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食品安全国家标准 食品接触材料及制品 乙二醇和二甘醇迁移量的测定
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GB 31604.44-2016
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标准编号: GB 31604.44-2016 (GB31604.44-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 乙二醇和二甘醇迁移量的测定
英文名称: Food contact materials -- Polymer -- Determination of monoethylene glycol and diethylene glycol in food simulants -- Gas chromatography
行业: 国家标准
中标分类: X09
字数估计: 8,815
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): GB/T 23296.18-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.44-2016: 食品安全国家标准 食品接触材料及制品 乙二醇和二甘醇迁移量的测定
GB 31604.44-2016 英文名称: Food contact materials -- Polymer -- Determination of monoethylene glycol and diethylene glycol in food simulants -- Gas chromatography
1 范围
本标准规定了食品接触材料及制品中乙二醇和二甘醇迁移量的气相色谱测定方法。
本标准适用于食品接触材料及制品中乙二醇和二甘醇迁移量的测定。
2 原理
对食品容器、包装材料模拟物中乙二醇和二甘醇采用毛细管气相色谱柱进行分离,氢火焰离子化检
测器进行检测。其中水基、酸性、酒精类食品模拟物直接进样分析,油基食品模拟物通过水萃取后进样分析,采用内标法定量,内标物为1,4-丁二醇。
3 试剂和材料
除非另有说明,所有试剂均为分析纯,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 冰乙酸(C2H4O2)。
3.1.2 无水乙醇(C2H6O)。
3.1.3 甲醇(CH4O)。
3.1.4 庚烷(C7H16)。
3.1.5 配制水基、酸性、酒精类、油基食品模拟物所需试剂:符合GB 31604.1的规定。
3.2 试剂配制
水基、酸性、酒精类、油基食品模拟物:按GB 5009.156的规定操作。
3.3 标准品
3.3.1 乙二醇(C2H6O2,CAS号:107-21-1)。
3.3.2 二甘醇(C4H10O3,CAS号:111-46-6)。
3.3.3 1,4-丁二醇(C4H10O2,CAS号:110-63-4)。
3.4 标准溶液配制
3.4.1 乙二醇(7500mg/L)和二甘醇(7500mg/L)储备液:分别准确称取乙二醇和二甘醇各0.75g于
两个烧杯中(精确至0.1mg),用甲醇溶解后分别转入100mL容量瓶中,用甲醇定容。此溶液于0℃~
4℃密封避光保存1个月。
3.4.2 1,4-丁二醇(10000mg/L)储备液:准确称取1g1,4-丁二醇于烧杯中(精确至0.1mg),用甲醇
溶解后转入100mL容量瓶中,用甲醇定容。此溶液于0℃~4℃密封避光保存1个月。
3.4.3 1,4-丁二醇(800mg/L)溶液:准确吸取2mL的1,4-丁二醇(10000mg/L)储备液于25mL容
量瓶中,用甲醇定容。此溶液于0℃~4℃密封避光保存,该溶液现用现配。
3.4.4 标准中间溶液:准确吸取2mL的1,4-丁二醇(10000mg/L)储备液于6个25mL容量瓶中,分
别加入0.0mL、0.5mL、1.0mL、2.5mL、5.0mL、10.0mL乙二醇和二甘醇储备液,用甲醇定容,得到乙
二醇和二甘醇浓度均为0.0mg/L、150.0mg/L、300.0mg/L、750.0mg/L、1500mg/L、3000mg/L的
标准中间溶液,1,4-丁二醇浓度为800mg/L。此溶液于0℃~4℃密封避光保存,该溶液现用现配。
4 仪器和设备
4.1 气相色谱仪:配氢火焰离子化检测器和数据自动分析软件。
4.2 分析天平:感量0.0001g和0.01g,以及0.1g。
4.3 分液漏斗:250mL,配聚四氟乙烯或玻璃瓶塞,使用前应干燥。
4.4 容量瓶:25mL和50mL,以及100mL。
4.5 带刻度移液管:1mL和2mL。
4.6 玻璃注射器:50mL。
4.7 过滤器:0.22μm有机相滤膜,针式。
5 分析步骤
5.1 标准工作溶液及试样制备
5.1.1 标准工作溶液的制备
5.1.1.1 水基、酸性、酒精类食品模拟物标准工作溶液
分别准确吸取各浓度标准中间溶液1mL于6个50mL容量瓶中,用水定容,得到水中乙二醇和二
甘醇浓度均为0.0mg/L、3.0mg/L、6.0mg/L、15.0mg/L、30.0mg/L、60.0mg/L的标准工作溶液。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乙二醇和二甘醇标准工作溶液。
5.1.1.2 油基食品模拟物标准工作溶液
分别准确称取50g(精确至0.1g)油基食品模拟物至6个250mL分液漏斗中,依次加入各浓度标
准中间溶液1mL,混合均匀,得到油基食品模拟物中乙二醇和二甘醇浓度分别为0.0mg/kg、3.0mg/kg、
6.0mg/kg、15.0mg/kg、30.0mg/kg、60.0mg/kg。在每个分液漏斗中加入50mL庚烷,充分混合,加
入水振荡萃取1min,静置5min,使两相分层;收集下层水相;再次用20mL水萃取油基食品模拟物;将
两次萃取水相合并,用水定容至50mL;取1mL定容液通过0.2μm滤膜过滤后供测定用。
