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食品安全国家标准 食品接触材料及制品 对苯二甲酸迁移量的测定
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GB 31604.21-2016
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标准编号: GB 31604.21-2016 (GB31604.21-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 对苯二甲酸迁移量的测定
英文名称: Food contact materials -- Polymer -- Determination of terephthalic acid in food simulants -- High performance liquid chromatography
行业: 国家标准
中标分类: X09
字数估计: 10,192
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2184-2008; GB/T 23296.10-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.21-2016: 食品安全国家标准 食品接触材料及制品 对苯二甲酸迁移量的测定
GB 31604.21-2016 英文名称: Food contact materials -- Polymer -- Determination of terephthalic acid 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对苯二甲酸迁移量的测定方法。
本标准适用于食品接触材料及制品中对苯二甲酸迁移量的测定。
２ 原理
食品模拟物中的对苯二甲酸通过高效液相色谱进行分离，采用紫外检测器进行检测。水基、酸性、
酒精类食品模拟物直接进样测定，橄榄油介质食品模拟物通过稀碳酸氢钠溶液提取后进样测定。以邻
苯二甲酸作内标，采用内标法定量。
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 三水合乙酸钠（Ｃ２Ｈ３Ｏ２Ｎａ·３Ｈ２Ｏ）。
３．１．２ 碳酸氢钠（ＮａＨＣＯ３）。
３．１．３ 正庚烷（狀-Ｃ７Ｈ１６）。
３．１．４ 甲醇（ＣＨ３ＯＨ）：色谱纯。
３．１．５ 异丙醇（Ｃ３Ｈ８Ｏ）。
３．１．６ 磷酸（Ｈ３ＰＯ４）。
３．１．７ 冰乙酸（ＣＨ３ＣＯＯＨ）。
３．１．８ 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。
３．２．２ １ｇ／Ｌ碳酸氢钠水溶液：称取１ｇ（精确至０．１ｇ）碳酸氢钠，用水溶解并定容于１Ｌ容量瓶中。
３．２．３ 乙酸钠缓冲液（ｐＨ＝３．６）：称取２５．０ｇ三水合乙酸钠溶于３５０ｍＬ水中，加入５．０ｍＬ磷酸，用约
５０ｍＬ冰乙酸调节ｐＨ至３．６，加水定容至５００ｍＬ。
３．２．４ ５０％乙酸溶液：量取５０ｍＬ冰乙酸于１００ｍＬ容量瓶中，用水定容。
３．３ 标准品
３．３．１ 对苯二甲酸（Ｃ８Ｈ６Ｏ４，ＣＡＳ号：１００-２１-０），纯度≥９９％，或经国家认证并授予标准物质证书的标准物质。
GB ３１６０４．２１-２０１６
３．３．２ 邻苯二甲酸（Ｃ８Ｈ６Ｏ４，ＣＡＳ号：８８-９９-３），纯度≥９９％，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 对苯二甲酸标准储备溶液（５００ｍｇ／Ｌ）：准确称取５０ｍｇ（精确至０．１ｍｇ）对苯二甲酸标准品，加入９０ｍＬ甲醇使其溶解，将溶液加热至５０℃，持续１ｈ，使对苯二甲酸充分溶解。待溶液冷却后转移至１００ｍＬ容量瓶，用甲醇定容。有效期为６个月。
３．４．２ 对苯二甲酸标准中间溶液：分别于６只２５ｍＬ容量瓶中加入０ｍＬ、１．０ｍＬ、２．０ｍＬ、５．０ｍＬ、１０．０ｍＬ、２０．０ｍＬ对苯二甲酸标准储备溶液，再分别加入５ｍＬ邻苯二甲酸内标储备溶液，用甲醇定容。
对苯二甲酸标准中间溶液的浓度分别为０．０ｍｇ／Ｌ、２０ｍｇ／Ｌ、４０ｍｇ／Ｌ、１００ｍｇ／Ｌ、２００ｍｇ／Ｌ、４００ｍｇ／Ｌ。
