GB 5009.11-2024National food safety standard - Determination of total arsenic and inorganic arsenic in food (English PDF)
食品安全国家标准 食品中总砷及无机砷的测定
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Issued by
NHC; SAMR
Level / Type
National · Mandatory
Issue date
February 8, 2024
Implementation date
August 8, 2024
Scope
GB 5009.11-2024 is the English-translated version of 食品安全国家标准 食品中总砷及无机砷的测定.
Part 1 of this standard specifies the methods for the determination of total arsenic in food; Methods 1 and 2 apply to all food, and Method 3 applies to total arsenic in food except milk powder and prepared milk powder, oils and fats and their products, condiments, and special dietary foods. Part 2 specifies the methods for the determination of inorganic arsenic in food, applicable to cereals and their products, aquatic animals and their products, edible fungi and their products, oils and fats and their products, condiments, supplementary foods for infants and young children, and similar foods.
Document preview — GB 5009.11-2024
National Standard of the People's Republic of China
Issued by: National Health Commission of the People’s Republic of China; State Administration for Market Regulation.
Contents
- Foreword4
- 1 Scope5
- 2 Principle5
- 3 Reagents and materials6
- 3 Reagents6
- 4 Instruments and equipment8
- 5 Analysis procedure8
- 6 Expression of analysis results11
- 7 Precision11
- 8 Others12
- 9 Principle12
- 10 Reagents and materials12
- 11 Instruments and equipment13
- 12 Analysis procedure14
- 13 Expression of analysis results15
- 14 Precision15
- 15 Others16
- 16 Principle16
- 17 Reagents and materials16
- 18 Instruments and equipment19
- 19 Analysis procedure20
- 20 Expression of analysis results25
- 21 Precision25
- 22 Others26
- 23 Principle26
- 24 Reagents and materials
- 25 Instruments and equipment
- 26 Analysis procedure
- 27 Expression of analysis results
- 28 Precision
- 29 Others
- Annex A Reference conditions for microwave digestion
- Annex B Reference conditions for instruments
- Annex C Reference conditions for instruments
- Annex D Chromatograms of LC-AFS method
- Annex E Chromatograms of LC-ICP/MS method
Foreword
This Standard replaces GB 5009.11-2014 “National food safety standard - Determination of total arsenic and inorganic arsenic in food”.
Compared with GB 5009.11-2014, the main changes in this Standard are as follows:
- ADD the graphite furnace atomic absorption spectrometry as Method 3;
- DELETE the silver salt method for the determination of total arsenic in food;
and MODIFY the sample digestion method;
- MODIFY the inductively coupled plasma mass spectrometry method as Method 2.
- ADD the microwave-assisted extraction method for extracting inorganic arsenic from rice samples in Method 1 and Method 2;
and expression of analysis results of Method 1 and Method 2;
determination conditions for the samples in Method 1 and Method 2.
1 Scope
Part 1 of this Standard specifies the methods for the determination of total arsenic in food.
Methods I and II of Part 1 of this Standard apply to the determination of total arsenic in food. Method 3 applies to the determination of total arsenic in food (except milk powder and prepared milk powder, oils and fats and their products, condiments, and special dietary foods).
Part 2 of this Standard specifies the methods for the determination of inorganic arsenic in food.
Part 2 of this Standard applies to the determination of inorganic arsenic in cereals and their products, aquatic animals and their products, edible fungi and their products, oils and fats and their products, condiments, supplementary foods for infants and young children, algae and their products.
2 Principle
After the sample is digested, thiourea is added to pre-reduce the pentavalent arsenic to trivalent arsenic, and then sodium borohydride or potassium borohydride is added to reduce the trivalent arsenic to generate arsine, which is loaded into the quartz atomizer by argon gas and decomposed into atomic arsenic. The atomic arsenic produces atomic fluorescence under the excitation of the emitted light of the arsenic hollow cathode lamp. Under fixed conditions, its fluorescence intensity is proportional to the arsenic concentration in the solution being tested. It is quantitatively determined by external standard method.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are analytical reagents, and the water is Grade 1 water specified in GB/T 6682.
