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食品安全国家标准 食品接触材料及制品 1-辛烯和四氢呋喃迁移量的测定
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GB 31604.14-2016
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标准编号: GB 31604.14-2016 (GB31604.14-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 1-辛烯和四氢呋喃迁移量的测定
英文名称: Food contact materials -- Polymer -- Determination of 1-octene and tetrahydrofuran in food simulants -- Gas chromatography
行业: 国家标准
中标分类: X09
字数估计: 12,110
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): GB/T 23296.4-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.14-2016: 食品安全国家标准 食品接触材料及制品 1-辛烯和四氢呋喃迁移量的测定
GB 31604.14-2016 英文名称: Food contact materials -- Polymer -- Determination of 1-octene and tetrahydrofuran 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-辛烯和四氢呋喃迁移量的测定方法。
本标准适用于食品接触材料及制品中1-辛烯和四氢呋喃迁移量的测定。
第一法 气相色谱法
2 原理
食品模拟物中1-辛烯、四氢呋喃经顶空进样后,在色谱柱中与内标物及其他组分分离,用氢火焰离
子化检测器检测,以内标法定量。
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。
3.1 试剂
3.1.1 N,N-二甲基乙酰胺(DMAC,C4H9NO):纯度 >99.0%。
3.1.2 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。
3.2 试剂配制
3.2.1 水基、酸性、酒精类、油基食品模拟物:按GB 5009.156操作。
3.3 标准品
3.3.1 1-辛烯(C8H16,CAS号:111-66-0),纯度≥99.5%,或经国家认证并授予标准物质证书的标准
物质。
3.3.2 异辛烷(C8H18,CAS号:540-84-1),纯度≥99.5%,或经国家认证并授予标准物质证书的标准
物质。
3.3.3 四氢呋喃(THF,C4H8O,CAS号:109-99-9),纯度≥98.0%,或经国家认证并授予标准物质证书
的标准物质。
3.3.4 四氢吡喃(THP,C5H10O,CAS号:142-68-7),纯度≥99.9%,或经国家认证并授予标准物质证书
的标准物质。
3.4 标准溶液配制
3.4.1 1-辛烯标准储备液(2mg/mL):量取45mLDMAC于50mL容量瓶中,带塞称量(精确至
0.0001g)。再加入1-辛烯100mg,约150μL,重新称量(精确至0.0001g)。用DMAC定容。精确计
算1-辛烯的浓度。于4℃避光保存,有效期3个月。
3.4.2 1-辛烯标准中间溶液(200μg/mL):准确移取1-辛烯标准储备液1.0mL于10mL容量瓶中,用
DMAC定容。保存条件同3.4.1。
3.4.3 1-辛烯水基、酸性、酒精类食品模拟物介质标准工作溶液:用移液管分别移取1.0mL水基、酸性、
酒精类食品模拟物于6个顶空瓶中,立即用隔垫和铝盖密封。用微量注射器透过隔垫依次加入200μL
异辛烷内标中间溶液,混匀。按附录A中表A.1用微量注射器透过隔垫向瓶中加入1-辛烯标准中间溶
液及DMAC,混匀。
3.4.4 1-辛烯橄榄油介质标准工作溶液:分别称取1g(精确至0.01g)橄榄油于6个顶空瓶中,立即用
隔垫和铝盖密封。用微量注射器透过隔垫依次加入200μL异辛烷内标中间溶液,混匀。按照附录A
中表A.1所列,向瓶中加入同样体积的1-辛烯标准中间溶液及DMAC,混匀。
3.4.5 异辛烷内标储备液(2mg/mL):量取45mLDMAC于50mL容量瓶中,带塞称量(精确至
0.001g)。再加入100mg异辛烷,约150μL,重新称量(精确至0.0001g),用DMAC定容。精确计算
异辛烷的浓度。保存条件同3.4.1。
3.4.6 异辛烷内标中间溶液(120μg/mL):移取3.0mL异辛烷内标储备液于50mL容量瓶中,用
DMAC定容。保存条件同3.4.1。
3.4.7 水基、酸性、酒精类THF标准储备液(2.2mg/mL):量取99mL水于100mL容量瓶中,带塞称
量(精确至0.0001g)。加入220mgTHF,约250μL,重新称重(精确至0.0001g),用水定容。精确计
算THF的浓度。于4℃避光保存,有效期1个星期。
3.4.8 水基、酸性、酒精类THF标准中间溶液(22μg/mL):量取90mL水于100mL容量瓶中,再移
入1.0mL水基THF标准储备液,用水定容。保存条件同3.4.7。
3.4.9 THF水基、酸性、酒精类食品模拟物介质标准工作溶液:分别量取45mL水基、酸性、酒精类食
品模拟物于6个50mL容量瓶中。按表A.2加入一定体积的水基、酸性、酒精类THF标准中间溶液,
用对应的食品模拟物定容。
准确移取上述溶液各10.0mL分别于6个顶空瓶中,立即用隔垫和铝盖密封。用微量注射器移取
100μL水基、酸性、酒精类THP内标中间溶液透过隔垫加入各顶空瓶中,混匀。
3.4.10 水基、酸性、酒精类THP内标储备液(1mg/mL):量取99mL水于100mL容量瓶中,带塞称
量(精确至0.0001g),加入100mgTHP,约150μL,重新称量(精确至0.0001g),用水定容。精确计
算THP的浓度。保存条件同3.4.7。
