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食品安全国家标准 食品接触材料及制品 1，3-丁二烯的测定和迁移量的测定
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GB 31604.12-2016
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标准编号: GB 31604.12-2016 (GB31604.12-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 1，3-丁二烯的测定和迁移量的测定
英文名称: Food contact materials -- Polymer -- Determination of 1, 3-butadiene in food simulants -- Gas chromatography
行业: 国家标准
中标分类: X09
字数估计: 10,131
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): GB/T 23296.3-2009; GB/T 23296.2-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.12-2016: 食品安全国家标准 食品接触材料及制品 1，3-丁二烯的测定和迁移量的测定
GB 31604.12-2016 英文名称: Food contact materials -- Polymer -- Determination of 1, 3-butadiene in food simulants -- Gas chromatography
1 范围
本标准规定了食品接触材料及制品中1,3-丁二烯的测定方法和迁移量的测定方法。
本标准适用于食品接触材料及制品中1,3-丁二烯的测定和迁移量的测定。
1,3-丁二烯的测定
2 原理
食品接触材料及制品经N,N-二甲基甲酰胺溶解或分散于顶空瓶中,加热使待测成分达到气液平
衡,然后定量吸取顶空气进行气相色谱测定。根据保留时间定性,n-戊烷作为内标物,以内标法定量。
3 试剂和材料
本方法所用水为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
N,N-二甲基甲酰胺(DMF):分析纯,在1,3-丁二烯和n-戊烷保留时间处无干扰峰。
3.2 标准品
3.2.1 1,3-丁二烯(C4H6,CAS号:106-99-0):2000μg/mL,或经国家认证并授予标准物质证书的标准
物质。
3.2.2 n-戊烷(C5H12,CAS号:106-66-0):纯度大于99.5%,或经国家认证并授予标准物质证书的标准
物质。
3.3 1,3-丁二烯标准溶液配制
3.3.1 1,3-丁二烯标准贮备液:吸取1,3-丁二烯标准品1.0mL移入10mL容量瓶中,加入N,N-二甲
基甲酰胺稀释至刻度,混匀,此溶液中1,3-丁二烯浓度为200μg/mL,避光保存,于-20℃保存,有效期
3个月,或于4℃保存,有效期为一周。
3.3.2 1,3-丁二烯标准使用液:吸取1,3-丁二烯标准贮备液0.1mL、0.2mL、0.3mL、0.4mL、0.5mL,
分别移入10mL容量瓶中,各加入N,N-二甲基甲酰胺稀释至刻度,混匀(每毫升相当于1,3-丁二烯
2μg、4μg、6μg、8μg、10μg),使用当天配制。
3.4 n-戊烷标准溶液配制
按照与3.3相似的过程用N,N-二甲基甲酰胺配制一份浓度约为10μg/mL的n-戊烷标准溶液。
4 仪器和设备
4.1 气相色谱仪(带氢火焰检测器)。
4.2 顶空自动进样器。
4.3 20mL顶空气测定瓶,配有表层涂聚氟乙烯硅橡胶盖及铝帽。
4.4 分析天平:感量0.1mg。
4.5 10mL容量瓶。
4.6 100μL微量注射器。
5 分析步骤
5.1 试样制备
取食品接触材料10g,用粉碎机粉碎或用剪刀剪成粒径小于或等于0.2cm的碎片,混匀,装入洁净
的容器内。
5.2 试液制备
称取0.5g(精确至0.01g)样品装入顶空瓶中,加入5.0mLN,N-二甲基甲酰胺,立即加盖密封,用
100μL微量注射器在顶空瓶中加入100μLn-戊烷标准溶液,充分振摇,使瓶中试样完全溶解或充分分
散,待测,同时做空白试验。
5.3 仪器参考条件
5.3.1 顶空进样器条件
顶空进样器条件列出如下:
a) 平衡时间:30min;
b) 炉温:80℃;
c) 压力:138kPa;
d) 加压时间:2min;
e) 进样时间:0.04min。
5.3.2 气相色谱条件
气相色谱条件列出如下:
a) 色谱柱:聚苯乙烯-二乙烯基苯石英毛细管柱,柱长30m,内径0.32mm,膜厚10μm,或等
效柱;
b) 柱温度程序:80℃保持12min,10℃/min升至120℃保持10min;
c) 进样口温度:220℃;
d) 检测器温度:250℃;
e) 载气氮气流速:50mL/min;
f) 氢气流速:10mL/min;
g) 空气流速:400mL/min;
h) 进样口恒压进样:100kPa。
5.4 校准溶液配制与校准曲线制作
取5只顶空瓶分别加入100μLn-戊烷标准溶液,再依次加入1,3-丁二烯系列标准溶液,此时校准
溶液中的1,3-丁二烯含量分别相当于0.2μg、0.4μg、0.6μg、0.8μg、1.0μg。气相色谱调至最佳工作状
态,将装有标准系列的顶空瓶置于顶空进样器中,取液上气进气相色谱,进行测定,得到相应n-戊烷和
1,3-丁二烯色谱峰。以1,3-丁二烯含量为横坐标,1,3-丁二烯峰面积与n-戊烷峰面积的比值为纵坐标
