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食品安全国家标准 食品接触材料及制品 己二酸二（2－乙基）己酯的测定和迁移量的测定
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GB 31604.28-2016
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标准编号: GB 31604.28-2016 (GB31604.28-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 己二酸二（2－乙基）己酯的测定和迁移量的测定
英文名称: National Food Safety Standard -- Food contact materials and products -- Determination of di (2-ethylhexyl) adipate and migration
行业: 国家标准
中标分类: X09
字数估计: 10,137
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2826-2011部分; GB/T 20500-2006部分; GB/T 20499-2006
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.28-2016: 食品安全国家标准 食品接触材料及制品 己二酸二（2－乙基）己酯的测定和迁移量的测定
GB 31604.28-2016 英文名称: National Food Safety Standard -- Food contact materials and products -- Determination of di (2-ethylhexyl) adipate and migration
1 范围
本标准规定了食品接触材料及制品中己二酸二(2-乙基)己酯(DEHA)的测定方法与迁移量的测定
方法。
本标准适用于聚氯乙烯制品中己二酸二(2-乙基)己酯的测定及迁移量的测定。
己二酸二(2-乙基)己酯的测定
2 原理
用四氢呋喃溶解试样,加入甲醇沉淀其中的聚合物,过滤后,DEHA留在滤液中,采用气相色谱-质
谱仪测定,外标法定量。
3 试剂与材料
3.1 试剂
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。
3.1.1 四氢呋喃(C4H8O,CAS号:109-99-9)。
3.1.2 甲醇(CH4O,CAS号:67-56-1)。
3.1.3 正己烷(C6H12,CAS号:110-54-3):色谱纯。
3.2 标准品
己二酸二(2-乙基)己酯(C22H42O4,CAS号:103-23-1):纯度≥99.8%,或经国家认证并授予标准物
质证书的标准物质。
3.3 标准溶液配制
3.3.1 DEHA标准储备液
称取DEHA100mg(精确至0.0001g),用正己烷溶解后,定容至50mL,获得DEHA浓度为
2mg/mL的标准储备液。溶液在冰箱中储存,有效期为1个月。
3.3.2 DEHA标准中间溶液
用刻度吸量管吸取2.5mL的DEHA标准储备液(3.3.1)至50mL容量瓶中,用正己烷稀释至刻
度,获得DEHA标准中间溶液,其浓度为100.0mg/L。溶液储存方式同3.3.1。
3.3.3 DEHA标准工作溶液
分别用刻度吸量管及微量注射器吸取50μL、0.2mL、0.5mL、1.0mL、2.0mL、5.0mL的DEHA
标准中间溶液(3.3.2)置于6个10mL容量瓶中,用正己烷稀释、定容,充分摇匀,获得浓度分别为
0.5mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20.0mg/L、50.0mg/L的DEHA标准工作溶液。溶液储
存方式同3.3.1。
4 仪器与设备
4.1 气相色谱-质谱联用仪:配电子轰击离子源(EI)。
4.2 分析天平(精度为0.1mg)。
4.3 超声波清洗器。
4.4 氮吹仪。
4.5 微量注射器:100μL。
4.6 试管:50mL。
注:实验所用的玻璃器皿,都经过甲醇淋洗,通风晾干后待用。
5 分析步骤
5.1 试样处理
取样品,用剪刀裁成样片,混合均匀。
5.2 试样溶液的制备
称取0.1g(精确至0.0001g)样品于50mL试管中,加入5mL四氢呋喃,超声提取30min,待样品
全部溶解后,缓慢加入25mL甲醇,沉淀聚氯乙烯高聚物,滤纸过滤后分别用5mL甲醇冲洗沉淀三次,
合并滤液于50mL容量瓶中,用甲醇定容并混合均匀,取100μL滤液室温下氮气吹干,用正己烷定容
至1.0mL,待测。若样品浓度超出标准工作溶液线性范围,可使用正己烷适当稀释后测定。
5.3 空白溶液的制备
除不加试样外,采用与5.2完全相同的分析步骤、试剂和用量。
5.4 仪器参考条件
5.4.1 色谱条件
色谱条件列出如下:
a) 色谱柱:固定相为(5%)二苯基-(95%)二甲基亚芳基硅氧烷共聚物,柱长30m,内径0.32mm,
膜厚0.25μm;
b) 柱温程序:初始温度为90℃,然后以15℃/min的速率升至280℃,保持10min;
c) 进样口温度:280℃;
d) 载气:氦气1.5mL/min;
e) 进样方式:分流方式,分流比为。
5.4.2 质谱条件
质谱条件列出如下:
a) 质谱接口温度:250℃;
b) 离子源温度:250℃;
c) 离子化方式:EI;
d) 离子化能量:70eV;
e) 测定方式:选择离子监测模式,DEHA的监测离子范围(m/z):40~370,DEHA的特征离子为
129、147、112、71,其中129为定量离子。
5.5 绘制标准工作曲线
按照5.4所列测定条件,分别将标准工作溶液(3.3.3)依次注入气相色谱-质谱仪中,以标准工作溶
液中浓度为横坐标,单位为毫克每升(mg/L),以对应DEHA峰面积为纵坐标,绘制标准曲线。标准色
谱图参见图A.1。
5.6 试样溶液的测定
5.6.1 定性测定
按照5.4所列测定条件,将试样溶液(5.2)、空白溶液(5.3)进样气相色谱-质谱仪测定。在相同的实
验条件下进行样品测定时,若试样溶液中待测物的色谱峰的保留时间与相应标准的色谱峰的保留时间
的偏差在±2.5%以内,并且在扣除背景后的样品质谱中,所选择的离子均出现,且样品谱图中定性离子
的相对丰度与浓度接近的标准溶液谱图中对应定性离子的相对丰度进行比较,偏差不超过表1规定的
范围,则可判定为样品中存在该种待测物。DEHA的特征离子及其丰度比见表2,DEHA质谱图见图
GB 31604.28-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Food contact materials and products -
Determination of di (2-ethylhexyl) adipate and migration
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of People's
Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
Determination of di (2-ethylhexyl) adipate (DEHA) ... 4
2 Principle... 4
3 Reagents and materials ... 4
4 Instruments and equipment ... 5
5 Analytical steps ... 6
6 Expression of the analytic result ... 8
7 Precision... 8
8 Others ... 8
Determination of di (2-ethylhexyl) adipate (DEHA) migration ... 9
9 Principle... 9
10 Reagents and materials... 9
11 Instruments and equipment ... 11
12 Analytical steps ... 11
13 Expression of the analytic result ... 13
14 Precision ... 13
15 Others ... 14
Appendix A Total ion flow chromatogram and mass spectrogram of standard
solution ... 15
Foreword
This standard replaces GB/T 20499-2006 "Method for the determination of di