3 Reagents
3.1.1 Sodium hydroxide (NaOH).
3.1.2 Potassium hydroxide (KOH).
3.1.3 Potassium borohydride (KBH4): analytical reagent.
3.1.4 Thiourea (CH4N2S): analytical reagent.
3.1.5 Hydrochloric acid (HCl).
3.1.7 Sulfuric acid (H2SO4).
3.1.8 Perchloric acid (HClO4).
3.1.10 Magnesium nitrate [Mg(NO3)2 · 6H2O]: analytical reagent.
3.1.11 Magnesium oxide (MgO): analytical reagent.
3.1.12 Ascorbic acid (C6H8O6): analytical reagent.
3.3 Reference material
3.4 Preparation of standard solutions
3.4.1 Arsenic standard stock solution (100 mg/L, calculated as As): Accurately weigh 0.0132 g of arsenic trioxide that has been dried at 100 °C for 2 h, add 1 mL of sodium hydroxide solution (100 g/L) and a small amount of water to dissolve, transfer to a 100 mL volumetric flask, add an appropriate amount of hydrochloric acid to adjust its acidity to near neutral, and dilute to the mark with water. Store in a refrigerator at 2 ℃ ~ 8 ℃ away from light, the validity period is 1 year. Or arsenic standard solution certified by the country and awarded a reference material certificate. 3.4.2 Arsenic standard use solution (1.00 mg/L, calculated as As): Accurately pipette 1. […]
4 Instruments and equipment
4.1 Atomic fluorescence spectrometer.
4.2 Electronic balance: the minimum division is 0.01 mg, 0.1 mg and 1 mg.
4.3 Homogenizer.
4.4 High-speed crusher.
4.5 Electrothermal digestion device: temperature-controlled electric heating plate or graphite digestion instrument, the maximum temperature is not less than 350 ℃, and the temperature control accuracy is ±5 ℃.
4.6 Muffle furnace.
4.8 Microwave digestion system: it is equipped with polytetrafluoroethylene digestion inner tank.
5 Analysis procedure
5.1 Preparation of samples
5.1.1 Solid samples
5.1.1.1 Dry samples
For samples such as cereals, dried edible fungi, and dried aquatic animal products, it shall take the edible parts and crush evenly; for powder samples such as solid dairy products, flour, cereal supplementary foods for infants and young children that are in a uniform shape, it shall shake well.
5.1.1.3 Quick-frozen and canned food
For thawed quick-frozen food, it shall take the edible parts and crush evenly; for canned food, it shall crush or homogenize evenly.
5.1.3 Semi-solid samples
5.2 Digestion of samples
5.2.1 Wet digestion
Weigh 0.5 g ~ 2.5 g (accurate to 0.001 g) of solid samples or 5.0 g ~ 10.0 g (accurate to 0.001 g) of liquid samples into a digestion bottle or digestion tube, add 20 mL of nitric acid, 4 mL of perchloric acid and 1.25 mL of sulfuric acid and leave overnight. The next day, heat and digest at 120 ℃ ~ 200 ℃ step by step. […]
6 Expression of analysis results
The arsenic content in the sample is calculated according to formula (1).
When the arsenic content is ≥ 1.00 mg/kg, the calculation results shall retain 3 significant figures; when the arsenic content is < 1.00 mg/kg, the calculation results shall retain 2 significant figures.
7 Precision
When the arsenic content in the sample is greater than 1.00 mg/kg, the absolute difference between the two independent determination results obtained under repeatability conditions shall not exceed 10 % of the arithmetic mean; when it is less than or equal to 1.00 mg/kg and greater than 0.10 mg/kg, the absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 15 % of the arithmetic mean; when it is less than or equal to 0.10 mg/kg, the absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 20 % of the arithmetic mean.
