GB 5009.268-2025 PDF English
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National food safety standard - Determination of multi-elements in foods
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GB 5009.268-2025: National food safety standard - Determination of multi-elements in foods---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GB5009.268-2025
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard – Determination of Multi-
Elements in Foods
Issued on: MARCH 16, 2025
Implemented on: SEPTEMBER 16, 2025
Issued by. National Health Commission of the People’s Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword... 3
1 Scope... 4
2 Principle... 4
3 Reagents and Materials... 5
4 Instruments and Equipment... 6
5 Analysis Steps... 7
6 Expression of Analysis Results... 9
7 Precision... 10
8 Others... 10
9 Principle... 12
1 Scope
The Part I of this Standard specifies the inductively coupled plasma mass spectrometry and
inductively coupled plasma emission spectrometry methods for the determination of multiple
elements in foods; and the Part II specifies the inductively coupled plasma emission
spectrometry method for the determination of multiple elements in nutritional fortifiers of
compound foods.
The Method I of the Part I is applicable to the determination of lithium, boron, sodium,
magnesium, aluminum, phosphorus, sulfur, potassium, calcium, titanium, vanadium, chromium,
manganese, iron, cobalt, nickel, copper, zinc, arsenic, selenium, rubidium, strontium,
molybdenum, cadmium, tin, antimony, barium, mercury, thallium and lead in foods; and the
Method II of the Part I is applicable to the determination of aluminum, arsenic, boron, barium,
calcium, cadmium, cobalt, chromium, copper, iron, potassium, magnesium, manganese,
molybdenum, sodium, nickel, phosphorus, lead, sulfur, selenium, tin, strontium, titanium,
vanadium and zinc in foods.
The Part II is applicable to the determination of calcium, copper, iron, potassium, magnesium,
manganese, sodium, phosphorus and zinc in nutritional fortifiers of compound foods with
minerals as raw materials, with or without auxiliary materials.
Part I Determination of Multi-Elements in Foods
Method I Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
2 Principle
After digestion, the specimen is measured by inductively coupled plasma mass spectrometry.
The qualitative analysis is based on the specific mass number (mass-to-charge ratio, m/z) of the
element; and the quantitative analysis is based on the intensity ratio of the mass spectrum signal
of the element to be measured and the mass spectrum signal of the internal standard element,
which is proportional to the concentration of the element to be measured.
3 Reagents and Materials
Unless otherwise specified, all reagents used in this Method are of guaranteed reagents; and
water is Grade-1 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3).
3.1.2 Nitric acid with high purity (HNO3). The content of the target element in the reagent is
less than 1 μg/L. For trace detection, nitric acid with high purity should be used.
3.1.3 Argon (Ar). Argon (≥99.995%) or liquid argon.
3.1.4 Helium (He). Helium (≥99.995%).
3.1.5 L-cysteine hydrochloride monohydrate (C3H10ClNO3S, CAS No.. 7048-04-6). ≥98%,
chromatographically pure.
3.1.6 Gold (Au) element solution. The mass concentration is 1,000 mg/L.
3.1.7 Isopropanol (C3H8O, CAS No.. 67-63-0). Chromatographically pure.
3.1.8 Hydrochloric acid (HCl).
3.2 Preparation of reagents
Take 50 mL of nitric acid, slowly add it into 950 mL of water and mix well.
3.2.2 Mercury standard dilution solution
3.3 Standard solution
3.3.1 Single element standard stock solution (1,000 mg/L or 100 mg/L). lithium, boron, sodium,
magnesium, aluminum, phosphorus, sulfur, potassium, calcium, titanium, vanadium, chromium,
manganese, iron, cobalt, nickel, copper, zinc, arsenic, selenium, rubidium, strontium,
molybdenum, cadmium, tin, antimony, barium, thallium, lead. Use single element standard
stock solution certified by the state and awarded with standard substance/standard sample
certificate. Multi-element mixed standard stock solution can also be used.
3.3.2 Mercury standard stock solution (1,000 mg/L or 100 mg/L). Use single element standard
stock solution certified by the state and awarded with standard substance/standard sample
certificate. Standard series needs to be prepared separately.
3.3.3 Single element standard internal standard stock solution (1,000 mg/L). Single element
standard stock solutions such as scandium, germanium, rhodium, indium, rhenium, bismuth,
etc.; and multi-element mixed standard internal standard stock solutions can also be used.