绘制校准曲线。
1,3-丁二烯气相色谱图参见图A.1。
5.5 试样溶液的测定
气相色谱调至最佳工作状态,将装有待测试液的顶空瓶置于顶空进样器中,取液上气进气相色谱,
进行测定,得到相应1,3-丁二烯与n-戊烷的色谱峰,根据保留时间定性,根据试样中1,3-丁二烯与内标
物n-戊烷峰面积比值计算定量。
6 分析结果的表述
试样中1,3-丁二烯的含量按式(1)计算:
计算结果保留两位有效数字。
7 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10%。
8 其他
方法检出限为0.1mg/kg,定量限为0.2mg/kg。
1,3-丁二烯迁移量的测定
食品接触材料及制品采用食品模拟物浸泡,1,3-丁二烯迁移到浸泡液中,取一定量模拟物浸泡液加
入顶空瓶中,加热使待测成分达到气液平衡,然后定量吸取顶空气进行气相色谱测定。根据保留时间定
性,n-戊烷作为内标物,以内标法定量。
10 试剂和材料
本方法所用水为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。
10.1 试剂
10.1.1 N,N-二甲基甲酰胺(DMF):分析纯,在1,3-丁二烯和n-戊烷保留时间处无干扰峰。
10.1.2 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。
10.2 试剂配制
10.3 标准品
10.3.1 1,3-丁二烯(C4H6,CAS号:106-99-0):2000μg/mL,或经国家认证并授予标准物质证书的标
准物质。
10.3.2 n-戊烷(C5H12,CAS号:106-66-0):纯度大于99.5%,或经国家认证并授予标准物质证书的标
准物质。
10.4 1,3-丁二烯标准溶液配制
10.4.1 1,3-丁二烯标准贮备液:吸取1,3-丁二烯标准品1.0mL移入10mL容量瓶中,加入N,N-二
甲基甲酰胺稀释至刻度,混匀,此溶液中1,3-丁二烯浓度为200μg/mL,避光保存,于-20℃保存,有效
期3个月,或于4℃保存,有效期为一周。
分别移入10mL容量瓶中,各加入N,N-二甲基甲酰胺稀释至刻度,混匀(每毫升相当于1,3-丁二烯
2μg、4μg、6μg、8μg、10μg),使用当天配制。
10.5 n-戊烷标准溶液配制
按照与3.3相似的过程用N,N-二甲基甲酰胺配制一份浓度约为10μg/mL的n-戊烷标准溶液。
11 仪器和设备
11.1 气相色谱仪(带氢火焰检测器)。
11.2 顶空自动进样器。
11.3 20mL顶空气测定瓶,配有表层涂聚氟乙烯硅橡胶盖及铝帽。
11.4 涡旋振荡器。
11.6 10mL容量瓶。
11.7 50μL微量注射器。
12 分析步骤
12.1 试液制备
12.1.1 水基、酸性、酒精类、油基食品模拟物
本标准食品模拟试验采用水基、酸性、酒精类、油基食品模拟物,所需试液通过迁移试验获取,可在
4℃冰箱中避光保存1周。
12.1.2 迁移试验
按照GB 5009.156及GB 31604.1的要求,对样品进行迁移试验,得到食品模拟物试液。如果得到
物试液应冷却或恢复至室温后进行下一步试验。
12.1.3 浸泡液的处理
食品模拟物配制过程参照GB 5009.156用5mL移液器移取5.0mL食品模拟物装入顶空瓶中,准
确称量移入液体质量,立即加盖密封,用50μL微量注射器在顶空瓶中加入50μLN,N-二甲基甲酰胺
和50μLn-戊烷标准溶液,混合均匀,待测。同时做空白试验。
GB 31604.12-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Food contact materials and products -
Determination of 1,3-butadiene and migration
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and materials ... 4
4 Instruments and equipment ... 5
5 Analysis procedure ... 5
6 Expression of analysis results ... 7
7 Precision ... 7
8 Others ... 8
9 Principle ... 8
10 Reagents and materials ... 8
11 Instruments and equipment ... 9
12 Analysis procedure ... 9
13 Expression of analysis results ... 11
14 Precision ... 11
15 Others ... 12
Annex A 1,3-butadiene gas chromatogram ... 13
Foreword
This Standard replaces GB/T 23296.2-2009 “Food contact materials - Polymer -
Determination of 1,3-butadiene in food simulants - Gas chromatography” and GB/T
23296.3-2009 “Food contact materials - Determination of 1,3-butadiene in plastics -
Gas chromatography”.
Compare this Standard with GB/T 23296.3-2009, the main changes are as follows.