3.4.11 水基、酸性、酒精类THP内标中间溶液(70μg/mL):量取90mL水于100mL容量瓶中,再移
入7.0mL水基THP内标储备液,用水定容。保存条件同3.4.7。
3.4.12 油性THF标准储备液(1.0mg/mL):量取45mLDMAC于50mL容量瓶中,带塞称量 (精确
至0.0001g)。再加入50mgTHF,约60μL,重新称量(精确至0.0001g),用DMAC定容。精确计算
THF的浓度。保存条件同3.4.7。
3.4.13 油性THF标准中间溶液(50μg/mL):移取1.0mL油性THF标准储备液于20mL容量瓶中,
用DMAC定容。保存条件同3.4.7。
3.4.14 THF橄榄油介质标准工作溶液:分别称取10g(精确至0.01g)橄榄油于6个顶空瓶中,立即用
隔垫和铝盖密封。用微量注射器移取100μL油性THP内标中间溶液透过隔垫分别加入各顶空瓶中。
按表A.3所示,向每个顶空瓶中加入一定体积的油性THF标准中间溶液和DMAC,配制与表A.3所列
浓度相近的标准工作溶液。
3.4.15 油性THP内标储备液(1mg/mL):量取45mLDMAC于50mL容量瓶中,带塞称量(精确至
0.0001g)。再加入50mgTHP,约60μL重新称量(精确至0.0001g),用DMAC定容。精确计算
THP的浓度。保存条件同3.4.7。
3.4.16 油性THP内标中间溶液(75μg/mL):移取1.5mL油性THP内标储备液于20mL容量瓶中,
用DMAC定容。保存条件同3.4.7。
4 仪器和设备
4.1 气相色谱仪:配备自动顶空进样器和氢火焰离子化检测器(FID)。
4.2 顶空瓶:20mL,配备铝盖和丁基橡胶或硅树脂橡胶隔垫,隔垫接触样品一面应涂有聚四氟乙烯。
注:THF可用于制造内涂聚四氟乙烯的丁基橡胶隔垫,这将对THF的分析产生严重干扰。因此在试验前应对隔
垫进行净化处理,用蒸馏水至少煮沸15min,再晾干。已净化未使用的隔垫,下次使用时应再次净化。
4.3 容量瓶:10mL、25mL、50mL、100mL。
4.4 微量注射器:25μL、50μL、100μL、250μL、500μL。
4.5 移液管:1mL、2mL、3mL、5mL、10mL。
5 分析步骤
5.1 试样制备
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
的食品模拟物试液不能马上进行下一步试验,应将食品模拟物试液于0℃~4℃冰箱中避光保存。
应将所得食品模拟物试液冷却或恢复至室温后进行下一步试验。
5.2 试液制备
5.2.1 用于测定1-辛烯的水基、酸性、酒精类食品模拟物试液的制备
从迁移试验中移取1.0mL水基食品模拟物于顶空瓶中,立即用隔垫和铝盖密封。用微量注射器
透过隔垫依次加入200μL异辛烷内标中间溶液和200μLDMAC,混匀。
从迁移试验中称取1g(精确至0.01g)橄榄油介质食品模拟物至顶空瓶中,以下按5.2.1“立即用隔
垫和铝盖密封”的操作步骤进行处理。
5.2.3 用于测定四氢呋喃的水基、酸性、酒精类食品模拟物试液的制备
从迁移试验中移取10.0mL水基、酸性、酒精类食品模拟物于顶空瓶中,立即用隔垫和铝盖密封。
用微量注射器透过隔垫加入100μL水基、酸性、酒精类THP内标中间溶液,混匀。
5.2.4 用于测定四氢呋喃的橄榄油介质食品模拟物试液的制备
从迁移试验中称取10g(精确至0.01g)橄榄油介质食品模拟物于顶空瓶中,立即用隔垫和铝盖密
封。用微量注射器透过隔垫加入100μL油性THP内标中间溶液(3.4.16),再用微量注射器迅速加入
300μLDMAC,混匀。
按照5.2所述步骤处理没有与食品接触材料接触的食品模拟物。
GB 31604.14-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard –
Food contact materials and articles - Determination of
migration of 1-octene and tetrahydrofuran
食品接触材料及制品
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
Method I -- Gas chromatography . 4
2 Principle . 4
3 Reagents and materials .. 4
4 Apparatus . 7
5 Analytical procedures . 7
6 Expression of analysis results . 10
7 Precision . 10
8 Others .. 10
Method II -- Gas chromatography-mass spectrometry . 10
9 Principle . 10
10 Reagents and materials . 10
11 Apparatus . 10
12 Analytical procedures .. 11
13 Expression of analysis results . 13
14 Precision . 13
15 Others . 13
Annex A Preparation tables of standard working solutions . 14
Annex B Standard substance chromatograms of the gas chromatographic
method and the gas chromatographic-mass spectrometric method. 15
Foreword
This Standard replaces GB/T 23296.4-2009, Food contact materials - Polymer -
Determination of 1-octene and tetrahydrofuran in food simulants - Gas chromatography.
Compared with GB/T 23296.4-2009, 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 1-octene and
tetrahydrofuran”;
