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食品安全国家标准 食品接触材料及制品 丙烯酰胺迁移量的测定
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GB 31604.18-2016
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标准编号: GB 31604.18-2016 (GB31604.18-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 丙烯酰胺迁移量的测定
英文名称: Food contact materials -- Polymer -- Determination of acrylamide in food simulants -- High performance liquid chromatography
行业: 国家标准
中标分类: X09
字数估计: 8,884
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): GB/T 23296.9-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.18-2016: 食品安全国家标准 食品接触材料及制品 丙烯酰胺迁移量的测定
GB 31604.18-2016 英文名称: Food contact materials -- Polymer -- Determination of acrylamide in food simulants -- High performance liquid chromatography
1 范围
本标准规定了食品接触材料及制品中丙烯酰胺迁移量的测定。
本标准适用于食品接触材料及制品中丙烯酰胺迁移量的液相色谱法检测。
2 原理
对于食品接触材料及其制品的食品模拟物采用液相色谱进行检测,其中水基、酸性、酒精类食品模
拟物直接进样,油基食品模拟物通过水萃取后进样,通过高效液相色谱(色谱柱为离子排斥柱)进行分
离,采用紫外检测器进行检测,方法采用外标峰面积法定量。
3 试剂和材料
除非另有说明,本方法所用试剂均为分析纯,水为GB/T 6682规定的一级水。试验中容器及转移
器具应避免使用塑料材质。
3.1 试剂
3.1.1 水基、酸性、酒精类、油基食品模拟物:所用试剂依据GB 31604.1的规定。
3.1.2 乙腈(C2H3N):色谱纯。
3.1.3 甲醇(CH3OH):色谱纯。
3.1.4 硫酸(H2SO4):优级纯。
3.2 试剂配制
3.2.1 水基、酸性、酒精类、油基食品模拟物:根据待测样品的预期用途和使用条件,按GB 5009.156
操作。
3.2.2 硫酸溶液(0.0036mol/L):量取0.1mL硫酸,用水定容至500mL,混匀。
3.3 标准品
丙烯酰胺(C3H5NO):纯度≥99%。
3.4 标准溶液配制
3.4.1 丙烯酰胺标准储备溶液(1000mg/L):准确称取丙烯酰胺标准品10mg(精确至0.1mg),用甲
醇定容至10mL,该储备液储存于0℃~4℃冰箱中。
3.4.2 丙烯酰胺标准中间溶液(10mg/L):吸取1.0mL丙烯酰胺贮备液用甲醇定容至100mL。
4 仪器和设备
4.1 高效液相色谱仪:配有紫外检测器。
4.2 分析天平:感量0.1mg和0.01g。
4.3 微孔滤膜:0.2μm。
4.4 具塞比色管:25mL。
5 分析步骤
5.1 试液制备
5.1.1 食品模拟物试液的制备
根据待测样品的预期用途和使用条件,按照GB 5009.156和GB 31604.1规定的迁移试验方法及试
验条件进行迁移试验。迁移试验结束后,将迁移试验所得模拟物充分混匀后,用于以下分析。
5.1.2 水基、酸性、酒精类食品模拟物试液的制备
将食品模拟物试液通过0.2μm微孔滤膜过滤后供测定用。
5.1.3 油基食品模拟物试液的制备
称取10g(精确至0.01g)油基食品模拟物试液至比色管中,加入10.0mL水,剧烈振荡1min,静置
分层。取下层水溶液,通过0.2μm滤膜过滤后供测定用。
5.1.4 空白溶液的制备
5.1.4.1 水基、酸性、酒精类食品模拟物空白溶液
移取未与样品接触过的食品模拟物,通过0.2μm微孔滤膜过滤后供测定用。
5.1.4.2 油基食品模拟物空白溶液
移取10g(精确至0.01g)未与样品接触过的食品模拟物,按照5.1.3操作。
5.1.5 水基、酸性、酒精类食品模拟物标准工作溶液
准确吸取丙烯酰胺标准中间溶液0.00mL、0.03mL、0.05mL、0.08mL、0.1mL、0.5mL于10mL
容量瓶中,用未与样品接触过的食品模拟物定容,得到丙烯酰胺浓度分别为0.00mg/L、0.03mg/L、
0.05mg/L、0.08mg/L、0.10mg/L、0.50mg/L的标准工作液。采用同样方式,分别用对应水基、酸性、
酒精类食品模拟物配制同样浓度系列的丙烯酰胺标准工作溶液。
5.1.6 油基食品模拟物标准工作溶液
分别称取10g(精确至0.01g)油基食品模拟物至5个比色管中,分别吸取丙烯酰胺标准中间溶液
(10mg/L)0.00mL、0.03mL、0.05mL、0.08mL、0.1mL、0.5mL于比色管中,混匀,加入10.0mL水,
剧烈振荡1min,静置分层。得到丙烯酰胺浓度分别为0.00mg/kg、0.03mg/kg、0.05mg/kg、0.08mg/kg、
0.10mg/kg、0.50mg/kg的标准工作液。取下层水溶液,通过0.2μm滤膜过滤后供测定用。
5.2 测定
5.2.1 液相色谱条件
a) 色谱柱:VenusilCIS,离子排斥色谱柱,柱长250mm,内径4.6mm,粒径5μm,或相当者;
b) 流动相:硫酸溶液:乙腈(91+9);
c) 流速:0.5mL/min;
d) 柱温:50℃;
e) 紫外检测器:波长198nm;
f) 进样量:20μL。
5.2.2 色谱测定
对标准溶液及样液依次进样测定,以标准工作溶液中丙烯酰胺浓度为横坐标,单位以“mg/L或
mg/kg”表示;以对应的峰面积为纵坐标,绘制标准曲线。用保留时间定性,外标法定量。在上述色谱条
件下丙烯酰胺保留时间为11.6min,色谱图见附录A。
6 分析结果的表述
由标准曲线得到试样溶液中丙烯酰胺的浓度,按GB 5009.156进行迁移量计算,得到食品接触材料
及制品中丙烯酰胺的迁移量。计算结果保留至小数点后两位。
7 精密度
在重复的条件下获得的两次独立测定结果的绝对差值不得超过10%。
8 其他
本方法对水基、酸性、酒精类食品模拟物中丙烯酰胺的检出限为0.01mg/L,油基食品模拟物中丙
烯酰胺的检出限为0.01mg/kg。
本方法对水基、酸性、酒精类食品模拟物中丙烯酰胺的定量限为0.03mg/L,油基食品模拟物中丙
烯酰胺的定量限为0.03mg/kg。
GB 31604.18-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard - Food contact materials
and articles - Determination of migration of acrylamide
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of the PRC
Table of Contents
Foreword . 3
1 Scope .. 4
2 Principle.. 4
3 Reagents and materials .. 4
4 Instruments and equipment . 5
5 Analytical procedures . 5
6 Expression of analysis results .. 7
7 Precision. 7
8 Others . 8
Appendix A Standard solution chromatogram . 9
Foreword
This standard replaces GB/T 23296.9-2009 “Food contact materials - Polymer
- Determination of acrylamide in food simulants - High performance liquid
chromatography”.
