Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard replaces the Method II in GB 5413.21-2010 National Food Safety Standard Determination of Calcium, Iron, Zinc, Sodium, Potassium, Magnesium, Copper and Manganese in Foods for Infants and Young Children, Milk and Milk Products, GB/T 23545-2009 Determination of Manganese in White Wine-Inductively Coupled Plasma Atomic Emission Spectrometry, GB/T 23374-2009 Determination of Aluminium in Foods - Inductively Coupled Plasma Mass Spectrometry, GB/T 18932.11-2002 Method for the Determination of Potassium, Phosphorus, Iron, Calcium, Zinc, Aluminium, Sodium, Magnesium, Boron, Manganese, Copper, Barium, Titanium, Vanadium, Nickel, Cobalt, Chromium Contents in Honey - Inductively Coupled Plasma Atomic Emission Spectrum, the Method II in SN/T0856—2011 Method for the Determination of Tin in Canned Food for Import and Export, SN/T 2208-2008 Determination of Sodium, Magnesium, Aluminium, Calcium, Chromium, Iron, Nickel, Copper, Zinc, Arsenic, Strontium, Molybdenum, Cadmium, Lead, Mercury, Selenium in Aquatic Products-Microwave Digestion-ICP/MS Method, SN/T 2056-2008 Determination of Lead, Arsenic, Cadmium, Copper, Iron Content in Tea for Import and Export-Inductively Coupled Plasma Atomic Emission Spectrometric Method, SN/T 2049-2008 Determination of Copper, Nickel, Lead, Manganese, Cadmium, Titanium in Food Grade of Phosphoric Acid for Import and Export-Inductively Coupled Plasma Atomic Emission Spectrometric Method, SN/T 2207-2008 Determination of Arsenic, Calcium, Lead Content in Food Additive DL-Tartaric Acid for Import and Export-ICP-AES Method and NY/T 1653-2008 Determination for Mineral Elements in Vegetables, Fruits and Derived Products by ICP-AES Method.
The following main changes have been made with respect to Method II in GB 5413.21-2010:
——the standard name is revised as “食品安全国家标准 食品中多元素的测定 (National Food Safety Standard - Determination of Multi-elements in Foods)”.
——the inductively coupled plasma-mass spectrometry is added as Method I;
——the inductively coupled plasma atomic emission spectrometry is modified as Method II;
——the application scope is modified;
——the contents of specimen preparation are modified;
——the contents of specimen digestion are modified;
——the method detection and quantitation limits are added.
National Food Safety Standard
Determination of Multi-elements in Foods
1 Scope
This standard specifies the inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) for the determination of multi-elements in foods.
Method I is applicable to the determination of boron, sodium, magnesium, aluminum, potassium, calcium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, arsenic, selenium, strontium, molybdenum, cadmium, tin, stibium, barium, mercury, thallium and lead contents in foods; Method II is applicable to the determination of aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc contents in foods.
Method I Inductively Coupled Plasma-mass Spectrometry (ICP-MS)
2 Theory
Use inductively coupled plasma-mass spectrometer to determine the content in the sample after digestion, conduct the quantitative analysis with specific mass number (mass-to-charge ratio, m/z) and conduct quantitative analysis in external standard method with that the strength ratio of mass spectrum signals of to-be-determined elements and internal standard element in direct proportion to the concentration of to-be-determined elements.
3 Reagents and Materials
Unless otherwise specified, guaranteed reagents and Grade 1 water (specified in GB/T 6682) are adopted for the purposes of this method.
3.1 Reagents
3.1.1 Nitric acid (HNO3): guaranteed reagent or higher purity.
3.1.2 Argon (Ar): argon (≥99.995%) or liquid argon.
3.1.3 Helium (He): helium (≥99.995%).
3.1.4 Gold element (Au) solution (1,000 mg/L).
3.2 Preparation of reagents
3.2.1 Nitric acid solution (5+95): take 50mL of nitric, slowly add it into 950mL of water and mix well.
3.2.2 Mercury standard stabilizer: take 2mL of gold element (Au) solution, dilute it to 1,000mL with nitric acid solution (5+95), and use such solution to prepare mercury standard solution.
Note: the mixed solution of 2g/L cysteine hydrochloride + nitric acid (5+95) or other equivalent stabilizer may be adopted as mercury standard stabilizer.
