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食品安全国家标准 食品中多元素的测定
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GB 5009.268-2016
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标准编号: GB 5009.268-2016 (GB5009.268-2016)
中文名称: 食品安全国家标准 食品中多元素的测定
英文名称: 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
行业: 国家标准
中标分类: C53;X82
国际标准分类: 67.100.10
字数估计: 16,192
发布日期: 2016-12-23
实施日期: 2017-06-23
旧标准 (被替代): GB 5413.21-2010 Partly; GB/T 23545-2009; GB/T 23374-2009; GB/T 18932.11-2002; SN/T 0856-2011 Partly; SN/T 2208-2008; SN/T 2056-2008; SN/T 2049-2008; SN/T 2207-2008; NY/T 1653-2008
标准依据: National Health and Family Planning Commission Notice No.17 of 2016
发布机构: 中华人民共和国国家卫生和计划生育委员会、国家食品药品监督管理总局
范围: 本标准规定了食品中多元素测定的电感耦合等离子体质谱法(ICP-MS)和电感耦合等离子体发射光谱法(ICP-OES)。第一法适用于食品中硼、钠、镁、铝、钾、钙、钛、钒、铬、锰、铁、钴、镍、铜、锌、砷、硒、锶、钼、镉、锡、锑、钡、汞、铊、铅的测定；第二法适用于食品中铝、硼、钡、钙、铜、铁、钾、镁、锰、钠、镍、磷、锶、钛、钒、锌的测定。
GB 5009.268-2016: 食品安全国家标准 食品中多元素的测定
GB 5009.268-2016 英文名称: 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
中华人民共和国国家标准
1 范围
本标准规定了食品中多元素测定的电感耦合等离子体质谱法(ICP-MS)和电感耦合等离子体发射
光谱法(ICP-OES)。
第一法适用于食品中硼、钠、镁、铝、钾、钙、钛、钒、铬、锰、铁、钴、镍、铜、锌、砷、硒、锶、钼、镉、锡、锑、
钡、汞、铊、铅的测定;第二法适用于食品中铝、硼、钡、钙、铜、铁、钾、镁、锰、钠、镍、磷、锶、钛、钒、锌的测定。
第一法 电感耦合等离子体质谱法(ICP-MS)
5 分析步骤
5.1 试样制备
5.1.1 固态样品
5.1.1.1 干样
豆类、谷物、菌类、茶叶、干制水果、焙烤食品等低含水量样品,取可食部分,必要时经高速粉碎机粉
碎均匀;对于固体乳制品、蛋白粉、面粉等呈均匀状的粉状样品,摇匀。
5.1.1.2 鲜样
蔬菜、水果、水产品等高含水量样品必要时洗净,晾干,取可食部分匀浆均匀;对于肉类、蛋类等样品取可食部分匀浆均匀。
5.1.1.3 速冻及罐头食品
经解冻的速冻食品及罐头样品,取可食部分匀浆均匀。
5.1.2 液态样品软饮料、调味品等样品摇匀。
5.1.3 半固态样品搅拌均匀。
5.2 试样消解
注:可根据试样中待测元素的含量水平和检测水平要求选择相应的消解方法及消解容器。
5.2.1 微波消解法
称取固体样品0.2g~0.5g(精确至0.001g,含水分较多的样品可适当增加取样量至1g)或准确移
取液体试样1.00mL~3.00mL于微波消解内罐中,含乙醇或二氧化碳的样品先在电热板上低温加热
除去乙醇或二氧化碳,加入5mL~10mL硝酸,加盖放置1h或过夜,旋紧罐盖,按照微波消解仪标准
操作步骤进行消解(消解参考条件见表B.1)。冷却后取出,缓慢打开罐盖排气,用少量水冲洗内盖,将
消解罐放在控温电热板上或超声水浴箱中,于100℃加热30min或超声脱气2min~5min,用水定容
至25mL或50mL,混匀备用,同时做空白试验。
5.2.2 压力罐消解法
称取固体干样0.2g~1g(精确至0.001g,含水分较多的样品可适当增加取样量至2g)或准确移取
液体试样1.00mL~5.00mL于消解内罐中,含乙醇或二氧化碳的样品先在电热板上低温加热除去乙
醇或二氧化碳,加入5mL硝酸,放置1h或过夜,旋紧不锈钢外套,放入恒温干燥箱消解(消解参考条件
见表B.1),于150℃~170℃消解4h,冷却后,缓慢旋松不锈钢外套,将消解内罐取出,在控温电热板上
或超声水浴箱中,于100℃加热30min或超声脱气2min~5min,用水定容至25mL或50mL,混匀备用,同时做空白试验。
5.3 仪器参考条件
5.3.1 仪器操作条件:仪器操作条件见表B.2;元素分析模式见表B.3。
注:对没有合适消除干扰模式的仪器,需采用干扰校正方程对测定结果进行校正,铅、镉、砷、钼、硒、钒等元素干扰
校正方程见表B.4。
5.3.2 测定参考条件:在调谐仪器达到测定要求后,编辑测定方法,根据待测元素的性质选择相应的内
标元素,待测元素和内标元素的m/z见表B.5。
5.4 标准曲线的制作
将混合标准溶液注入电感耦合等离子体质谱仪中,测定待测元素和内标元素的信号响应值,以待测