NOTE. When using single element standards to prepare mixed standard solutions and internal standard
solutions, it is necessary to pay attention to the impurity content of the target element in the single element
standard.
3.4 Preparation of standard solutions
3.4.1 Mixed standard solution. Take an appropriate amount of single element standard stock
solution or multi-element mixed standard stock solution; dilute it step by step with nitric acid
solution (5+95) to prepare a mixed standard solution series. For the preparation method and
mass concentration of each element, see Tables A.1 and A.2.
3.4.2 Mercury standard solution. Take an appropriate amount of mercury standard stock
solution; dilute it step by step with mercury standard diluent (A or B) to prepare a standard
solution series. The mass concentration is shown in Table A.3.
3.4.3 Internal standard solution. Take an appropriate amount of single-element internal standard
stock solution or multi-element mixed standard internal standard stock solution; and use nitric
acid solution (5+95) to prepare an internal standard solution of appropriate concentration. The
concentration of the internal standard solution is shown in A.2.
NOTE. Isopropanol can be appropriately added to the internal standard solution to reduce the
sensitization effect of elements such as arsenic and selenium caused by incomplete sample digestion (see
Table A.4 for preparation method).
4 Instruments and Equipment
4.1 Inductively coupled plasma mass spectrometer (ICP-MS).
4.2 Balance. With sensitivity of 0.001 g.
4.3 Microwave digester.
4.4 Pressure digester.
4.5 Constant temperature drying oven.
4.6 Temperature-controlled electric heating plate or adjustable electric furnace.
4.7 Ultrasonic water bath.
4.8 Sample crushing equipment. homogenizer, high-speed crusher, etc.
5 Analysis Steps
5.1 Preparation of specimen
NOTE. If there are requirements for preparation of specimen, refer to the relevant methods.
5.1.1 Solid samples
5.1.2 Liquid samples
For specimens such as beverages and condiments, shake them evenly.
5.1.3 Semi-solid samples
Stir or homogenize evenly.
5.2 Sample digestion
5.2.1 Microwave digestion method
Weigh 0.2 g~1.0 g of specimen (accurate to 0.001 g, the specimen with high water content can
be appropriately increased to 3.0 g), or accurately pipette 0.50 mL~3.00 mL of specimen into
the microwave digestion inner tank. For specimens containing ethanol or carbon dioxide, first
heat them on a hot plate at low temperature to remove the ethanol or carbon dioxide; add 3 mL
~ 5 mL of nitric acid (if the volume of the liquid in the digestion inner tank does not meet the
instrument requirements, it can be supplemented with water); cover it and leave it for 1 h or
overnight. Tighten the tank cover (for specimens with high tin content, add 1 mL of
hydrochloric acid before covering it); and digest according to the standard operating procedures
of the microwave digestion instrument (see Table B.1 for digestion reference conditions). After
cooling, take it out; slowly open the can lid to vent; rinse the inner lid with a small amount of
water. Place the digestion can on a temperature-controlled hot plate or in an ultrasonic water
bath, heat at 100°C for 30 min or ultrasonically degas for 2 min~5 min; make constant volume
to 25 mL or 50 mL with water; mix well and set aside. Perform a blank test at the same time.
NOTE. To avoid element loss caused by excessive pressure during digestion, it should use a high-
pressure microwave digestion container.
5.2.2 Pressure tank digestion method
Weigh 0.2 g ~ 2.0 g of specimen (accurate to 0.001 g, the specimen with high water content can
be appropriately increased to 5.0 g), or accurately pipette 0.50 mL ~ 5.00 mL of specimen into
the digestion inner tank. For specimens containing ethanol or carbon dioxide, first heat them
on a hot plate at low temperature to remove the ethanol or carbon dioxide. Add 3 mL ~ 5 mL
of nitric acid; leave them for 1 h or overnight; tighten the stainless-steel jacket (for specimens
with high tin content, add 1 mL of hydrochloric acid before covering it); place them in a
constant temperature drying oven for digestion (see Table B.1 for digestion reference
conditions); digest at 160 ℃ ~170 ℃ for 4 h. After cooling, slowly loosen the stainless-steel
jacket; take out the digestion inner tank; heat them on a temperature-controlled hot plate or in
an ultrasonic water bath at 100 ℃ for 30 min or ultrasonically degas for 2 min ~5 min. Use
water to make constant volume to 25 mL or 50 mL; mix well and set aside. Perform a blank
test at the same time.