3.3 Standards
3.3.1 Element stock solution (1,000mg/L or 100mg/L): use simple-element or multi-element standard stock solution, with approved and awarded with reference material certificate by the nation, of plumbum, cadmium, arsenic, mercury, selenium, chromium, tin, copper, iron, manganese, zinc, nickel, aluminum, stibium, potassium, sodium, calcium, magnesium, boron, barium, strontium, molybdenum, thallium, titanium, vanadium and cobalt.
3.3.2 Internal standard element stock solution (1,000mg/L): the standard stock solution, approved and awarded with reference material certificate by the nation, of simple or multiple internal standard element(s) such as scandium, germanium, indium, rhodium, rhenium and bismuth.
3.4 Preparation of standard solutions
3.4.1 Mixed standard working solution: pipet proper amount of simple element standard stock solution or multi-element mixed standard stock solution, dilute it with nitric acid solution (5+95) step by step to a series of mixed standard working solution; see Table A.1 for the mass concentration of each element.
Note: properly adjust the mass concentration range of each element in the standard series according to the mass concentration level of element in sample digestion solution.
3.4.2 Mercury standard working solution: take proper amount of mercury stock solution, dilute it with mercury standard stabilizer step by step to a series of standard working solution, and see Table A.1 for the concentration range.
3.4.3 Internal standard working solution: take proper amount of internal standard stock solution of simple element or multiple elements, prepare it with nitric acid solution (5+95) into an internal standard working solution of proper concentration, and see A.2 for the concentration.
Note: the internal standard solution can be added quantitatively by hand during preparation of mixed standard working solution and sample digestion solution, or added online by apparatus.
4 Apparatuses
4.1 Inductively coupled plasma-mass spectrometer (ICP-MS).
4.2 Balance: with a sensibility of 0.1mg and 1mg.
4.3 Microwave digestion instrument: equipped with polytetrafluoroethylene digestion inner tank.
4.4 Pressure digestion tank: equipped with polytetrafluoroethylene digestion inner tank.
4.5 Constant-temperature dry oven.
4.6 Temperature control electric heating board.
4.7 Ultrasonic water bath.
4.8 Sample grinding equipment: refiner and high speed disintegrator.
5 Analytical Procedures
5.1 Specimen preparation
5.1.1 Solid samples
5.1.1.1 Dry samples
As for the samples with low moisture content, such as bean, cereal, fungi, tea, dried fruit and bakery products, take the edible parts and grind them uniformly with high speed disintegrator, if necessary; as for the powder samples in uniform state, such as solid milk products, albumen powder and flour, shake well.
5.1.1.2 Fresh samples
As for the samples with high moisture content, such as vegetable, fruit and aquatic product, clean and dry them in the air, take their edible parts and homogenize uniformly; as for samples such as meat and egg, take their edible parts and homogenize uniformly.
5.1.1.3 Quick-frozen foods and canned foods
As for the samples of unfrozen quick-frozen foods and canned foods, take the edible parts and homogenize uniformly.
5.1.2 Liquid samples
As for samples such as soft drink and flavorings, shake well.
5.1.3 Semi-solid samples
Stir well.
5.2 Specimen digestion
Note: corresponding decomposition method and digestion vessel may be selected according to the content level of to-be-tested element in the specimen and the requirements of test level.
5.2.1 Microwave digestion method
Weigh 0.2g~0.5g (to the nearest 0.001g; as for the sample with more water content, the sampling quantity may be increased properly up to 1g) of solid sample, or accurately transfer 1.00mL~3.00mL of liquid specimen into the microwave digestion inner tank; as for the sample containing ethanol or carbon dioxide, first heat it over low heat on the electric heating board to remove ethanol or carbon dioxide, add 5mL~10mL of nitric acid, cover and leave it standstill for 1h or one night, tighten the tank cover and digest it in accordance with the standard operating procedures of microwave digestion instrument (see Table B.1 for digestion reference conditions). Take out the tank after cooling, slowly uncover it for venting, wash the inner cover with a small quantity of water, put the digestion tank on temperature control electric heating board or in ultrasonic water bath at 100℃ for 30min or ultrasonic degasification for 2min~5min; scale the volume with water to 25mL or 50mL, mix well for future use and carry out blank test simultaneously.