- The standard name is revised to “National food safety standard - Food contact
materials and products - Determination of 1,3-butadiene and migration”;
- ADD the determination of 1,3-butadiene migration in food contact materials.
National food safety standard -
Food contact materials and products -
Determination of 1,3-butadiene and migration
1 Scope
This Standard specifies the determination method for 1,3-butadiene in food contact
materials and products and the determination method for migration.
This Standard applies to the determination of 1,3-butadiene in food contact materials
and products and the determination of migration.
Determination of 1,3-butadiene
2 Principle
Food contact materials and products are dissolved or dispersed in the headspace
bottle with N, N-dimethylformamide. HEAT to bring the components to be determined
to gas-liquid equilibrium. The headspace gas is then quantitatively taken for
determination by gas chromatography. QUALIFY according to the retention time, using
n-pentane as the internal standard; QUANTIFY by internal standard method.
3 Reagents and materials
The water used in this method is Grade I water specified in GB/T 6682. Containers
and transfer apparatus in the test shall avoid the use of plastic materials.
3.1 Reagents
N, N-Dimethylformamide (DMF). Analytical grade, with no interference peak at 1,3-
butadiene and n-pentane retention times.
3.2 Standards
3.2.1 1,3-butadiene (C4H6, CAS number. 106-99-0). 2000 μg/mL, or standard
substances certified by the state and awarded the standard substance certification.
3.2.2 n-pentane (C5H12, CAS number. 106-66-0). with the purity greater than 99.5 %,
or standard substances certified by the state and awarded the standard substance
WEIGH 0.5 g (to the nearest 0.01 g) of sample into a headspace bottle; ADD 5.0 mL
of N, N-dimethylformamide; immediately COVER to seal; USE a 100 μL micro syringe
to ADD 100 μL of n-pentane standard solution to the headspace bottle; SHAKE well,
so that the sample in the bottle is completely dissolved or fully dispersed for
determination. At the same time, carry out the blank test.
5.3 Instrument reference conditions
Headspace sample injector conditions are listed below.
a) balance time. 30 min;
b) furnace temperature. 80 °C;
c) pressure. 138 kPa;
d) pressurizing time. 2 min;
e) sample injection time. 0.04 min;
f) transmission line temperature. 85 °C.