5.3 Instrument reference conditions
5.3.1 Instrument operating conditions. See Table B.2 for instrument operating conditions; See
Table B.3 for element analysis modes.
NOTE. For instruments without a suitable interference elimination mode, interference correction
equations are required to correct the measurement results. See Table B.4 for interference correction
equations for vanadium, arsenic, selenium, molybdenum, cadmium, lead and other elements.
5.3.2 Determination reference conditions. After tuning the instrument to meet the measurement
requirements, edit the measurement method and select the corresponding internal standard
element according to the properties of the element to be measured. See Table B.5 for the m/z of
the element to be measured and the internal standard element.
5.4 Drawing of standard curve
Introduce the mixed standard solution and mercury standard solution into the inductively
coupled plasma mass spectrometer; determine the signal response values of the element to be
measured and the internal standard element; and draw a standard curve with the concentration
of the element to be measured as the horizontal axis and the ratio of the signal response value
of the element to be measured to the selected internal standard element as the vertical axis.
5.5 Determination of specimen solution
Introduce the blank and specimen solutions into the inductively coupled plasma mass
spectrometer respectively; determine the signal response values of the element to be measured
and the internal standard element; and obtain the concentration of the element to be measured
in the digestion solution according to the standard curve.
NOTE. In order to reduce the memory effect of the injection system, it is recommended to use mercury
standard diluent and nitric acid solution (5+95) to clean the injection system in turn when measuring the
standard solution and sample solution.
6 Expression of Analysis Results
7 Precision
When the content of each element in the specimen is greater than 1.0 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 1.0
mg/kg and greater than 0.1 mg/kg, the absolute difference between the two independent
determination results obtained under repeatability conditions shall not exceed 15% of the
arithmetic mean. When it is less than or equal to 0.1 mg/kg, the absolute difference between the
two independent determination results obtained under repeatability conditions shall not exceed
20% of the arithmetic mean.
8 Others
The specimen is calculated by making constant volume to 50mL by 0.5 g (mL) or 2.0 g (mL).
The method detection limit and method quantification limit of each element are shown in Table
1.
10.3 Standard solution
10.3.1 Single element standard stock solution (1,000 mg/L or 10,000 mg/L). aluminum, arsenic,
boron, barium, calcium, cadmium, cobalt, chromium, copper, iron, potassium, magnesium,
manganese, molybdenum, sodium, nickel, phosphorus, lead, sulfur, selenium, tin, strontium,
titanium, vanadium, zinc. Use single element standard stock solution certified by the state and
awarded with standard substance/standard sample certificate, or multi-element mixed standard
stock solution.
10.3.2 Preparation of standard solutions. Accurately pipette an appropriate amount of single-
element standard stock solution or multi-element mixed standard stock solution; and dilute it
step by step with nitric acid solution (5 +95) to prepare a series of mixed standard solutions.
The mass concentration of each element is shown in Table A.5.
11 Instruments and Equipment
11.1 Inductively coupled plasma optical emission spectrometer (ICP-OES).
11.2 Balance. With sensitivity of 0.01 g or 0.001 g.
11.3 Microwave digestion instrument.
11.4 Pressure digester.
11.5 Constant temperature drying oven.
11.6 Temperature-controlled hot plate or adjustable electric furnace.
11.7 Muffle furnace.
11.8 Specimen crushing equipment. homogenizer, high-speed crusher, etc.
11.9 Graphite digestion device.
12 Analysis Steps
12.1 Preparation of specimen
The same as 5.1.
12.2 Digestion of specimen
12.2.1 Microwave digestion method
The same as 5.2.1.
12.2.2 Pressure tank digestion method
The same as 5.2.2.
12.2.3 Wet digestion method
Weigh 0.5 g ~ 5.0 g (accurate to 0.001 g, the specimen with high water content can be
appropriately increased to 10.0 g) of specimen, or accurately pipette 2.00 mL~10.0 mL of the
specimen into a glass or polytetrafluoroethylene digestion vessel. For specimens containing
ethanol or carbon dioxide, first heat them on a hot plate at low temperature to remove the
ethanol or carbon dioxide; add 10 mL of nitric acid + perchloric acid (10+1) mixed solution;
and digest on a hot plate or graphite digestion device. If the digestion solution turns brown-
black during the digestion process, a small amount of mixed acid shall be appropriately added
until white smoke is emitted and the digestion solution is colorless and transparent or slightly
yellow. Cool it; make constant volume to 25 mL or 50 mL with water; and mix it for later use.
