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食品安全国家标准 食品接触材料及制品 邻苯二甲酸酯的测定和迁移量的测定
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GB 31604.30-2016
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标准编号: GB 31604.30-2016 (GB31604.30-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 邻苯二甲酸酯的测定和迁移量的测定
英文名称: Determination of phthalate esters in food plastic packaging materials
行业: 国家标准
中标分类: X09
字数估计: 12,171
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2037-2007; GB/T 21928-2008
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.30-2016: 食品安全国家标准 食品接触材料及制品 邻苯二甲酸酯的测定和迁移量的测定
GB 31604.30-2016 英文名称: Determination of phthalate esters in food plastic packaging materials
1 范围
本标准规定了食品接触材料及制品中邻苯二甲酸酯的测定和迁移量的测定方法。
本标准适用于食品塑料包装材料及制品中邻苯二甲酸酯类物质的测定以及食品接触材料及制品中
邻苯二甲酸酯类物质迁移量的测定。
邻苯二甲酸酯的测定
2 原理
食品塑料包装材料及制品经粉碎后,用正己烷超声提取,提取液经过滤后,采用气相色谱-质谱联用
法测定。采用特征选择离子监测扫描模式(SIM),以保留时间和碎片的丰度比定性,外标法定量。
3 试剂和材料
除非另有说明,本方法所用试剂均为色谱纯(或分析纯再进行重蒸馏)。水为采用全玻璃装置进行
重蒸馏的水,且储存于玻璃容器中。
3.1 试剂
3.1.1 正己烷(C6H14)。
3.1.2 丙酮(CH3COCH3)。
3.2 邻苯二甲酸酯标准品
邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二烯丙酯(DAP)、邻苯二甲酸二
异丁酯(DIBP)、邻苯二甲酸二正丁酯(DBP)、邻苯二甲酸二(2-甲氧基)乙酯(DMEP)、邻苯二甲酸二
(4-甲基-2-戊基)酯(BMPP)、邻苯二甲酸二(2-乙氧基)乙酯(DEEP)、邻苯二甲酸二戊酯(DPP)、邻苯二
甲酸二己酯(DHXP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二(2-丁氧基)乙酯(DBEP)、邻苯二甲
酸二环己酯(DCHP)、邻苯二甲酸二(2-乙基)己酯(DEHP)、邻苯二甲酸二苯酯(DPhP)、邻苯二甲酸二
正辛酯(DNOP)、邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二壬酯(DNP):纯度 >95.0%。
3.3 标准溶液的配制
3.3.1 18种邻苯二甲酸酯标准储备液(1000μg/mL):分别准确称取18种邻苯二甲酸酯标准品
25mg,用正己烷溶解并准确定容至25mL,于4℃冰箱中避光保存。
3.3.2 17种邻苯二甲酸酯标准使用液(10μg/mL):准确移取除邻苯二甲酸二异壬酯外17种邻苯二甲
酸酯标准储备液(1000μg/mL)1mL至100mL容量瓶中,加入正己烷定容至100mL,于4℃冰箱中
避光保存。
3.3.3 邻苯二甲酸二异壬酯标准使用液(100μg/mL):准确移取邻苯二甲酸二异壬酯标准储备液
(1000μg/mL)10mL至100mL容量瓶中,加入正己烷定容至100mL,于4℃冰箱中避光保存。
3.3.4 邻苯二甲酸酯系列标准工作溶液:准确移取适量邻苯二甲酸酯标准使用液,用正己烷配制浓度
为0.02mg/L、0.05mg/L、0.10mg/L、0.20mg/L、0.50mg/L、1.00mg/L的17种邻苯二甲酸酯类物质
的混合标准使用液和浓度为0.5mg/L、1.0mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20.0mg/L的邻苯
二甲酸二异壬酯(DINP)单标使用液。
4 仪器和设备
4.1 气相色谱-质谱联用仪(GC-MS)。
4.2 分析天平:感量0.0001g和0.01g。
4.3 超声波发生器。
4.4 玻璃器皿。
注:所用玻璃器皿洗净后,用重蒸水淋洗3次,丙酮浸泡1h,在200℃ 下烘烤2h,冷却至室温备用。
5 分析步骤
5.1 试样制备
取5g典型样品,将试样(不含保鲜膜)剪碎至单个碎片直径≤0.2cm,保鲜膜碎片直径≤0.3cm,混
合均匀,准确称取0.2g~0.5g试样(精确至0.0001g)于具塞三角瓶中,加入20mL正己烷,超声提取
30min后过滤,残渣再用20mL正己烷重复提取1次,合并滤液于50mL容量瓶中,用正己烷定容至刻
度,再视试样中邻苯二甲酸酯含量作相应的稀释,混匀后过0.45μm有机相玻璃滤膜,进气相色谱-质谱
仪分析。
5.2 空白试验
试验中使用的试剂按5.1处理,进行GC-MS分析。
5.3 仪器参考条件
5.3.1 气相色谱参考条件
a) 色谱柱:5%苯基-甲基聚硅氧烷石英毛细管柱或性能类似的分析柱,规格为:柱长30.0m,内径
0.25mm,膜厚0.25μm;
b) 进样口温度:260℃;
c) 升温程序:初始柱温60℃,保持1min,以20℃/min升温至220℃,保持1min,再以5℃/min
升温至250℃,保持1min,再以20℃/min升温至290℃,保持7.5min;
d) 载气:氦气(纯度 >99.999%),流速:1mL/min;
e) 进样方式:不分流进样;
f) 进样量:1μL。
5.3.2 质谱参考条件
a) 色谱与质谱接口温度:280℃;
b) 离子源温度:230℃;
c) 电离方式:电子轰击电离源(EI);
d) 监测方式:选择离子扫描模式(SIM),监测离子参见附录B;
e) 电离能量:70eV;
f) 溶剂延迟:7min。
5.4 标准曲线的制作
将系列标准工作液分别注入气相色谱-质谱仪中,测定相应的邻苯二甲酸酯化合物的定量离子的峰
面积,以标准工作液的浓度为横坐标,以各邻苯二甲酸酯化合物的定量离子的峰面积为纵坐标,绘制标
准曲线。
5.5 试样溶液的测定
将试样溶液注入气相色谱-质谱仪中,得到各邻苯二甲酸酯化合物的定量离子的峰面积,根据标准
曲线得到待测液中各邻苯二甲酸酯化合物的浓度。
5.6 定性
试样待测液和标准品的选择离子在相同保留时间处(±0.5%)出现,并且对应质谱碎片离子的质荷
比与标准品一致,其丰度比与标准品相比应符合表1,可定性确证目标分析物。各邻苯二甲酸酯类化合