元素的浓度为横坐标,待测元素与所选内标元素响应信号值的比值为纵坐标,绘制标准曲线。
5.5 试样溶液的测定
将空白溶液和试样溶液分别注入电感耦合等离子体质谱仪中,测定待测元素和内标元素的信号响
应值,根据标准曲线得到消解液中待测元素的浓度。
7 精密度
样品中各元素含量大于1mg/kg时,在重复性条件下获得的两次独立测定结果的绝对差值不得超
过算术平均值的10%;小于或等于1mg/kg且大于0.1mg/kg时,在重复性条件下获得的两次独立测
定结果的绝对差值不得超过算术平均值的15%;小于或等于0.1mg/kg时,在重复性条件下获得的两
次独立测定结果的绝对差值不得超过算术平均值的20%。
8 其他固体样品以0.5g定容体积至50mL,液体样品以2mL定容体积至50mL计算,本方法各元素的
检出限和定量限见表1。
9 原理
样品消解后,由电感耦合等离子体发射光谱仪测定,以元素的特征谱线波长定性;待测元素谱线信
号强度与元素浓度成正比进行定量分析。
10 试剂和材料除非另有说明,本方法所用试剂均为优级纯,水为GB/T 6682规定的一级水。
10.1 试剂
10.1.1 硝酸(HNO3):优级纯或更高纯度。
10.1.2 高氯酸(HClO4):优级纯或更高纯度。
10.1.3 氩气(Ar):氩气(≥99.995%)或液氩。
10.2 试剂配制
10.2.1 硝酸溶液(5+95):取50mL硝酸,缓慢加入950mL水中,混匀。
10.2.2 硝酸-高氯酸(10+1):取10mL高氯酸,缓慢加入100mL硝酸中,混匀。
10.3 标准品
10.3.1 元素贮备液(1000mg/L或10000mg/L):钾、钠、钙、镁、铁、锰、镍、铜、锌、磷、硼、钡、铝、锶、
钒和钛,采用经国家认证并授予标准物质证书的单元素或多元素标准贮备液。
10.3.2 标准溶液配制:精确吸取适量单元素标准贮备液或多元素混合标准贮备液,用硝酸溶液(5+95)逐
级稀释配成混合标准溶液系列,各元素质量浓度见表A.2。
注:依据样品溶液中元素质量浓度水平,可适当调整标准系列各元素质量浓度范围。
11 仪器和设备
11.1 电感耦合等离子体发射光谱仪。
11.2 天平:感量为0.1mg和1mg。
11.3 微波消解仪:配有聚四氟乙烯消解内罐。
11.4 压力消解器:配有聚四氟乙烯消解内罐。
11.5 恒温干燥箱。
11.6 可调式控温电热板。
11.7 马弗炉。
11.9 样品粉碎设备:匀浆机、高速粉碎机。
12 分析步骤
12.1 试样制备同5.1。
12.2 试样消解注:可根据试样中目标元素的含量水平和检测水平要求选择相应的消解方法及消解容器。
12.2.1 微波消解法同5.2.1。
12.2.2 压力罐消解法同5.2.2。
12.2.3 湿式消解法
准确称取0.5g~5g(精确至0.001g)或准确移取2.00mL~10.0mL试样于玻璃或聚四氟乙烯消
解器皿中,含乙醇或二氧化碳的样品先在电热板上低温加热除去乙醇或二氧化碳,加10mL硝酸-高氯
量混合酸,直至冒白烟,消化液呈无色透明或略带黄色,冷却,用水定容至25mL或50mL,混匀备用;同时做空白试验。
12.2.4 干式消解法
准确称取1g~5g(精确至0.01g)或准确移取10.0mL~15.0mL试样于坩埚中,置于500℃~
550℃的马弗炉中灰化5h~8h,冷却。若灰化不彻底有黑色炭粒,则冷却后滴加少许硝酸湿润,在电
热板上干燥后,移入马弗炉中继续灰化成白色灰烬,冷却取出,加入10mL硝酸溶液溶解,并用水定容
至25mL或50mL,混匀备用;同时做空白试验。
12.3 仪器参考条件
优化仪器操作条件,使待测元素的灵敏度等指标达到分析要求,编辑测定方法、选择各待测元素合
适分析谱线,仪器操作参考条件见B.3.1,待测元素推荐分析谱线见表B.6。
将标准系列工作溶液注入电感耦合等离子体发射光谱仪中,测定待测元素分析谱线的强度信号响
应值,以待测元素的浓度为横坐标,其分析谱线强度响应值为纵坐标,绘制标准曲线。
12.5 试样溶液的测定
将空白溶液和试样溶液分别注入电感耦合等离子体发射光谱仪中,测定待测元素分析谱线强度的
信号响应值,根据标准曲线得到消解液中待测元素的浓度。
14 精密度同第7章。
15 其他
固体样品以0.5g定容体积至50mL,液体样品以2mL定容体积至50mL计算,本方法各元素的检出限和定量限见表2。
GB 5009.268-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard –
Determination of multi-elements in foods
ISSUED ON. DECEMBER 23, 2016
IMPLEMENTED ON. JUNE 23, 2017
Issued by. National Health and Family Planning Commission of the PRC;
State Food and Drug Administration.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle... 4
3 Reagents and materials ... 4
4 Instruments and equipment ... 6
5 Analytical procedures ... 6