8 Others
When the weighing mass of a solid sample is 1.0 g and the constant volume is 25 mL, the method detection limit is 0.01 mg/kg and the method quantitation limit is 0.04 mg/kg. When the sampling volume of a liquid sample is 2 g and the constant volume is 25 mL, the method detection limit is 0.005 mg/kg and the method quantitation limit is 0.02 mg/kg.
9 Principle
After digestion treatment, the sample is atomized in a graphite furnace and the absorbance is measured at 193.7 nm. Within a certain concentration range, the absorbance value of arsenic is proportional to the arsenic content. It is quantitatively determined by external standard method.
10 Reagents and materials
Unless otherwise stated, the reagents used in this method are guarantee reagents, and the water is Grade 1 water specified in GB/T 6682.
10.1 Reagents
10.1.2 Hydrogen peroxide (H2O2): 30 %.
10.1.3 Palladium nitrate [Pd(NO3)2].
10.1.4 Sodium hydroxide (NaOH).
10.3 Reference material
10.4 Preparation of standard solutions
10.4.1 Arsenic standard stock solution (100 mg/L, calculated as As): Same as 3.4.1. 10.4.3 Arsenic standard series solutions: Take an appropriate amount of arsenic standard use solution (1. […]
11 Instruments and equipment
11.1 Atomic absorption spectrometer: it is equipped with a graphite furnace atomizer.
11.2 Electronic balance: the minimum division is 0.01 mg, 0.1 mg and 1 mg.
11.3 Temperature control electric heating plate: the temperature control accuracy is ±5 ℃.
11.4 Microwave digestion system.
11.7 Homogenizer.
11.8 High-speed crusher.
NOTE: Glassware and polytetrafluoroethylene digestion inner tanks need to be soaked in (1 + 4) nitric acid solution for 24 h, rinsed repeatedly with tap water, and finally rinsed with water.
12 Analysis procedure
12.2 Digestion of samples
12.2.1 Microwave digestion method
Weigh 0.2 g ~ 0.8 g (accurate to 0.001 g) of solid samples and samples of oils and fats and their products, or weigh 1.0 g ~ 3.0 g (accurate to 0.001 g) of samples containing more water or liquid samples into a digestion tank; add 5 mL ~ 8 mL of nitric acid and leave it for more than 30 min. For samples that are difficult to digest such as meat and aquatic animals and their products, add 0.5 mL ~ 1 mL of hydrogen peroxide, cover the safety valve, and put the digestion tank into the microwave digestion system. According to different types of samples, set up appropriate microwave digestion procedures (see Table A.2) and perform digestion according to relevant steps. After digestion is completed, reduce acid to 0. […]
13 Expression of analysis results
The arsenic content in the sample is calculated according to formula (2).
When the arsenic content is ≥ 1.00 mg/kg, the calculation results shall retain 3 significant figures; when the arsenic content is < 1.00 mg/kg, the calculation results shall retain 2 significant figures.
14 Precision
15 Others
When the weighing mass of a solid sample is 0.5 g and the constant volume is 25 mL, the method detection limit is 0.03 mg/kg and the method quantification limit is 0.09 mg/kg. When the sampling mass of a liquid sample is 2 g and the constant volume is 25 mL, the method detection limit is 0.008 mg/kg and the method quantitation limit is 0.03 mg/kg.
16 Principle
After the inorganic arsenic in the sample is extracted with dilute nitric acid, it is separated by liquid chromatography. The separated target compound reacts with potassium borohydride or sodium borohydride in an acidic environment to generate gaseous arsenic compounds, which are determined with an atomic fluorescence spectrometer. It is qualitatively determined by retention time and mass-to-charge ratio, and quantitatively determined by external standard method.
17 Reagents and materials
Unless otherwise stated, the reagents used in this method are guarantee reagents, and the water is Grade 1 water specified in GB/T6682.