Perform a blank test at the same time.
NOTE. For specimens with high tin content, it is recommended to add 1 mL of hydrochloric acid when
making the constant volume.
12.2.4 Dry digestion method (except for elements such as arsenic, cadmium, lead, sulfur,
selenium and tin)
Weigh 1.0 g ~ 5.0 g (accurate to 0.01 g, the specimen with high water content can be
appropriately increased to 15.0 g) of specimen, or accurately pipette 10.0 mL~15.0 mL of the
specimen into a crucible; carbonize it on an electric furnace with a low fire until it stops
smoking; and then place it in a muffle furnace at 500℃ ~550℃ for ash 5 h~8 h; and cool. If
the ash is not thorough and there are black carbon particles, add a little nitric acid to moisten it
after cooling; dry it on the electric hot plate; move it into the muffle furnace and continue to
ash it into white ash; cool it. Take it out; add 10 mL of nitric acid solution to dissolve it; and
make constant volume to 25 mL or 50 mL with water; mix it well for later use. Perform a blank
test at the same time.
12.3 Instrument reference conditions
Optimize the instrument operating conditions so that the sensitivity and other indicators of the
elements to be measured meet the analysis requirements; edit the determination method; select
the appropriate analytical spectrum line for each element to be measured. See B.3.1 for the
instrument operation reference conditions; and see Table B.6 for the recommended analytical
spectrum lines of the elements to be measured.
12.4 Drawing of standard curve
Introduce the standard solution into the inductively coupled plasma emission spectrometer;
measure the intensity signal response value of the analytical spectrum line of the element to be
measured; and draw a standard curve with the concentration of the element to be measured as
the horizontal axis and the intensity signal response value of the analytical spectrum line as the
vertical axis.
12.5 Determination of specimen solution
Introduce the blank and specimen solutions into the inductively coupled plasma emission
spectrometer respectively; measure the intensity signal response value of the analytical
spectrum line of the element to be measured; and obtain the concentration of the element to be
measured in the digestion solution according to the standard curve.
13 Expression of Analysis Results
16 Principle
After the specimen is dissolved in nitric acid, it is measured by inductively coupled plasma
emission spectrometer. The qualitative analysis is carried out based on the element's
characteristic emission spectrum line wavelength; and the quantitative analysis is based on the
signal intensity of the element's spectrum line proportional to the element concentration.
17 Reagents and Materials
Unless otherwise specified, the reagents used in this method are all guaranteed reagents; and
the water is Grade-1 water specified in GB/T 6682.
17.1 Reagents
17.1.1 Nitric acid (HNO3).
17.1.2 Hydrochloric acid (HCl).
17.1.3 Argon (Ar). Argon (≥99.995%) or liquid argon.
17.2 Preparation of reagents
17.2.1 Nitric acid solution (10+90). Take 100 mL of nitric acid; slowly add it to 900 mL of
water; and mix well.
17.2.2 Nitric acid solution (4+96). Take 40 mL of nitric acid; slowly add it to 960 mL of water;
and mix well.
17.3 Standard solution
17.3.1 Element standard stock solution (1,000 mg/L or 10,000 mg/L). Calcium, copper, iron,
potassium, magnesium, manganese, sodium, phosphorus, zinc. Use single element standard
stock solution certified by the state and awarded with standard material/standard sample
certificate; and multi-element mixed standard stock solution can also be used.
17.3.2 Preparation of standard solution. Accurately pipette an appropriate amount of single
element standard stock solution or multi-element mixed standard stock solution; and dilute it
step by step with nitric acid solution (4+96) to prepare a series of mixed standard working
solutions. The mass concentration of each element is shown in Table C.1 of Appendix C.
18 Instruments and Equipment
18.1 Inductively coupled plasma optical emission spectrometer (ICP-OES).
18.2 Analytical balance. With sensitivity of 0.000 1 g.
18.3 Ultrasonic generator.
18.4 High-speed crusher.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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