6 Expression of analysis results ... 8
7 Precision... 10
8 Others ... 10
9 Principle... 11
10 Reagents and materials... 11
11 Instruments and equipment ... 12
12 Analytical procedures ... 12
13 Expression of analytical results ... 14
14 Precision ... 14
15 Others ... 14
Appendix A Mass concentration of standard solution series ... 16
Appendix B Instrument reference conditions ... 18
National food safety standard –
Determination of multi-elements in foods
1 Scope
This standard specifies inductively coupled plasma mass spectrometry (ICP-
MS) and inductively coupled plasma emission spectrometry (ICP-OES) for the
determination of multi-element in foods.
The 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, molybdenum, cadmium, tin,
antimony, mercury, thallium, and lead in foods; the 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 in foods.
Method I. Inductively coupled plasma mass spectrometry (ICP-MS)
2 Principle
The sample is digested and determined by inductively coupled plasma mass
spectrometry. It is subject to qualitative determination by the specific mass
number of element (mass/charge ratio, m/z). The quantitative analysis is
performed by the use of external standard method and by that the ratio between
the strength ratio of the mass spectrometry signal of the tested element to the
internal standard element mass spectrometry signal and the concentration of
the element to be determined.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are all guaranteed
grade, the water is a level 1 water as specified in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3). Guaranteed grade or higher purity.
3.1.2 Argon (Ar). Argon (≥ 99.995%) or liquid argon.
3.1.3 Helium (He). Helium (≥ 99.995%).
internal standard use solution of appropriate concentration, the concentration
of the internal standard use solution is as shown in A.2.
Note. The internal standard solution can either be manually added
quantitatively in the preparation of mixed standard working solution and sample
digestion solution, or be added online by the instrument.
4 Instruments and equipment
4.1 Inductively coupled plasma mass spectrometry (ICP-MS).
4.2 Balance. The sensitivity is 0.1 mg and 1 mg.
4.3 Microwave digestion instrument. 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 control electric heating plate.