-- the gas chromatography-mass spectrometry is added;
-- the preparation of food simulant test solutions is changed;
-- the expression of analysis results is changed;
-- the detection limits and quantitation limits are changed.
National food safety standard –
Food contact materials and articles - Determination of
migration of 1-octene and tetrahydrofuran
1 Scope
This Standard specifies the method for the determination of migration of 1-octene and
tetrahydrofuran in food contact materials and articles.
This Standard applies to the determination of migration of 1-octene and
tetrahydrofuran in food contact materials and articles.
Method I -- Gas chromatography
2 Principle
1-octene and tetrahydrofuran in food simulants are separated from internal standard
substances and other components in a chromatographic column after headspace
sample injection; a hydrogen flame ionization detector is used for testing; and the
internal standard method is used for quantitation.
3 Reagents and materials
Unless indicated otherwise, all reagents used for this method are analytically pure and
the water is grade one water specified in GB/T 6682.
3.1 Reagents
3.1.1 N,N-Dimethylacetamide (DMAC, C4H9NO). of purity > 99.0%.
3.1.2 Water-based, acidic, alcoholic and oil-based food simulants. the reagents used
are as specified in GB 31604.1.
3.2 Reagent preparation
3.2.1 Water-based, acidic, alcoholic and oil-based food simulants. the operation is as
specified in GB 5009.156.
3.3 Standard substances
of isooctane internal standard stock solution to a 50 mL volumetric flask and use DMAC
to add to scale. The storage conditions are the same as those specified in 3.4.1.
3.4.7 Water-based, acidic and alcoholic THF standard stock solution (2.2 mg/mL).
measure 99 mL of water to pour into a 100 mL volumetric flask and weigh with the
stopper (accurate to 0.000 1 g). Add 220 mg of THF, about 250 μL; weigh once again
(accurate to 0.000 1 g); and use water to add to scale. Calculate the concentration of
THF accurately. Store in a dark place at 4°C, with a period of validity of one week.
3.4.8 Water-based, acidic and alcoholic THF standard intermediate solution (22
μg/mL). measure 90 mL of water to pour into a 100 mL volumetric flask; transfer 1.0
storage conditions are the same as those specified in 3.4.7.
3.4.9 Water-based, acidic based and alcoholic food simulant medium standard
working solution of THF. measure respectively 45 mL of water-based, acidic and
alcoholic food simulants to pour into six 50 mL volumetric flasks. Add a certain volume
of water-based, acidic and alcoholic THF standard intermediate solution in accordance
with Table A.2 and use corresponding food simulants to add to scale.
