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食品安全国家标准 动物源性食品中全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的测定
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GB 5009.253-2016
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标准编号: GB 5009.253-2016 (GB5009.253-2016)
中文名称: 食品安全国家标准 动物源性食品中全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的测定
英文名称: National Food Safety Standard -- Determination of Perfluorooctane Sulfonate (PFOS) and Perfluorooctanoic Acid (PFOA) in Animal-derived Food
行业: 国家标准
中标分类: X09
字数估计: 8,892
发布日期: 2016-08-31
实施日期: 2017-03-01
标准依据: 国家卫生和计划生育委员会公告2016年第11号
GB 5009.253-2016: 食品安全国家标准 动物源性食品中全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的测定
GB 5009.253-2016 英文名称: National Food Safety Standard -- Determination of Perfluorooctane Sulfonate (PFOS) and Perfluorooctanoic Acid (PFOA) in Animal-derived Food
中华人民共和国国家标准
1 范围
本标准规定了动物源性食品中全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)含量的同位素稀释液相
色谱-串联质谱测定方法。
本标准适用于动物源性食品中PFOS和PFOA含量的测定。
5 样品制备
鱼、虾、蟹、贝类、章鱼、鸡肉、猪肉、牛肉取其可食部分(去骨,去壳),切成小块,用粉碎机制成肉糜;
蛋品去壳,制成匀浆;牛奶,混匀备用。将样品置于玻璃样品瓶中,密封,标识后置于-18℃保存。
6 分析步骤
6.1 样品前处理
6.1.1 提取
称取试样5g(准确至0.01g)(样品使用前解冻均质),置于50mL聚丙烯离心管中,加入内标混合
使用溶液Ⅱ400μL,加水5mL,漩涡混合1min,加入10mL乙腈(3.2)和30μL盐酸(3.3),震荡
10min。加入2g氯化钠(3.4),再次振摇10min,以5000r/min离心10min。移取上层乙腈溶液于另
一试管中,在45℃水浴中氮气吹至约4mL,待净化。
6.1.2 净化
将上述溶液转移至装有100mgPSA(3.6)、40mgC18(3.7)和20mgGCB(3.8)的15mL聚丙烯离
心管中,振摇10min,以5000r/min离心10min,移取上清溶液于另一试管中,在45℃水浴中氮气吹
至干,用1mL甲醇(3.1)溶解,吸入1mL注射器,经0.22μm有机滤膜过滤后,待测。
6.2 测定
6.2.1 液相色谱参考条件
6.2.1.1 为降低高效液相色谱管道中引入的PFOS和PFOA的污染,液相系统中加一预柱,并对部分
特氟龙材质管路替换为PEEK管路或不锈钢管路。
6.2.1.2 分析色谱柱:C18,150mm×2.1mm(内径),5μm,或相当者。
6.2.1.3 预吸附柱:C18,50mm×4.6mm(内径),5μm,或相当者。
6.2.1.4 流动相梯度洗脱程序见表1。
6.2.1.5 流速:200μL/min。
6.2.1.6 进样量:10μL。
6.2.2 质谱参考条件
6.2.2.1 离子源:电喷雾离子源负离子模式(ESI-)。
6.2.2.2 扫描方式:多反应监测模式(MRM)。
6.2.2.3 分辨率:单位分辨率。其他质谱条件参见附录A。
6.2.3 定性测定
按照6.2.1和6.2.2所述条件测定试样和标准工作溶液,试样的质量色谱峰保留时间应与标准物质
一致,允许偏差小于±2.5%;定性离子对的相对丰度与浓度相当的标准工作溶液的相对丰度一致,定性
离子参考附录 A表 A.1,相对丰度允许偏差不超过表2规定的范围,则可判断样品中存在相应的被测物。
6.2.4 定量测定
以各混合系列标准工作溶液中的PFOA或PFOS浓度和PFOA或PFOS与其相对应的13C同位
素标记物的峰面积比绘制标准曲线,按照内标法进行定量计算。在6.2.1所述的色谱条件下,PFOA和
PFOS的参考保留时间约为7.66min和8.78min,13C4-PFOA和1,2,3,4-13C4-PFOS的参考保留时间
约为7.66min和8.79min,标准溶液的多反应监测(MRM)图参见附录B。
标准工作溶液和样液中待测物的响应值均应在标准曲线的线性响应范围内,如果含量超过范围,则
重新取样分析,增加相应内标添加量,使内标浓度与待测液浓度相匹配,然后用甲醇稀释到适当浓度后分析。
6.3 空白试验
除不加试样外,均按6.1及6.2所述操作步骤进行。
7 质量控制
7.1 取样抽样
取样抽样均应采用不锈钢仪器,避免接触塑料。
7.2 有机溶剂和试验器皿
本标准中使用到的所有有机溶剂及试验器皿,在使用前,应进行空白试验。如本底值高于定量限,
应对有机溶剂进行重蒸,或更换试验器皿,直至本底值低于定量限。
9 精密度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30%。
10 其他本方法PFOA和PFOS的检出限分别为0.002μg/kg和0.02μg/kg,定量限分别为0.01μg/kg和0.1μg/kg。
附 录 A
质谱参考条件
质谱参考条件:
a) 喷嘴电压:-500V;
b) 雾化气压力:45Pa;
c) 鞘气温度:260℃;
d) 鞘气流速:11L/min;
e) 干燥气温度:300℃;
f) 干燥气流速:6L/min;
g) 毛细管电压:-3500V;
h) 定性离子对、定量离子对、碎裂电压、碰撞电压、驻留时间见表A.1。
GB 5009.253-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Standard for Food Safety -
Determination of Perfluorooctane Sulfonate (PFOS) and
Perfluorooctanoic Acid (PFOA) in Animal-derived Food
ISSUED ON. AUGUST 31, 2016
IMPLEMENTED ON. MARCH 1, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China
Table of Contents
1 Scope ... 3
2 Principle ... 3
3 Reagents and Materials ... 3
4 Instruments and Equipment ... 5
5 Preparation of Samples ... 5
6 Analytical Procedures ... 5
7 Mass Control ... 7
8 Expression of Analysis Results ... 8
9 Precision ... 8
10 Others ... 8
Appendix A Mass Spectrometry Reference Conditions ... 10
Appendix B Typical Liquid Chromatography of PFOA and PFOS and the
Internal Standard – Tandem Mass Spectrometry MRM Figure ... 11
National Standard for Food Safety -
Determination of Perfluorooctane Sulfonate (PFOS) and
Perfluorooctanoic Acid (PFOA) in Animal-derived Food
1 Scope
This Standard specifies the method of isotope dilution liquid chromatography-tandem
mass spectrometry in the determination of PFOS and PFOA in animal-derived food.