３．４．３ 水基、酸性、酒精类食品模拟物介质标准工作溶液：分别移取２．０ｍＬ对苯二甲酸标准中间溶液于６个５０ｍＬ容量瓶中，用对应的食品模拟物定容。水基、酸性、酒精类食品模拟物中对苯二甲酸标准工作液浓度分别为０．０ｍｇ／Ｌ、０．８ｍｇ／Ｌ、１．６ｍｇ／Ｌ、４．０ｍｇ／Ｌ、８．０ｍｇ／Ｌ、１６．０ｍｇ／Ｌ；内标浓度均为８．０ｍｇ／Ｌ。
３．４．４ 橄榄油介质标准工作溶液：分别称取橄榄油５０ｇ于６个２５０ｍＬ分液漏斗中，准确移入２．０ｍＬ对苯二甲酸标准中间溶液，混合均匀后加入５０ｍＬ正庚烷，再混匀。再加入２０ｍＬ碳酸氢钠溶液，充分振荡１ｍｉｎ，静置１５ｍｉｎ分层。用１００ｍＬ烧杯收集下层水相，然后加入２０ｍＬ碳酸氢钠溶液重新提取上层油相。摇匀后静置，待两相分离后，用烧杯收集下层水相，合并两次水相提取溶液。用注射器或真空泵（流速１０ｍＬ／ｍｉｎ～２０ｍＬ／ｍｉｎ）使提取液通过固相萃取Ｃ１８柱。收集滤液于５０ｍＬ容量瓶中，加入１．０ｍＬ５０％乙酸溶液，用水定容。取１ｍＬ～２ｍＬ滤液用滤膜过滤。对苯二甲酸的标准工作液浓度分别为 ０．０ｍｇ／ｋｇ、０．８ｍｇ／ｋｇ、１．６ｍｇ／ｋｇ、４．０ｍｇ／ｋｇ、８．０ｍｇ／ｋｇ、１６．０ｍｇ／ｋｇ；内标浓度均为８．０ｍｇ／ｋｇ。
３．４．５ 邻苯二甲酸内标储备溶液（１０００ｍｇ／Ｌ）：准确称取０．１ｇ（精确至０．１ｍｇ）邻苯二甲酸标准品，用１０ｍＬ异丙醇溶解，然后将溶液转移至１００ｍＬ容量瓶中并以异丙醇定容。有效期为６个月。
３．４．６ 邻苯二甲酸内标中间溶液（２００ｍｇ／Ｌ）：取５ｍＬ邻苯二甲酸内标储备溶液于２５ｍＬ容量瓶中，用甲醇定容。
４ 仪器设备
４．１ 高效液相色谱仪：配紫外检测器和１０μＬ定量环。
４．２ 分析天平：感量０．１ｍｇ、０．１ｇ。
４．３ ｐＨ计。
４．４ 固相萃取Ｃ１８柱：十八烷基硅烷（ＯＤＳ）４００ｍｇ。
４．５ 水系微孔滤膜：０．４５μｍ。
５ 分析步骤
５．１ 样品迁移试验
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。
GB ３１６０４．２１-２０１６
５．２ 试液制备
５．２．１ 水基、酸性、酒精类食品模拟物试液的制备
移取５０．０ｍＬ从迁移试验中得到的水基食品模拟物于预先盛有２．０ｍＬ邻苯二甲酸内标中间溶液的１００ｍＬ锥形瓶中，混合均匀，取１ｍＬ～２ｍＬ用滤膜过滤待测。
５．２．２ 橄榄油模拟物试液的制备
称取５０．０ｇ从迁移试验中得到的橄榄油介质食品模拟物于２５０ｍＬ分液漏斗中，加入２．０ｍＬ内标中间溶液，混合均匀后量取５０ｍＬ的正庚烷于分液漏斗中。再按３．４．４“再加入２０ｍＬ碳酸氢钠溶液取１ｍＬ～２ｍＬ滤液用滤膜过滤”步骤操作，溶液待测。
５．３ 空白试液的制备
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。
５．４ 测定
５．４．１ 液相色谱测定参考条件
液相色谱测定参考条件列出如下：
ａ） 色谱柱：Ｃ１８柱，柱长２５０ｍｍ，内径４．６ｍｍ，粒径５μｍ，或相当者；ｂ） 流动相：Ａ：１５０ｍＬ乙酸钠缓冲液（３．２．５）＋７５０ｍＬ水；Ｂ：甲醇；
测定水基、酸性、酒精类模拟物试液时：流动相为Ａ＋Ｂ＝８０＋２０（体积比）；测定橄榄油模拟物试液时：流动相为Ａ＋Ｂ＝８５＋１５（体积比）；
ｃ） 流速：１．５ｍＬ／ｍｉｎ；
ｄ） 柱温：室温；
ｅ） 进样量：１０μＬ；ｆ） 紫外检测器：波长２４２ｎｍ。
５．４．２ 绘制标准工作曲线
按照５．４．１所列测定条件，对标准工作溶液依次进样测定。以标准工作溶液中对苯二甲酸浓度为
横坐标，单位以“ｍｇ／Ｌ或ｍｇ／ｋｇ”表示，以对苯二甲酸／邻苯二甲酸的峰面积比值为纵坐标，分别绘制标准工作曲线。标准溶液色谱图参见附录Ａ。
５．４．３ 试液测定
对空白溶液和食品模拟物试液依次进样，扣除空白值，得到对苯二甲酸／邻苯二甲酸的峰面积比值。
６ 分析结果的表述
由标准曲线得到试样溶液中对苯二甲酸的浓度，按GB ５００９．１５６进行迁移量计算，得到食品接触材料及制品中对苯二甲酸的迁移量。计算结果保留两位有效数字。
７ 确证
当上述结果超过特定迁移限量值（ＳＭＬ）时，用液相色谱-串联质谱法或其他有效方法确证。液相色谱-串联质谱法分析参考条件及色谱图参见附录Ｂ和附录Ｃ。
８ 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％。
９ 其他
水基、酸性、酒精类模拟物中对苯二甲酸的方法检出限为０．３ｍｇ／Ｌ；橄榄油模拟物中对苯二甲酸的方法检出限为０．３ｍｇ／ｋｇ。
水基、酸性、酒精类模拟物中对苯二甲酸的方法定量限为１．０ｍｇ／Ｌ；橄榄油模拟物中对苯二甲酸的方法定量限为１．０ｍｇ／ｋｇ。