5.1.2 食品模拟物试液的制备
5.1.2.1 总则
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
验条件进行操作。迁移试验结束后,将迁移试验所得模拟物充分混匀后,取部分用于分析。
迁移试验获取的模拟物,可在0℃~4℃冰箱中避光保存一周。
5.1.2.2 水基、酸性、酒精类食品模拟物
在50mL容量瓶中,准确移取1mL的1,4-丁二醇(800mg/L)溶液,加入迁移试验中获得的水基、
酸性、酒精类食品模拟物定容,混合均匀后取1mL过滤后供测定用。
5.1.2.3 油基食品模拟物
准确称取迁移试验中得到的油基食品模拟物50g(精确至0.1g)于250mL分液漏斗中,准确移取
1mL的1,4-丁二醇(800mg/L)溶液,加入50mL庚烷,充分混合,加入20mL水充分振荡萃取1min,
静置5min,使两相分层,收集下层水相;再次用20mL水充分萃取油基食品模拟物;将两次萃取水相合
并,用水定容至50mL;混合均匀后取1mL过滤后供测定用。
5.1.3 空白试液的制备
按照5.1.2的操作处理未与食品容器、包装材料接触的食品模拟物。
5.2 测定
5.2.1 仪器参考条件
a) 色谱柱:硝基对苯二酸修饰的聚乙二醇毛细管色谱柱,柱长30m,内径0.32mm,膜厚1μm,
或同等性能的色谱柱;
b) 柱温:100℃保持1min,以10℃/min升温至200℃,保持8min;
c) 载气:氮气,流速1mL/min;
d) 检测器温度:220℃;
e) 进样模式:不分流进样,0.5min后打开分流阀;
f) 进样口温度:220℃;
5.2.2 标准工作曲线的制作
对5.1.1中制备的标准工作溶液在所列仪器参数下进行检测,以乙二醇或二甘醇质量浓度为横坐
标,以乙二醇或二甘醇与内标物1,4-丁二醇色谱峰峰面积对应比值为纵坐标,绘制标准工作曲线,得到
线性方程。标准色谱图参见附录A。
5.2.3 定量测定
对食品模拟物试液和空白试液依次进样,分别得到乙二醇或二甘醇与内标物1,4-丁二醇色谱峰峰
面积对应比值;根据标准曲线得到试样溶液中乙二醇或二甘醇的含量,扣除空白值。
6 分析结果的表述
由标准曲线求得的试样溶液中乙二醇和二甘醇的浓度,按GB 5009.156进行迁移量的计算,得到食
7 重复性
在重复性条件下获得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
本方法对水基、酸性、酒精类食品模拟物中乙二醇或二甘醇的定量限为3mg/L。
本方法对油基食品模拟物中乙二醇或二甘醇的定量限为3mg/kg。
GB 31604.44-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard - Food contact materials
and articles - Determination of migration of ethylene
glycol and diethylene glycol
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
3. No action is required - Full-copy of this standard will be automatically &
immediately delivered to your EMAIL address in 0~60 minutes.
Table of Contents
Foreword ... 3
1 Scope .. 4
2 Principle ... 4
3 Reagents and materials .. 4
4 Apparatus ... 5
5 Analytical procedures ... 6
6 Expression of analytical results ... 8
7 Repeatability ... 8
8 Others ... 8
Annex A Chromatogram of ethylene glycol or diethylene glycol in the standard
working solutions of food simulants .. 9
Foreword
This Standard replaces GB/T 23296.18-2009, Food contact materials - Polymer -
Determination of monoethylene glycol and diethylene glycol in food simulants - Gas
chromatography.
Compared with GB/T 23296.18, the major changes of this Standard are as follows.
-- the standard name is changed into “National food safety standard - Food contact
materials and articles - Determination of migration of ethylene glycol and
diethylene glycol”;
-- the test types for food simulants are added.
National food safety standard - Food contact materials
and articles - Determination of migration of ethylene
glycol and diethylene glycol
1 Scope
This Standard specifies the gas chromatographic method for the determination of
migration of ethylene glycol and diethylene glycol in food contact materials and articles.