17.1 Reagents
17.1.1 Ammonium dihydrogen phosphate (NH4H2PO4): analytical reagent.
17.1.2 Diammonium hydrogen phosphate [(NH4)2HPO4]: analytical reagent.
17.1.3 Ammonium nitrate (NH4NO3): analytical reagent.
17.1.4 Dipotassium hydrogen phosphate (K2HPO4 · 3H2O): analytical reagent.
17.1.5 Potassium borohydride (KBH4): analytical reagent.
17.1.6 Potassium hydroxide (KOH).
17.1.9 Hydrochloric acid (HCl).
17.1.10 Ammonia (NH3 · H2O).
17.1.11 n-hexane [CH3(CH2)4CH3]: chromatographically pure.
17.3 Reference materials
17.3.2 Potassium dihydrogen arsenate (KH2AsO4, CAS number: 7784-41-0) reference material: purity ≥ 99.5 %.
17.4 Preparation of standard solutions
17.4.1 Arsenite [As(Ⅲ)] standard stock solution (100 mg/L, calculated as As): Accurately weigh 0.0132 g of arsenic trioxide that has been dried at 100 °C for 2 h, add 1 mL of 100 g/L potassium hydroxide solution and a small amount of water to dissolve, transfer to a 100 mL volumetric flask, add an appropriate amount of hydrochloric acid to adjust its acidity to near neutral, and add water to dilute to the mark. Store in a refrigerator at 2 ℃ ~ 8 ℃ away from light, the validity period is 1 year. […]
18 Instruments and equipment
18.1 Liquid chromatography-atomic fluorescence spectrometer (LC-AFS): it consists
of a liquid chromatograph and an atomic fluorescence spectrometer.
18.2 Tissue homogenizer.
18.5 Centrifuge: speed ≥ 8000 r/min.
18.6 pH meter: the accuracy is 0.01.
18.7 Electronic balance: the minimum division is 0.01 mg, 0.1 mg and 1 mg.
18.9 Ultrasonic cleaner.
18.10 Filter membrane: 0.45 μm.
NOTE: Glassware and microwave extraction inner tanks need to be soaked in (1 + 4) nitric acid solution for 24 h, rinsed repeatedly with tap water, and finally rinsed with water.
19 Analysis procedure
19.1 Preparation of samples
19.1.1 Solid samples
19.1.1.2 Fresh samples
For samples such as fresh edible fungi, aquatic animals, it shall wash and dry, and take the edible parts and homogenize until homogeneous.
19.1.1.3 Quick-frozen and canned food
For thawed quick-frozen food, it shall take the edible parts and crush evenly; for canned food, it shall crush or homogenize evenly.
19.1.3 Semi-solid samples
19.2 Extraction of samples
19.2.1 Cereals and their products
19.2.1.1 Hot extraction method
Weigh about 0.5 g ~ 1.0 g of the sample (accurate to 0.001 g) into a 50 mL polypropylene centrifuge tube, and add 20 mL of 0.15 mol/L nitric acid solution. Make hot extraction in a thermostat at 90 ℃ for 2.5 h, and shake for 1 min every 0. […]
19.2.1.2 Microwave-assisted extraction method
Weigh about 0.5 g ~ 0.8 g of the sample (accurate to 0.001 g) into a microwave extraction tank, add 15 mL of 0. […]
19.2.2 Aquatic animals and their products
Weigh about 0.5 g ~ 1.0 g of the sample (accurate to 0.001 g) into a 50 mL polypropylene centrifuge tube, and add 20 mL of 0. […]
19.3 Reference conditions for instruments
20 Expression of analysis results
The content of As(Ⅲ) or As(Ⅴ) in the sample is calculated according to formula (3).
The inorganic arsenic content is equal to the sum of As(Ⅲ) content and As(Ⅴ) content.
When the inorganic arsenic content is ≥ 1.00 mg/kg, the calculation results shall retain 3 significant figures; when the inorganic arsenic content is < 1.00 mg/kg, the calculation results shall retain 2 significant figures.