This Standard shall be applicable to the determination of PFOS and PFOA in
animal-derived food.
2 Principle
Adopt acetonitrile to extract PFOS and PFOA from the sample. Start dispersive solid
phase extraction and purification; adopt liquid chromatography-tandem mass
spectrometer to determine PFOS and PFOA. Adopt the internal standard method to
quantify the content.
3 Reagents and Materials
Unless otherwise indicated, the reagents adopted under this method are of analytical
purity. The water is first-grade water as specified in GB/T 6682.
3.1 Methanol (CH3OH). chromatographic purity.
3.2 Acetonitrile (CH3CN). chromatographic purity.
3.3 Hydrochloric acid (HCl).
3.4 Sodium chloride (NaCl).
3.5 Ammonium acetate (CH3COONH4). chromatographic purity.
3.6 N-propyl ethylenediamine solid phase adsorbent (PSA). 40 μm~60 μm, ProElut
filler, or equivalent.
3.7 C18 absorbent. 40 μm~60 μm, ProElut filler, or equivalent.
3.8 Graphitized carbon black adsorbent (GCB). 40 μm~60 μm, ProElut filler, or
mixed series of standard working fluid of PFOA (density. 0.05 μg/L, 0.1 μg/L, 0.5 μg/L,
1.0 μg/L, 2.0 μg/L, 10.0 μg/L) and mixed series of standard working fluid of PFOS
(density. 0.1 μg/L, 0.2 μg/L, 1.0 μg/L, 10.0 μg/L, 20.0 μg/L, 40.0 μg/L). Prepare mixed
series of standard working solution of 13C4-PFOA (density. 1.0 μg/L) and 1, 2, 3,
4-13C4-PFOS (density. 5.0 μg/L) that contains 13C isotope. Store under the
temperature of -4°C. It can remain valid for 2 months.
4 Instruments and Equipment
4.1 Liquid chromatography-tandem mass spectrometer. equipped with ESI source.
4.2 Nitrogen blowing instrument.
4.3 Grinder.
4.4 Centrifuge, speed≥5,000 r/min.
4.5 Homogenizer, reference speed. 3,400 r/min~24,000 r/min.
4.6 Analytical balance. division value. 0.1 mg and 0.01 g.
5 Preparation of Samples
Take edible part (remove the bone and shell) from fish, shrimp, crab, shellfish,
octopus, chicken, pork and beef. Cut into small pieces, then, use grinder to make it
into meat paste; remove eggshell, then, homogenize it; mix up milk for later usage.
Place the sample in the glass sample bottle, seal it, label it; store it under the
temperature of -18°C.
6 Analytical Procedures
6.1.1 Extracting
Weigh-take 5 g (accurate to 0.01 g) of sample (before usage, unfreeze and
homogenize the sample); place it in 50 mL polypropylene centrifuge tube. Add 400 μL
of mixed standard solution II, then, add 5 mL of water. Start 1 min whirlpool mixing,
then, add 10 mL of acetonitrile (3.2) and 30 μL of hydrochloric acid (3.3); shake it for
10 min. Add 2 g of sodium chloride (3.4); shake again for 10 min; centrifuge at 5,000
r/min for 10 min. Remove supernatant acetonitrile solution, then, place it in another
tube. Place the tube in water bath at 45°C, then, blow nitrogen till it is dry. Add 1 mL of
methanol (3.1) to dilute; use injector to inhale 1 mL. Use 0.22 μm organic membrane
Before usage, conduct blank test on all organic solvents and test vessels adopted in
this Standard. If their base value is higher than the limit of quantitation, re-evaporate
the organic solvents, or replace the test vessels, until the base value is lower than the
limit of quantitation.
8 Expression of Analysis Results
The content of PFOA and PFOS in the sample shall be calculated in accordance with
Formula (1).
Where.
X - The content of PFOA or PFOS in the sample, expressed in (μg/kg);
chromatographic peak of corresponding internal standard substance in the test
solution, and PFOA or PFOS density obtained through standard curve line, expressed
in (μg/L);
Ao - The peak area ratio between PFOA or PFOS chromatographic peak and the
chromatographic peak of corresponding internal standard substance in the blank
solution, and PFOA or PFOS density obtained through standard curve line, expressed
in (μg/L);
V - The ultimate constant volume of the test solution, expressed in (mL);
f - Dilution times of the test solution;
The calculation result shall be expressed as the arithmetic mean value of two
independent determination results obtained under repeatability conditions. The result
shall retain two significant figures.
9 Precision
The absolute difference between the two independent determination results obtained
under repeatability conditions shall not exceed 30% of the arithmetic mean value.
10 Others
The detection limit of PFOA is 0.002 μg/kg; the detection limit of PFOS is 0.02 μg/kg.
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