This Standard applies to the determination of migration of ethylene glycol and
diethylene glycol in food contact materials and articles.
2 Principle
Use the capillary gas chromatographic column to separate ethylene glycol and
diethylene glycol in food containers and packaging materials; and use the hydrogen
flame ionization detector for determination. Analyze sample directly for water-base,
acidic and alcoholic food simulants; analyze sample of oil-base food simulants after
water extraction; use the internal standard method for quantitation, with 1,4-butanediol
as the internal standard substance.
3 Reagents and materials
Unless specified otherwise, all reagents are analytically pure reagents and all water is
grade I water which is specified in GB/T 6682. Plastic material shall be avoided in the
production of the containers and transferring vessels in the test.
3.1 Reagents
3.1.1 Glacial acetic acid (C2H4O2).
3.1.2 Absolute ethyl alcohol (C2H6O).
3.1.3 Methyl alcohol (CH4O).
3.1.4 Normal heptane (C7H16).
3.1.5 Reagents required for the preparation of water-base, acidic, alcoholic and oil-
base food simulants. as specified in GB 31604.1.
3.2 Preparation of reagents
4.4 Volumetric flasks. 25 ml, 50 mL and 100 mL.
4.5 Graduated pipettes. 1 mL and 2 mL.
4.6 Glass injection syringe. 50 mL.
4.7 Filter. 0.22 μm organic phase filter membrane, needle type.
5 Analytical procedures
5.1 Preparation of standard working solutions and samples
5.1.1 Preparation of standard working solutions
5.1.1.1 Standard working solutions of water-base, acidic and alcoholic food simulants
Accurately absorb 1 mL of standard intermediate solutions of all concentrations
then obtain the standard working solutions of the concentrations of ethylene glycol and
diethylene glycol in water 0.0 mg/L, 3.0 mg/L, 6.0 mg/L, 15.0 mg/L, 30.0 mg/L and 60.0
mg/L. Use the same method and use the corresponding water-base, acidic and
alcoholic food simulants to prepare the same concentration series of standard working
solutions of ethylene glycol and diethylene glycol.
5.1.1.2 Standard working solutions of oil-base food simulants
Accurately weigh 50 g (accurate to 0.1 g) of oil-base food simulants to pour into six
250 mL separating funnels; add in succession 1 mL of the standard intermediate
solutions of all concentrations; mix up; and obtain the oil-base food simulants of the
15.0 mg/L, 30.0 mg/L and 60.0 mg/L. Add 50 mL of heptane to every separating funnel;
mix up; add water for oscillation extraction for 1 min; allow to stand for 5 min; and
separate two phases into layers. Collect the lower water phase. And use 20 mL of
water to extract oil-base food simulants once again. Combine the water for the two
extractions; and add water dropwise to 50 mL. Take 1 mL of the solution to pass
through a 0.2 μm filter membrane before using it for the determination.
5.1.2 Preparation of food simulants’ test solution
5.1.2.1 General
In accordance with the intended use and working conditions of samples to be tested,
specified in GB 5009.156 and GB 31604.1. After the migration test, mix up all the
simulants which are obtained in the migration test and take part for the analysis.
The simulants obtained from the migration test may be stored in a refrigerator in a dark
Measure the standard working solutions prepared in 5.1.1 under the listed instrument
parameters; plot the standard working curve, using the mass concentration of ethylene
glycol or diethylene glycol as the abscissa, and using the corresponding ratio of the
chromatographic peak area of ethylene glycol or diethylene glycol to that of the internal
standard substance 1,4-butanediol; and obtain the linear equation. For the standard
chromatogram see Annex A.
Inject samples of food simulants’ test solutions and blank solutions in succession; and
obtain respectively the corresponding ratios of the chromatographic peak area of
ethylene glycol or diethylene glycol to that of the internal standard substance 1,4-
butanediol. Obtain the contents of ethylene glycol or diethylene glycol in the sample
solutions in accordance with the standard curve, deducting the blank values.
6 Expression of analytical results
In accordance with the concentrations of ethylene glycol and diethylene glycol in the
sample solutions which are obtained from the standard curve, calculate the migration
volume as specified in GB 5009.156; and obtain the migrations of ethylene glycol and
the third decimal place.
7 Repeatability
The absolute difference between the results of two independent measurements under
repeatable conditions shall not exceed 10% of the arithmetic mean value.
8 Others
The limit of quantitation of this method for ethylene glycol or diethylene glycol in water-
base, acidic and alcoholic food simulants is 3 mg/L.
The limit of quantitation of this method for ethylene glycol or diethylene glycol in oil-
base food simulants is 3 mg/kg.
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