1.19 Diatomite for purification: 26 μm (e.g. Celite 545 AW, Supelco 20199-U or equivalent products).
3.2 Reagent preparation
3.2.1 Activated silica gel: Wash the silica gel with methanol and then dichloromethane, and bake at 600°C for at least 12 h after the solvent is evaporated. Freshly prepare before use.
3.2.2 Acidified silica gel (mass fraction: 44%): Weigh 112.0 g of activated silica gel in a 250 mL rotary flask with stopper and grinding mouth, add 88.0 g of concentrated sulfuric acid, seal it and place it on a shaking table to oscillate until the silica gel is in an even flow state. Freshly prepare before use.
3.2.3 Alkalized silica gel (mass fraction: 33%): Weigh 100.0 g of activated silica gel in a 250 mL rotary flask with stopper and grinding mouth, add 49.0 g of 1 mol/L sodium hydroxide solution, seal it and place it on a shaking table to oscillate until the silica gel is in an even flow state. Freshly prepare before use.
3.2.4 Silver nitrate silica gel: Weigh 10.0 g of silver nitrate in a 250 mL rotary flask with stopper and grinding mouth, add 40 mL of water to dissolve it, then slowly add 90.0 g of activated silica gel, seal it and place it on a shaking table to oscillate until the silica gel is in an even flow state. Freshly prepare before use.
3.2.5 Alkaline aluminium oxide: Activate alkaline aluminium oxide at 600°C for 24 h. Freshly prepare before use.
3.2.6 Aqueous florisil (mass fraction: 1%): Take a quantity of florisil into Soxhlet extractor, extract it with n-hexane and dichloromethane (by volume ratio of 1:1) for 24 h; weigh 99.0 g after the solvent dries, add 1.0 mL of water, and mix it evenly in a closed container (such as a glass flask with stopper or a glass triangular flask with stopper). Freshly prepare before use.
3.2.7 Mixed activated carbon: Weigh 9.0 g of activated carbon and 41.0 g of diatomite for purification, mix them evenly in a closed container (such as glass flask with stopper or glass triangle flask with stopper), and then activate them at 130°C for 6 h. Freshly prepare before use.
3.2.8 Anhydrous sodium sulfate: Take anhydrous sodium sulfate and burn it at 660°C for 6 h. Freshly prepare before use.
3.3 Standard solution
3.3.1 Standard solution for resolution test: solution containing natural PCDD/Fs. See Table B.1 of Annex B for the specific compounds and concentrations.
3.3.2 Standard solution for PCDD/Fs isotope labeled quantitative internal standard: solution containing 15 types of 13C12-PCDD/Fs. See Table B.2 for the specific compounds and concentrations.
Contents of GB 5009.205-2024
Foreword i
1 Scope
2 Principle
3 Reagents and materials
4 Instruments and apparatus
5 Analytical procedures
6 Expression of analysis results
7 Precision
8 Detection limit
9 Others
10 Principle
11 Reagents and materials
12 Instruments and apparatus
13 Analytical steps
14 Expression of analysis results
15 Precision
16 Quantitative limit of the method
17 Others
Annex A 17 types of 2,3,7,8-substituted PCDD/Fs and 12 types of DL-PCBs with names, CAS numbers, IUPAC numbers, and WHO specified toxic equivalent factors (TEF)
Annex B Standard solution
Annex C Technical requirements for determination methods
Annex D Separation and purification process of automatic sample purification system
Annex E Chromatogram of standard solution