Foreword I
1 Scope
2 Theory
3 Reagents and Materials
4 Apparatuses
5 Analytical Procedures
6 Expression of Analysis Results
7 Precision
8 Others
9 Theory
10 Reagents and Materials
11 Apparatuses
12 Analytical Procedures
13 Expression of Analysis Results
14 Precision
15 Others
Annex A Mass Concentration of Standard Solution Series
Annex B Reference Conditions of Apparatuses
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard replaces the Method II in GB 5413.21-2010 National Food Safety Standard Determination of Calcium, Iron, Zinc, Sodium, Potassium, Magnesium, Copper and Manganese in Foods for Infants and Young Children, Milk and Milk Products, GB/T 23545-2009 Determination of Manganese in White Wine-Inductively Coupled Plasma Atomic Emission Spectrometry, GB/T 23374-2009 Determination of Aluminium in Foods - Inductively Coupled Plasma Mass Spectrometry, GB/T 18932.11-2002 Method for the Determination of Potassium, Phosphorus, Iron, Calcium, Zinc, Aluminium, Sodium, Magnesium, Boron, Manganese, Copper, Barium, Titanium, Vanadium, Nickel, Cobalt, Chromium Contents in Honey - Inductively Coupled Plasma Atomic Emission Spectrum, the Method II in SN/T0856—2011 Method for the Determination of Tin in Canned Food for Import and Export, SN/T 2208-2008 Determination of Sodium, Magnesium, Aluminium, Calcium, Chromium, Iron, Nickel, Copper, Zinc, Arsenic, Strontium, Molybdenum, Cadmium, Lead, Mercury, Selenium in Aquatic Products-Microwave Digestion-ICP/MS Method, SN/T 2056-2008 Determination of Lead, Arsenic, Cadmium, Copper, Iron Content in Tea for Import and Export-Inductively Coupled Plasma Atomic Emission Spectrometric Method, SN/T 2049-2008 Determination of Copper, Nickel, Lead, Manganese, Cadmium, Titanium in Food Grade of Phosphoric Acid for Import and Export-Inductively Coupled Plasma Atomic Emission Spectrometric Method, SN/T 2207-2008 Determination of Arsenic, Calcium, Lead Content in Food Additive DL-Tartaric Acid for Import and Export-ICP-AES Method and NY/T 1653-2008 Determination for Mineral Elements in Vegetables, Fruits and Derived Products by ICP-AES Method.
The following main changes have been made with respect to Method II in GB 5413.21-2010:
——the standard name is revised as “食品安全国家标准 食品中多元素的测定 (National Food Safety Standard - Determination of Multi-elements in Foods)”.
——the inductively coupled plasma-mass spectrometry is added as Method I;
——the inductively coupled plasma atomic emission spectrometry is modified as Method II;
——the application scope is modified;
——the contents of specimen preparation are modified;
——the contents of specimen digestion are modified;
——the method detection and quantitation limits are added.
National Food Safety Standard
Determination of Multi-elements in Foods
1 Scope
This standard specifies the inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) for the determination of multi-elements in foods.
Method I is applicable to the determination of boron, sodium, magnesium, aluminum, potassium, calcium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, arsenic, selenium, strontium, molybdenum, cadmium, tin, stibium, barium, mercury, thallium and lead contents in foods; Method II is applicable to the determination of aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc contents in foods.
Method I Inductively Coupled Plasma-mass Spectrometry (ICP-MS)
2 Theory
Use inductively coupled plasma-mass spectrometer to determine the content in the sample after digestion, conduct the quantitative analysis with specific mass number (mass-to-charge ratio, m/z) and conduct quantitative analysis in external standard method with that the strength ratio of mass spectrum signals of to-be-determined elements and internal standard element in direct proportion to the concentration of to-be-determined elements.
3 Reagents and Materials
Unless otherwise specified, guaranteed reagents and Grade 1 water (specified in GB/T 6682) are adopted for the purposes of this method.
3.1 Reagents
3.1.1 Nitric acid (HNO3): guaranteed reagent or higher purity.
3.1.2 Argon (Ar): argon (≥99.995%) or liquid argon.
3.1.3 Helium (He): helium (≥99.995%).
3.1.4 Gold element (Au) solution (1,000 mg/L).
3.2 Preparation of reagents
3.2.1 Nitric acid solution (5+95): take 50mL of nitric, slowly add it into 950mL of water and mix well.
3.2.2 Mercury standard stabilizer: take 2mL of gold element (Au) solution, dilute it to 1,000mL with nitric acid solution (5+95), and use such solution to prepare mercury standard solution.
Note: the mixed solution of 2g/L cysteine hydrochloride + nitric acid (5+95) or other equivalent stabilizer may be adopted as mercury standard stabilizer.