GB 31604.21-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard –
Food contact materials and articles –
Determination of migration of terephthalic acid
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
2 Principle . 4
3 Reagents and materials .. 4
4 Apparatus . 6
5 Analytical procedures . 6
6 Expression of analysis results .. 8
7 Confirmation . 8
8 Precision . 8
9 Others . 8
Annex A Terephthalic acid standard substance chromatogram . 10
Annex B Liquid chromatography-tandem mass spectrometry confirmation
reference conditions . 11
Annex C Terephthalic acid multiple-reaction monitoring (MRM) chromatogram
. 13
Foreword
This Standard replaces GB/T 23296.10-2009, Food contact materials - Polymer -
Determination of terephthalic acid in food simulants - High performance liquid
chromatography, and SN/T 2184-2008, Food contact materials - Polymer materials -
Determination of terephthalic acid in food simulants - HPLC.
Compared with GB/T 23296.10-2009 and SN/T 2184-2008, 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 terephthalic acid”;
-- the preparation of food simulant test solution 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 terephthalic acid
1 Scope
This Standard specifies the method for the determination of migration of terephthalic
acid in food contact materials and articles.
This Standard applies to the determination of migration of terephthalic acid in food
contact materials and articles.
2 Principle
Terephthalic acid in food simulants is separated using high performance liquid
chromatograph and then tested using ultraviolet detector. The food simulants of water-
based, acidic and alcoholic types are sampled and tested directly; and the food
simulants of olive oil medium is extracted using diluted hydrochloric acid solution
before being sampled and tested. Phthalic acid is used as the internal standard 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 Sodium acetate trihydrate (C2H3O2Na·3H2O).