5.3.2 Gas chromatographic conditions
Gas chromatographic conditions are listed below.
with column length of 30 m, inner diameter of 0.32 mm, membrane thickness of
10 μm, or equivalent column;
b) column temperature program. maintain at 80 °C for 12 min, rise to 120 °C at a
rate of 10 °C/min and maintain for 10 min;
c) inlet temperature. 220 °C;
d) detector temperature. 250 °C.
e) carrier gas nitrogen flow rate. 50 mL/min;
f) hydrogen flow rate. 10 mL/min;
g) air flow rate. 400 mL/min;
5.4 Preparation of calibration solution and plotting of calibration curve
10.4.1 1,3-butadiene standard stock solution. PIPETTE 1.0 mL of 1,3-butadiene
standard and TRANSFER into a 10 mL volumetric flask; ADD N, N-dimethylformamide
to DILUTE to the mark, MIX. The concentration of 1,3-butadiene in this solution is 200
μg/mL. The solution shall be stored in the dark, which is valid for 3 months at -20 °C,
or valid for one week at 4 °C.
10.4.2 1, 3-butadiene standard use solution. PIPETTE 0.1 mL, 0.2 mL, 0.3 mL, 0.4 mL,
0.5 mL of 1, 3-butadiene standard stock solution; TRANSFER into 10 mL volumetric
flasks, respectively. ADD N, N-dimethylformamide respectively to DILUTE to the mark,
Prepare at the day when it is to be used.
10.5 Preparation of n-pentane standard solution
Following the procedure similar to that of 3.3, use N, N-dimethylformamide to prepare
a portion of n-pentane standard solution at a concentration of about 10 μg/mL.
11 Instruments and equipment
11.1 Gas chromatograph (with hydrogen flame detector).
11.2 Headspace auto sample injector.
11.3 20 mL headspace gas measuring bottle, with fluorinated vinyl silicone coated
rubber cap and aluminum cap.
11.5 Analytical balance. with a division of 0.1 mg.
11.6 10 mL volumetric flask.
11.7 50 μL micro syringe.
12 Analysis procedure
12.1 Preparation of sample solution
12.1.1 Water-based, acidic, alcohol-based, oil-based food simulants
In this Standard, the food simulation test uses water-based, acidic, alcohol-based, oil-
based food simulants. The required sample solutions are obtained by the migration
test, which may be stored in the refrigerator at 4 °C keeping away from light for 1 week.
e) carrier gas nitrogen flow rate. 50 mL/min;
f) hydrogen flow rate. 10 mL/min;
g) air flow rate. 400 mL/min;
h) inlet constant-pressure injection. 100 kPa.
12.3 Preparation of calibration solution and plotting of calibration curve
ADD 1,3-butadiene-free food simulants in 5 headspace bottles respectively according
to the sample solution preparation procedure of 12.1.3; ADD 50 μL of 1,3-butadiene
series standard solution instead of adding 50 μL of N, N-dimethylformamide in 12.1.3,
at this point the 1,3-butadiene content in the calibration solutions is corresponding to
headspace gas to gas chromatograph, and calculate the ratio of the peak area of 1,3-
butadiene to the peak area of n-pentane. The calibration curve is plotted with the
content of 1,3-butadiene as abscissa and the ratio of peak area of 1,3-butadiene to
peak area of n-pentane as ordinate. QUANTIFY according to the ratio of the peak area
of 1,3-butadiene in the sample and the peak area of n-pentane in the internal standard.
1,3-butadiene gas chromatogram is shown in Figure A.1.
12.4 Determination of sample solution
ADJUST the gas chromatogram to the best working condition; PLACE the headspace
bottles containing sample solutions to be determined in the headspace sample injector;
corresponding n-pentane and 1,3-butadiene peak. QUALIFY according to the retention
time, and MEASURE the corresponding peak area.
13 Expression of analysis results
The content of 1,3-butadiene in the sample solution is obtained from t...
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