3.3 Standards
3.3.1 Element stock solution (1,000mg/L or 100mg/L): use simple-element or multi-element standard stock solution, with approved and awarded with reference material certificate by the nation, of plumbum, cadmium, arsenic, mercury, selenium, chromium, tin, copper, iron, manganese, zinc, nickel, aluminum, stibium, potassium, sodium, calcium, magnesium, boron, barium, strontium, molybdenum, thallium, titanium, vanadium and cobalt.
3.3.2 Internal standard element stock solution (1,000mg/L): the standard stock solution, approved and awarded with reference material certificate by the nation, of simple or multiple internal standard element(s) such as scandium, germanium, indium, rhodium, rhenium and bismuth.
3.4 Preparation of standard solutions
3.4.1 Mixed standard working solution: pipet proper amount of simple element standard stock solution or multi-element mixed standard stock solution, dilute it with nitric acid solution (5+95) step by step to a series of mixed standard working solution; see Table A.1 for the mass concentration of each element.
Note: properly adjust the mass concentration range of each element in the standard series according to the mass concentration level of element in sample digestion solution.
3.4.2 Mercury standard working solution: take proper amount of mercury stock solution, dilute it with mercury standard stabilizer step by step to a series of standard working solution, and see Table A.1 for the concentration range.
3.4.3 Internal standard working solution: take proper amount of internal standard stock solution of simple element or multiple elements, prepare it with nitric acid solution (5+95) into an internal standard working solution of proper concentration, and see A.2 for the concentration.
Note: the internal standard solution can be added quantitatively by hand during preparation of mixed standard working solution and sample digestion solution, or added online by apparatus.
4 Apparatuses
4.1 Inductively coupled plasma-mass spectrometer (ICP-MS).
4.2 Balance: with a sensibility of 0.1mg and 1mg.
4.3 Microwave digestion instrument: equipped with polytetrafluoroethylene digestion inner tank.
4.4 Pressure digestion tank: equipped with polytetrafluoroethylene digestion inner tank.
4.5 Constant-temperature dry oven.
4.6 Temperature control electric heating board.
4.7 Ultrasonic water bath.
4.8 Sample grinding equipment: refiner and high speed disintegrator.
5 Analytical Procedures
5.1 Specimen preparation
5.1.1 Solid samples
5.1.1.1 Dry samples
As for the samples with low moisture content, such as bean, cereal, fungi, tea, dried fruit and bakery products, take the edible parts and grind them uniformly with high speed disintegrator, if necessary; as for the powder samples in uniform state, such as solid milk products, albumen powder and flour, shake well.
5.1.1.2 Fresh samples
As for the samples with high moisture content, such as vegetable, fruit and aquatic product, clean and dry them in the air, take their edible parts and homogenize uniformly; as for samples such as meat and egg, take their edible parts and homogenize uniformly.
5.1.1.3 Quick-frozen foods and canned foods
As for the samples of unfrozen quick-frozen foods and canned foods, take the edible parts and homogenize uniformly.
5.1.2 Liquid samples
As for samples such as soft drink and flavorings, shake well.
5.1.3 Semi-solid samples
Stir well.
5.2 Specimen digestion
Note: corresponding decomposition method and digestion vessel may be selected according to the content level of to-be-tested element in the specimen and the requirements of test level.
5.2.1 Microwave digestion method
Weigh 0.2g~0.5g (to the nearest 0.001g; as for the sample with more water content, the sampling quantity may be increased properly up to 1g) of solid sample, or accurately transfer 1.00mL~3.00mL of liquid specimen into the microwave digestion inner tank; as for the sample containing ethanol or carbon dioxide, first heat it over low heat on the electric heating board to remove ethanol or carbon dioxide, add 5mL~10mL of nitric acid, cover and leave it standstill for 1h or one night, tighten the tank cover and digest it in accordance with the standard operating procedures of microwave digestion instrument (see Table B.1 for digestion reference conditions). Take out the tank after cooling, slowly uncover it for venting, wash the inner cover with a small quantity of water, put the digestion tank on temperature control electric heating board or in ultrasonic water bath at 100℃ for 30min or ultrasonic degasification for 2min~5min; scale the volume with water to 25mL or 50mL, mix well for future use and carry out blank test simultaneously.
Contents of GB 5009.268-2016
Foreword I
1 Scope
2 Theory
3 Reagents and Materials
4 Apparatuses
5 Analytical Procedures
6 Expression of Analysis Results
7 Precision
8 Others
9 Theory
10 Reagents and Materials
11 Apparatuses
12 Analytical Procedures
13 Expression of Analysis Results
14 Precision
15 Others
Annex A Mass Concentration of Standard Solution Series
Annex B Reference Conditions of Apparatuses