3.1.2 Sodium bicarbonate (NaHCO3).
3.1.3 Normal heptane (n-C7H16).
3.1.4 Methyl alcohol (CH3OH). chromatographically pure.
3.1.5 Isopropyl alcohol (C3H8O).
3.1.6 Phosphoric acid (H3PO4).
water-based, acidic and alcoholic food simulants are respectively 0.0 mg/L, 0.8 mg/L,
1.6 mg/L, 4.0 mg/L, 8.0 mg/L and 16.0 mg/L; and the internal standard concentrations
are all 8.0 mg/L.
3.4.4 Olive oil medium standard working solution. weigh respectively 50 g of olive oil
to pour in six 250 mL separating funnels; accurately transfer 2.0 mL of terephthalic acid
then mix up. Then add 20 mL of sodium bicarbonate solution; fully shake up for 1 min;
and allow to stand for layering. Use a 100 mL beaker to collect the lower layer water
phase; then add 20 mL of sodium bicarbonate solution to extract the upper layer oil
phase once again. Allow to stand after shaking up, use a beaker to collect the lower
layer water phase after two phases separates; and combine the two water-phase
extraction solutions. Use an injection syringe or vacuum pump (flow velocity 10
mL/min~20 mL/min) to make the extraction solution pass through the solid-phase
extraction C18 column. Collect the filtrate in a 50 mL volumetric flask; add 1.0 mL of 50%
acetic acid solution; and use water to add to scale. Take 1 mL~2 mL of the filtrate to
terephthalic acid are respectively 0 mg/kg, 0.8 mg/kg, 1.6 mg/kg, 4.0 mg/kg, 8.0 mg/kg
and 16.0 mg/kg; and the internal standard concentrations are all 8.0 mg/kg.
3.4.5 Phthalic acid internal standard stock solution (1 000 mg/L). accurately weigh
0.1 g (accurate to 0.1 mg) of phthalic acid standard substance; use 10 mL of isopropyl
alcohol to dissolve; and then transfer the solution to a 100 mL volumetric flask and add
isopropyl alcohol to scale. The period of validity is 6 months.
3.4.6 Terephthalic acid internal standard intermediate solution (200 mg/L). take 5 mL
of phthalic acid internal standard stock solution to pour into a 25 mL volumetric flask;
and use methyl alcohol to add to scale.
4.1 High performance liquid chromatograph. equipped with ultraviolet detector and
10 μL quantitative loops.
4.2 Analytical balance. of sensitivity 0.1 mg and 0.1 g.
4.3 pH meter.
4.4 Solid-phase extraction C18 column. octadecyl silane (ODS) 400 mg.
4.5 Hydrophilic microporous filter membrane. 0.45 μm.
5 Analytical procedures
5.1 Sample migration test
e) sample volume. 10 μL;
5.4.2 Plotting of standard working curves
Carry out determination of standard working solutions in turn in accordance with the
determination conditions listed in 5.4.1. Plot respectively standard working curves
using the terephthalic acid concentrations in standard working solutions as the
abscissa, in mg/L or mg/kg, and the peak area ratio of terephthalic acid/phthalic acid
as the ordinate. For the standard solution chromatograms refer to Annex A.
5.4.3 Test solution determination
Inject blank solutions and food simulant test solutions in turn, deducting blank values;
and obtain the peak area ratio of terephthalic acid/phthalic acid.
Obtain the terephthalic acid concentration of test solution from standard curves; and
calculate migration in accordance with GB 5009.156; and then obtain the migration of
terephthalic acid in food contact materials and articles. The calculation results are
rounded off to two significant digits.
7 Confirmation
When the above-mentioned results exceed specific migration limits, use the liquid
chromatography-tandem mass spectrometry or other effective methods for
confirmation. For the reference conditions for the liquid chromatography-tandem mass
spectrometry see Annex B and Annex C.
The absolute difference obtained from two independent determination results under
repeatable conditions shall not be 10% exceeding the arithmetic mean value.
9 Others
The detection limit for terephthalic acid in water-based, acidic and alcoholic simulants
is 0.3 mg/L; and the detection limit for terephthalic acid in olive oil simulants is 0.3
mg/kg.
The quantitation limit for terephthalic acid in water-based, acidic and alcoholic
simulants is 1.0 mg/L; and the quantitation limit for terephthalic acid in olive oil simulant
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