Determination of Multiple Elements in Food 1 - National Food Safety Standard
Publish Date: 2016-12-23
Implement date: 2017-06-23
Issued by: The National Health and Family Planning Commission of the People's Republic of China, and the State Food and Drug Administration
Standard Status: currently valid
This is the National Standard of the People's Republic of China, GB5009-268-2016, Determination of Multiple Elements in Food, there are two analytical methods. Method 1: Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Method 2: Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). This article describes the Method 1.
The Method 1 of this standard specifies inductively coupled plasma mass spectrometry (ICP-MS) for the determination of multiple elements in food. Suitable for determination of boron, sodium, magnesium, aluminum, potassium, calcium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, arsenic, selenium, strontium, molybdenum, cadmium, tin, antimony, barium, mercury, thallium and lead in food.
The English version of this standard is translated from the Chinese original GB5009-268-2016. In case of discrepancies in the translated version, the original Chinese standard GB5009-268-2016 (Chinese version) shall prevail. This translated version can provide reference for food production enterprises.
Standard Text of GB5009-268-2016
A. Standard Cover of GB5009-268-2016
B. Table of contents
C. Standard Preface of GB5009-268-2016
Foreword
This standard replaces:
* The second method of GB5413.21-2010 "National Food Safety Standard, Determination of Calcium, Iron, Zinc, Sodium, Potassium, Magnesium, Copper and Manganese in Infant and Young Children's Food and Dairy";
* GB/T23545-2009 Determination of Manganese in "Liquor", Inductively Coupled Plasma Atomic Emission Spectrometry";
* GB/T23374-2009 "Determination of Aluminum in Food, Inductively Coupled Plasma Mass Spectrometry";
* GB/T18923.11-2002 "Determination method of Potassium, Phosphorus, Iron, Calcium, Zinc, Aluminum, Sodium, Magnesium, Boron, Manganese, Copper, Barium, Titanium, Vanadium, Nickel, Cobalt and Chromium Content in Honey, Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES);
* The second method of SN/T0856-2011 "Testing Methods for Tin in Canned food for Import and Export";
* SN/T2208-2008 "Determination of Sodium, Magnesium, Aluminum, Calcium, Chromium, Iron, Nickel, Copper, Zinc, Arsenic, Strontium, Molybdenum, Cadmium, Lead, Mercury and Selenium in Aquatic Products, Microwave Digestion-Inductively Coupled Plasma-Mass Spectrometry";
* SN/T2056-2008 "Determination of lead, arsenic, cadmium, copper and iron content in imported and exported tea, inductively coupled plasma atomic emission spectrometry";
* SN/T2049-2008 "Determination of copper, nickel, lead, manganese, cadmium and titanium in import and export food grade phosphoric acid, inductively coupled plasma atomic emission spectrometry";
* SN/T2207-2008 "Determination of Arsenic, Calcium and Lead Content in Imported and Exported Food Additives DL-Tartaric Acid, Inductively Coupled Plasma Atomic Emission Spectrometry";
* NY/T1653-2008 "Determination of Mineral Elements in Vegetables, Fruits and Products, Inductively Coupled Plasma Emission Spectroscopy".
Compared with the second method of GB5413.21-2010, the main changes of this standard are as follows:
—— The name of the standard was changed to "National Food Safety Standard - Determination of Multiple Elements in Food";
—— Added inductively coupled plasma mass spectrometry as the first method;
—— Modify inductively coupled plasma emission spectrometry as the second method;
—— Modified the scope of application;
—— Modified some contents of sample preparation;
—— Modified the content of sample digestion;
—— Increased method detection limit and quantification limit
D. Standard Content of GB5009-268-2016
National Food Safety Standard
Determination of Multiple Elements in Food
1. Scope
The first method is suitable for the determination of boron, sodium, magnesium, aluminum, potassium, calcium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, arsenic, selenium, strontium, molybdenum, cadmium, tin, antimony, barium, mercury, thallium and lead in food. The second method is applicable to the determination of aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium and zinc in food.
This standard specifies inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES) for the determination of multiple elements in food.
The First Method: Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
2. Principle
After the sample is digested, it is determined by inductively coupled plasma mass spectrometer, and qualitative analysis is carried out with the specific mass number (mass-to-charge ratio, m/z) of the element. Using the external standard method, quantitative analysis is carried out with the intensity ratio of the mass spectrum signal of the element to be tested and the mass spectrum signal of the internal standard element in direct proportion to the concentration of the element to be tested.
3. Reagents and Materials
Unless otherwise stated, all reagents used in this method are of guaranteed reagent (Gr). The water is the first grade water specified in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3): Guaranteed reagent (Gr) or higher purity.
…….
3.2 Reagent Preparation
3.2.1 Nitric acid solution (5+95): Take 50 mL of nitric acid, slowly add it to 950 mL of water …….
…….
3.3 Standard Chemicals
3.3.1 Elemental stock solution (1000mg/L or 100mg/L): lead, cadmium, arsenic …….
…….
3.4 Standard Solution Preparation
3.4.1 Mixed standard working solution: Take an appropriate amount of single-element standard stock solution or multi-element mixed standard stock ……. The mass concentration of each element is shown in Table A.1.