Accurately transfer 10.0 mL of the above-mentioned solutions to six headspace bottles
respectively and immediately seal using insulator and aluminium cover. Use a micro-
syringe to transfer 100 μL of water-based, acidic and alcoholic THP internal standard
3.4.10 Water-based, acidic based and alcoholic THP internal standard stock solution
(1 mg/mL). weigh 99 mL of water to pour into a 100 mL volumetric flask; weigh with the
stopper (accurate to 0.000 1 g); add 100 mg of THP, about 150 μL; weigh once again
(accurate to 0.000 1 g); and use water to add to scale. Accurately calculate the
concentration of THP. The storage conditions are the same as those specified in 3.4.7.
3.4.11 Water-based, acidic based and alcoholic THP internal standard intermediate
solution (70 μg/mL). measure 90 mL of water to pour into a 100 mL volumetric flask;
transfer 7.0 mL of water-based THP internal standard stock solution; and use water to
add to scale. The storage conditions are the same as those specified in 3.4.7.
to pour into a 50 mL volumetric flask and weigh with the stopper (accurate to 0.000 1
g). Then add 50 mg of THF, about 60 μL; weigh once again (accurate to 0.000 1 g);
and use DMAC to add to scale. Accurately calculate the concentration of THF. The
storage conditions are the same as those specified in 3.4.7.
3.4.13 Oil-based THF standard intermediate solution (50 μg/mL). transfer 1.0 mL of
oil-based THF standard stock solution to a 20 mL volumetric flask and use DMAC to
add to scale. The storage conditions are the same as those specified in 3.4.7.
In accordance with the requirements of GB 5009.156 and GB 31604.1, carry out
migration test for sample and obtain food simulant test solutions. If a food simulant test
at 0°C~4°C, which shall be kept out of the sun.
Cool or restore the food simulant test solutions to room temperature for further test.
5.2 Test solution preparation
5.2.1 Preparation of water-based, acidic and alcoholic food simulant test
solutions for the determination of 1-octylene
Transfer 1.0 mL of water-based food simulant from the migration test to a headspace
bottle, and immediately seal using insulator and aluminium cover. Use a micro-syringe
to add in turn 200 μL of isooctane internal standard intermediate solution and 200 μL
of DMAC through the insulator; and mix up.
determination of 1-octylene
Weigh 1 g (accurate to 0.01 g) of olive oil medium food simulant from the migration
test to place in a headspace bottle; and hereafter, process in accordance with the
operating procedures of 5.2.1 “and immediately seal using insulator and aluminium
cover .”.
5.2.3 Preparation of water-based, acidic and alcoholic food simulant test
solution for the determination of tetrahydrofuran
Transfer 10.0 mL of water-based, acidic and alcoholic food simulant test solution from
the migration test to a headspace bottle, and immediately seal using insulator and
alcoholic THP internal standard intermediate solution through the insulator; and mix
up.
5.2.4 Preparation of olive oil medium food simulant test solutions for the
determination of tetrahydrofuran
Weigh 10 g (accurate to 0.01 g) of olive oil medium food simulant from the migration
test to place into a headspace bottle, and immediately seal using insulator and
aluminium cover. Use a micro-syringe to add 100 μL of oil-based THP internal standard
intermediate solution (3.4.16) through the insulator; then use a micro-syringe to add
rapidly 300 μL of DMAC; and mix up.
Process the food simulants in accordance with the procedures specified in 5.2, which
are not in contact with food contact materials.
5.4 Determination
f) sampling method. split stream sampling with a split ratio of 10.1;
g) sample volume. 250 μL;
h) transmission line temperature. 250°C;
i) ionization mode. EI;
j) solvent delay. 2.2 min;
k) mass spectrum scanning method. selected ion mode (SIM), turning off filament
l) isooctane. quantitative ion m/z 57, qualitative ions m/z 58 and 99; 1-octene.
quantitative ion m/z 70, qualitative ions m/z 83 and 112; tetrahydrofuran.
quantitative ion m/z 72, qualitative ions m/z 71 and 73; tetrahydropyrane.
quantitative ion m/z 85, qualitative ions m/z 67 and 86.
12.4.2 Plotting of standard working curves
Carry out determination of standard working solutions in turn in accordance with the
determination conditions listed in 12.4.1. Plot standard working curves using the 1-
octene or tetrahydrofuran concentrations in standard working solutions as the abscissa,
in mg/L or mg/kg, and the peak area ratio of 1-octene/isooctane or
chromatogram of gas chromatography-mass spectrometry refer to Annex B.
12.4.3 Confirmation
Take test solutions (12.2) to carry out the confirmatory test of the internal standard
method in accordance with the gas chromatographic-mass spectrome...
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