4.8 Sample crushing equipment. Homogenizer, high-speed crusher.
5 Analytical procedures
5.1 Specimen preparation
5.1.1 Solid sample
5.1.1.1 Dry sample
For the samples of low moisture content such as beans, cereals, fungi, tea,
dried fruits, baked goods, etc., TAKE the edible parts, if necessary, USE high-
speed crusher to crush it evenly; for the uniform powder sample such as solid
dairy products, protein powder, flour, etc., SHAKE it uniformly.
For the samples of high moisture content such as vegetables, fruits, and aquatic
products, it shall be washed clean when necessary, dried naturally, and the
edible parts shall be homogenized uniformly; for such samples as meat, eggs,
etc., the edible parts shall be homogenized uniformly.
5.1.1.3 Frozen and canned food
the digestion tank on the temperature control electric hot plate or in the
ultrasonic bath, HEAT it at 100 °C for 30 min or PERFORM ultrasonic degassing
for 2 min ~ 5 min, USE water to make the volume reach to 25 mL or 50 mL, MIX
it uniformly to prepare for use, meanwhile PERFORM blank test.
5.3.1 Instrument operating conditions. Instrument operating conditions are
shown in Table B.2; elemental analysis modes are shown in Table B.3.
Note. For instruments that do not have a suitable interference elimination mode,
the interference correction equation shall be used to correct the measurement
results. The interference correction equations for lead, cadmium, arsenic,
molybdenum, selenium, vanadium, and other elements are given in Table B.4.
5.3.2 Determination reference conditions. After tuning the instrument to meet
the measurement requirements, EDIT the measurement method and SELECT
the appropriate internal standard element based on the nature of the element
standard element.
5.4 Production of standard curves
INJECT the mixed standard solution into an inductively coupled plasma mass
spectrometer, to measure the signal response values of the test element and
the internal standard element. USE the concentration of the test element as the
abscissa and the ratio of the response signal value of the test element to the
selected internal standard element as the ordinate, to draw a standard curve.
5.5 Determination of specimen solution
Respectively INJECT the blank solution and the specimen solution into an
values of the test element and the internal standard element, and to obtain the
concentration of the test element in the digestion solution in accordance with
the standard curve.
6 Expression of analysis results
6.1 Calculation of low-content test elements
The content of the low-content test element in the specimen is calculated in
accordance with the formula (1).
12.2.1 Microwave digestion method
Same as 5.2.1.
Same as 5.2.2.
12.2.3 Wet digestion method
Accurately WEIGH 0.5 g ~ 5 g (accurate to 0.001 g) or accurately PIPETTE
2.00 mL ~ 10.0 mL of specimen in glass or PTFE digestion vessel; for the
sample containing ethanol or carbon dioxide, first HEAT it on a hot plate at low
temperature to remove ethanol or carbon dioxide, ADD 10 mL of nitric acid-
perchloric acid (10 + 1) mixed solution, MAKE it subject to digestion on an
electric hot plate or graphite digestion device, if the digestion solution becomes
brown and black in the digestion process, it may add a small amount of mixed
colorless, transparent or slightly yellow, COOL it, USE water to make its volume
reach to 25 mL or 50 mL, MIX it uniformly to prepare for use; meanwhile
PERFORM blank test.
12.2.4 Dry digestion method
Accurately WEIGH 1 g ~ 5 g (accurate to 0.01 g) or accurately PIPETTE 10.0
mL ~ 15.0 mL of specimen in the crucible, PLACE it in 500 °C ~ 550 °C muffle
furnace to ash it for 5 h ~ 8 h, COOL it down. If the ash is not complete, there
will be black charcoal particles, then ADD a little nitric acid to wet it after cooling,
after drying it on an electric hot plate, TRANSFER it into the muffle furnace to
acid solution to dissolve it, USE water to make its volume reach to 25 mL or 50
mL, MIX it uniformly to prepare for use; meanwhile PERFORM blank test.
12.3 Instrument reference conditions
OPTIMIZE the operating conditions of the instrument, so that the sensitivity of
the element to be determined meets the analysis requirements. EDIT the
determination method and SELECT the appropriate analysis spectral line of
each test element, the instrument operating conditions are as shown in B.3.1,
the recommended analysis spectral line of the test element is as shown in Table
B.6.
INJECT the standard series working solution into an inductively coupled plasma
emission spectrometer, to measure the strength signal response value of the
analytical spectral line of the test element. USE the concentration of the test
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