物的保留时间、定性离子和定量离子见附录B。各邻苯二甲酸酯类化合物标准物质的气相色谱-质谱选
择离子色谱图见附录C。
GB 31604.30-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard – Food Contact
Materials and Articles – Determination of the Content
and Migration of Phthalate Esters
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of PRC
Table of Contents
Foreword ... 4
1 Scope ... 5
2 Principle ... 5
3 Reagents and Materials ... 5
4 Apparatus ... 6
5 Analytical Procedures ... 7
6 Expression of Analytical Results ... 8
7 Precision ... 9
8 Others ... 9
9 Principle ... 9
10 Reagents and Materials ... 10
11 Apparatus ... 10
12 Analytical Procedures ... 11
13 Expression of Analytical Results ... 12
14 Precision ... 13
15 Others ... 13
Appendix A Information on 18 kinds of Commonly Used Phthalate Ester
Plasticizers ... 14
Appendix B Quantitative and Qualitative Selective Ion List of Phthalate Ester
Compounds ... 15
Appendix C Gas Chromatography – Mass Spectrometry Total Ion
Chromatogram of Phthalate Ester Standard Sample Solution ... 16
National Food Safety Standard – Food Contact
Materials and Articles – Determination of the Content
and Migration of Phthalate Esters
1 Scope
This Standard specifies the determination of the content and migration of phthalate
esters in the food contact materials and articles.
This Standard is applicable to the determination of the content of phthalate esters in
the food plastic packaging materials, and the determination of migration of phthalate
esters in food contact materials and articles.
Determination of Phthalate Esters
2 Principle
After crushing the food plastic packaging materials and articles, use n-hexane to
conduct the ultrasonic extraction; after filtering the extracting solution, use gas
chromatography-mass spectrometry to determine. Adopt the feature selective ion
monitoring scan mode (SIM), so that retain the qualitative of abundance ratio of the
time and fragments; use external standard method to quantify.
3 Reagents and Materials
Unless otherwise is specified, the reagents used in this Method are all
chromatographic pure (or analytically pure that has been redistilled). Water shall be
the one redistilled by a full glass device and stored in the glass vessel.
3.1 Reagents
3.1.1 N-hexane (C6H14).
3.12 Acetone (CH3COCH3).
3.2 Standard substance of phthalate esters
5 Analytical Procedures
5.1 Specimen preparation
Take 5g of typical sample; shear the specimen (excluding the preservative film) into
single pieces with diameter≤0.2cm; the preservative film piece diameter≤0.3cm; then
mix evenly; accurately take 0.2g~0.5g of specimen (accurate to 0.0001g) into
stoppered triangular flask; add 20mL of n-hexane; perform ultrasonic extraction for
30min and filter; after than the residue is re-extracted once by 20mL of n-hexane;
combine the filtrate into 50mL volumetric flask; use n-hexane to make constant volume
to the scale; then dilute it as per the content of phthalate esters in the specimen; after
mixing evenly, pass through a 0.45µm organic phase glass filter film; and be analyzed
in the gas chromatograph-mass spectrometer.