As compared with GB/T 23296.9-2009, the main changes of this standard are
as follows.
- CHANGE the standard name into “National food safety standard - Food
contact materials and articles - Determination of migration of acrylamide”;
- ADD the scope of application;
- MODIFY the food simulant preparation;
- MODIFY the processing of oil-based food simulant test solutions.
National food safety standard - Food contact materials
and articles - Determination of migration of acrylamide
1 Scope
This standard specifies the determination of the migration of acrylamide in food
contact materials and articles.
This standard applies to the use of liquid chromatography for the detection of
acrylamide migration in food contact materials and articles.
2 Principle
The food simulants of food contact materials and articles are tested by liquid
chromatography, wherein the water-based, acidic, and alcoholic food simulants
are directly injected, the oil-based food simulants are injected after water
extraction and separated through high-performance liquid chromatography.
(The column is an ion exclusion column), detected by a UV detector, and it is
quantified using the external standard peak area method.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are of analytical
grade, and the water is grade I water as specified in GB/T 6682. Containers
and transfer apparatus used in the test shall avoid the use of plastic materials.
3.1 Reagents
3.1.1 Water-based, acidic, alcoholic, oil-based food simulants. The reagents
used shall be in accordance with the provisions of GB 31604.1.
3.1.2 Acetonitrile (C2H3N). Chromatographically pure.
3.1.3 Methanol (CH3OH). Chromatographically pure.
3.1.4 Sulfuric acid (H2SO4). Excellent grade.
3.2 Reagent preparation
3.2.1 Water-based, acidic, alcohol-based, oil-based food simulants. In
accordance with the expected use of the sample to be tested and the conditions
5.1.3 Preparation of oil-based food simulant test solution
WEIGH 10 g (accurate to 0.01 g) of oil-based food simulant test solution to the
colorimetric tube, ADD 10.0 mL of water, SHAKE it vigorously for 1 min, LET it
be standing for stratification. TAKE the lower layer aqueous solution, MAKE it
pass through a 0.2 μm filter membrane for measurement.
5.1.4 Preparation of blank solutions
5.1.4.1 Water-based, acidic, alcoholic food simulant blank solution
PIPETTE food simulant that had not been contacted with the sample, FILTER
it through a 0.2 μm microporous membrane for measurement.
5.1.4.2 Oil-based food simulant blank solution
PIPETTE 10 g (accurate to 0.01 g) of the food simulant that has not been
contacted with the sample, OPERATE in accordance with 5.1.3.
solution
Accurately PIPETTE 0.00 mL, 0.03 mL, 0.05 mL, 0.08 mL, 0.1 mL, 0.5 mL of
acrylamide standard intermediate solution in a 10 mL volumetric flask, USE the
food simulant that has not been in contact with the sample to make its volume
reach to the mark, to obtain the standard working solution which has a
concentration of acrylamide of 0.00 mg/L, 0.03 mg/L, 0.05 mg/L, 0.08 mg/L,
0.10 mg/L, 0.50 mg/L. In the same manner, respectively USE the corresponding
water-based, acidic, and alcoholic food simulants to prepare the same
concentration series of acrylamide standard working solutions.
Respectively WEIGH 10 g (accurate to 0.01 g) of oil-based food simulants into
5 colorimetric tubes, respectively PIPETTE 0.00 mL, 0.03 mL, 0.05 mL, 0.08
mL, 0.1 mL and 0.5 mL of acrylamide standard intermediate solution (10 mg/L)
in the colorimetric tube, MIX it uniformly, ADD 10.0 mL of water, SHAKE it
vigorously for 1 min, LET it be standing for stratification. The acrylamide
concentration of the obtained standard working solution is respectively 0.00
mg/kg, 0.03 mg/kg, 0.05 mg/kg, 0.08 mg/kg, 0.10 mg/kg, and 0.50 mg/kg. TAKE
the lower layer aqueous solution, MAKE it pass through a 0.2 μm filter
membrane for measurement.
5.2.1 Liquid chromatography conditions
a) Column. Venusil CIS, ion exclusion column, column length 250 mm, inner
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