21 Precision
When the inorganic arsenic content in the sample is greater than 1.00 mg/kg, the absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 10 % of the arithmetic mean; when it is less than or equal to 1.00 mg/kg and greater than 0.10 mg/kg, the absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 15 % of the arithmetic mean; when it is less than or equal to 0.10 mg/kg, the absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 20 % of the arithmetic mean.
22 Others
When the sample mass is 1.0 g and the volume of added extraction reagent is 20 mL, the method detection limit is 0.02 mg/kg and the method quantitation limit is 0.05 mg/kg.
23 Principle
After the inorganic arsenic in the sample is extracted with dilute nitric acid, etc., it is separated by liquid chromatography. The separated target compound is atomized and sent into the inductively coupled plasma-torch flame by the carrier gas, undergoes processes such as evaporation, dissociation and atomization, enters the mass spectrometer through the ion collection system, and the mass spectrometer performs separation and determination based on the mass-to-charge ratio. It is qualitatively determined by retention time and mass-to-charge ratio, and quantitatively determined by external standard method.
24 Reagents and materials
Unless otherwise stated, the reagents used in this method are guarantee reagents, and the water is Grade 1 water specified in GB/T 6682.
24.1 Reagents
24.1.1 Diammonium hydrogen phosphate [(NH4)2HPO4]: analytical reagent.
24.1.2 Nitric acid (HNO3).
24.1.3 Hydrogen peroxide (H2O2): 30 %.
24.1.4 n-hexane [CH3(CH2)4CH3]: chromatographically pure.
24.1.5 Methanol (CH3OH): chromatographically pure.
24.1.7 Potassium hydroxide (KOH).
24.1.9 Ammonium carbonate [(NH4)2CO3]: analytical reagent.
24.1.10 Dipotassium hydrogen phosphate (K2HPO4 · 3H2O): analytical reagent.
24.1.11 Ammonium nitrate (NH4NO3): analytical reagent.
24.2 Preparation of reagents
24.2.1 Nitric acid solution (0.15 mol/L): Measure 10 mL of nitric acid, add water to dilute to 1000 mL, and mix well. 24.2.2 Nitric acid + hydrogen peroxide solution (0.15 mol/L nitric acid + 0.45 % hydrogen peroxide): Measure 10 mL of nitric acid and 15 mL of 30 % hydrogen peroxide, add water to dilute to 1000 mL, and mix well. Freshly prepare each time before use. 24.2.3 Mobile phase A (10 mmol/L diammonium hydrogen phosphate + 1 % methanol, pH = 8.4): Accurately weigh 1.320 g of diammonium hydrogen phosphate, place in a 1000 mL volumetric flask, dissolve with water, add 10 mL of methanol, dilute with water to the mark, adjust pH to 8. […]
25 Instruments and equipment
25.1 Liquid chromatography-inductively coupled plasma mass spectrometry (LC-
ICP/MS): it consists of a liquid chromatograph and an inductively coupled plasma mass spectrometer.
25.2 Tissue homogenizer.
25.3 High-speed crusher.
25.4 Centrifuge: speed ≥ 8000 r/min.
25.9 Ultrasonic cleaner.
25.10 Filter membrane: 0.45 μm.
NOTE: Glassware and microwave extraction tanks need to be soaked in (1 + 4) nitric acid solution for 24 h, rinsed repeatedly with tap water, and finally rinsed with water.
26 Analysis procedure
26.2 Extraction of samples
26.2.1 Cereals and their products
26.2.1.1 Hot extraction method
26.2.1.2 Microwave-assisted extraction method
26.2.3 Supplementary foods for infants and young children
Remaining clauses in the full document
- 26.3 Reference conditions for instruments
- 26.4 Plotting of standard curve
- 26.5 Determination of sample solution
- 27 Expression of analysis results
- 28 Precision
- 29 Others
- Annex A Reference conditions for microwave digestion
- Annex B Reference conditions for instruments
- Annex C Reference conditions for instruments
- Annex D Chromatograms of LC-AFS method
- Annex E Chromatograms of LC-ICP/MS method
......
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