Table A.1 Mass concentration of standard solution series of elements in the ICP-MS Method
Note: According to the element mass concentration level in the sample digestion solution, appropriately adjust the mass concentration range of each element in the standard series.
…….
4. Instruments and Equipment
4.1 Inductively coupled plasma mass spectrometer (ICP-MS)
4.2 Balance: Sensitive amount is 0.1mg and 1mg.
4.3 Microwave Digestion Apparatus: Equipped with PTFE digestion inner tank.
4.4 Pressure digestion tank: Equipped with PTFE digestion inner tank.
4.5 Constant temperature drying oven
4.6 Temperature-controlled electric heating plate
4.7 Ultrasonic water bath
4.8 Sample crushing equipment: homogenizer, high-speed crusher
5. Analysis steps
5.1 Specimen Preparation
5.1.1 Solid samples
5.1.1.1 Dry samples
For samples with low water content such as beans, grains …….
…….
5.1.2 Liquid samples
Samples of soft drinks, condiments, etc., shake well.
5.1.3 Semi-solid samples
Stir well.
5.2 Sample digestion
Note: …….
5.2.1 Microwave digestion
Weigh 0.2g～0.5g of solid sample (accurate to 0.001g, the sample with more water content can be appropriately increased to 1g) or …….
Table B.1 Reference Conditions for Sample Digestion Apparatus
5.2.2 Pressure tank digestion method
Weigh 0.2g ~ 1g of solid dry sample …….
5.3 Instrument reference conditions
5.3.1 Instrument operating conditions: the operating conditions of the instrument are shown in Table B.2; the elemental analysis mode is shown in Table B.3.
Table B.2 Operational Reference Conditions for Inductively Coupled Plasma Mass Spectrometer
Table B.3 Elemental Analysis Mode of Inductively Coupled Plasma Mass Spectrometer
Note: For instruments without a suitable interference elimination mode, the interference correction equation should be used to correct the measurement results. The interference correction equation of lead, cadmium, arsenic, molybdenum, selenium, vanadium and other elements is shown in Table B.4.
Table B.4 Elemental Interference Correction Equation Reference Table
5.3.2 Measurement reference conditions: After tuning the …….
Table B.5 Reference table for selection of isotopes of elements to be measured and isotopes of internal standard elements (m/z)
5.4 Preparation of standard curve
The mixed standard solution was injected into the…….
5.5 Determination of sample solution
…….
6. Presentation of analysis results
6.1 Calculation of low-content analyte elements
The content of the low-content element to be tested in the sample is calculated according to formula (1):
----------- (1)
In formula (1):
X --- The content of the element to be measured in the sample, in milligrams per kilogram or milligrams per liter (mg/kg or mg/L);
ρ --- Mass concentration of the tested element in the sample solution, in micrograms per liter (μg/L);
…….
6.2 Calculation of high-content analyte elements
The content of the high-content element to be measured in the sample is calculated according to formula (2):
------------- (2)
In formula (2):
X ---- The content of the element to be measured in the sample, in milligrams per kilogram or milligrams per liter (mg/kg or mg/L);
…….
7. Precision
When the content of each element …….
8 Others
The solid sample is calculated from a constant volume of 0.5 g to 50mL. Liquid samples are calculated from a constant volume of 2 mL to 50mL. The detection limit and quantification limit of each element in this method are shown in Table 1.
Table 1 Inductively coupled plasma mass spectrometry (ICP-MS) detection limit and quantification limit
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Note: Commonly used Chinese food standards include mandatory national standards (the code starts with "GB") and recommended national standards (the code starts with "GB/T")
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References Articles
1. Principle of Inductively Coupled Plasma-Mass Spectrometer (ICP-MS)
2. Principle of Inductively Coupled Plasma - Optical Emission Spectrometer
3. Determination of Tin in Food 1 - National Food Safety Standard
4. Determination of Tin in Food 2 - National Food Safety Standard
5. Hazard Analysis and Critical Control Point (HACCP) System - General Requirements for Food Processing Plant
6. General Hygienic Regulation for Food Production - National Food Safety Standard
7. GB5749—2022 Standards for Drinking Water Quality
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Related Testing Equipment
1. SUP-70 Inductively Coupled Plasma-Mass Spectrometer ( ICP-MS): can detect dozens of elements and isotopes at one time, ultra-trace analysis, automatic.
2. SUP-70M Vehicle-mounted Inductively Coupled Plasma-Mass Spectrometer: can detect dozens of elements and isotopes in one-time ultra-trace, anti-vibration.
3. SUP-72 Inductively Coupled Plasma-Mass Spectrometer: is a high-sensitivity, rapid food detection and ultra-trace analysis instrument, automatic.
4. SUP-735 Inductively Coupled Plasma-Mass Spectrometer ( ICP-MS /MS, ICP-QQQ ): is a space tandem multi-stage quadrupole mass spectrometer equipped with an inductively coupled plasma.
5. Laboratory Equipment and Instruments: include precision weighing equipment, evaporators, drying ovens and food testing instruments.
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