5.2 Blank test
The reagents used in the test shall be treated as per 5.1; and analyzed in GC-MS.
5.3.1 Gas chromatography reference conditions
a) Chromatographic column. 5% polyphenylmethylsiloxane quartz capillary column
or analytical column with similar performance; the specification indicates column
length of 30.0m, inner diameter of 0.25mm, film thickness of 0.25µm;
b) Sample inlet temperature. 260°C;
c) Temperature rise program. maintain the initial column temperature of 60°C for
1min; raise temperature to 220°C by 20°C/min, maintain for 1min; raise
temperature to 250°C by 5°C/min, maintain for 1min; then raise temperature to
290°C by 20°C/min, maintain for 7.5min;
e) Sampling injecting method. splitless sample injection;
f) Sample injecting volume. 1µL.
5.3.2 Mass spectrometry reference conditions
a) Gas chromatography and mass spectrometry interface temperature. 280°C;
b) Ion source temperature. 230°C;
c) Ionization mode. electron impact ionization source (EI);
10 Reagents and Materials
Unless otherwise is specified, the reagents used in this Method are all
chromatographic pure (or analytically pure that has been redistilled). Water shall be
10.1 Reagents
10.1.1 N-hexane (C6H14).
10.1.2 Absolute alcohol (C2H5OH).
10.1.3 Acetic acid (CH3COOH).
10.1.4 Reagents required for preparing the acidic and alcoholic food simulants. abide
by the provisions of GB 31604.1.
10.1.5 Isooctane. oil-based food simulants.
10.2 Standard substance
The standard substance for 18 kinds of phthalate esters, the same as 3.2.
10.3.1 Standard stock solution. the same as 3.3.1.
10.3.2 17 kinds of phthalate esters standard use solutions. the same as 3.3.2.
10.3.3 Diisononyl ortho-phthalate standard use solution. the same as 3.3.3.
10.3.4 Phthalate ester standard serial working solution. accurately pipette
appropriate amount of phthalate ester standard use solution; use n-hexane to prepare
17 kinds of phthalate ester mixing standard use solutions with concentrations of
0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 3.0mg/L, 8.0mg/L, 10.0mg/L, as well as single-
labeled diisononyl ortho-phthalate (DINP) with concentrations of 0.5mg/L, 1.0mg/L,
3.0mg/L, 8.0mg/L, 10.0mg/L for later-use.
11.1 Gas chromatography-mass spectrometer. with electron impact source (EI).
11.2 Centrifuge.
11.3 Oscillator.
11.4 Solid phase extraction device.
11.5 Constant temperature oven.
11.6 Low-temperature incubator.
11.7 Centrifuge tube. 10mL.
11.8 Volumetric flask. 10mL.
11.9 Glassware.
acetone for 1h; bake at 200°C for 2h; cool off to the room temperature for later-use.
12 Analytical Procedures
12.1 Preparation of food simulant test solution
According to the requirements of GB 5009.156 and GB 31604.1, perform the migration
test against the sample; then obtain the food simulant test solution.
12.2 Treatment of soaking solution
Place the soaking solution at the room temperature; for the isooctane and 95% ethanol
aqueous solution (≥ 50% alcoholic food) simulant soaking solution, accurately take
10g±0.01g of soaking solution into the pear-shaped distillation flask; reduce pressure
dissolve; perform vortex oscillation for 3min; centrifuge for 5min at 4000r/min; collect
the supernatant for the instrument test.
For other simulant soaking solutions (including water-based, acidic food, < 50%
alcoholic food simulant), take 10g±0.01g of simulant soaking solution into 25mL
centrifuge tube; add 4mL of n-hexane; shake and extract for 10min; centrifuge for 5min
at 4000r/min speed; take out the upper layer of n-hexane; repeatedly extract twice;
combine the n-hexane phase into pear-shaped distillation flask; reduce pressure in
45°C water bath; perform rotary evaporation to dryness; add 1mL of n-hexane to
dissolve; perform vortex oscillation for 3min; centrifuge for 5min at 4000r/min; collect
The sample solution can be diluted as per the specific conditions, so that the measured
value shall be within the linear range of the standard curve.
12.3 Blank test
The reagents used in the test shall be treated as per 12.2; perform the GC-MS analysis.
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