(2-ethylhexyl) adipate migrating from polyvinyl chloride film in contact with
foodstuffs", “Method for the determination of di (2-ethylhexyl) adipate” in GB/T
20500-2006 “Method for the determination of di (2-ethylhexyl) adipate and
di-n-octyl adipate in polyvinyl chloride film” and “Method for the determination
of di (2-ethylhexyl) adipate migration” in SN/T 2826-2011 “Food contact
materials for export. Polymers. Determination of adipate plasticizers in food
stimulants. Gas chromatography-mass spectrometry”.
The main differences of this standard in comparison with GB/T 20499-2006
and GB/T 20500-2006 are as follows.
- Changed the name of the standard to "National Food Safety Standard -
Food contact materials and products - Determination of di (2-ethylhexyl)
adipate and migration";
- Deleted the gas chromatography-mass spectrometry for determination of
di (2-ethylhexyl) adipate.
National Food Safety Standard - Food contact materials
and products - Determination of di (2-ethylhexyl) adipate
and migration
1 Scope
This standard specifies the methods of determination of di (2-ethylhexyl)
adipate (DEHA) and migration in food contact materials and products.
This standard is applicable to the determination of di (2-ethylhexyl) adipate
and migration in polyvinyl chloride products.
Determination of di (2-ethylhexyl) adipate (DEHA)
2 Principle
Dissolve the sample with tetrahydrofuran and precipitate the polymer by
methanol. After filtration, DEHA remains in the filtrate. Determine by gas
chromatography-mass spectrometer and quantify by external standard
method.
3 Reagents and materials
3.1 Reagent
Unless otherwise stated, the reagents used in this method shall be analytical
pure. The water shall be the primary water specified in GB/T 6682.
3.1.1 Tetrahydrofuran (C4H8O, CAS No..109-99-9)
3.1.2 Methanol (CH4O,CAS No..67-56-1)
3.1.3 N-hexane (C6H12,CAS No..110-54-3). Chromatographic pure
3.2 Standard product
standard substance certified by the State and granted the standard
The mass spectrum conditions are as follows.
a) Mass spectrum interface temperature. 250°C;
b) Temperature of ion source. 250°C;
c) Ionization mode. EI;
d) Ionization energy. 70 eV;
e) Determination method. select the ion monitoring mode, the monitoring
ion range(m/z) of DEHA. 40~370, the DEHA characteristic ions of are.
129, 147, 112, 71, of which 129 is quantitative ion;
5.5 Making of standard curve
According to the determination conditions listed in 5.4, inject the standard
working solution (3.3.3) into the gas chromatography-mass spectrometer in
turn. The standard curve was drawn with the concentration of the standard
working solution as the horizontal coordinate with the unit of mg per liter
(mg/L), and the corresponding peak area of DEHA as the vertical coordinate.
See figure A.1. for a standard chromatogram.
5.6 Determination of sample solution
5.6.1 Qualitative determination
sample solution (5.2) and the blank solution (5.3) into the gas
chromatography-mass spectrometer for determination. When determine the
sample under the same experimental conditions, if the deviation of the
chromatographic peak retention time of the substance to be determined in the
sample solution is within ±2.5% of the chromatographic peak retention time of
the standard substance; and all the selected ions appear in the sample mass
spectrometry after background subtraction; and the deviation of the relative
abundance of the qualitative ion in the sample spectrum compared with the
relative abundance of the qualitative ion in the standard solution with similar
determined that there is such substance in the sample. The characteristic
ions and their abundance ratios of DEHA are shown in Table 2. For DEHA
chromatogram see figure A.2.
Table 1 -- Maximum allowable deviation of relative ion abundance in
qualitative confirmation
Relative ion abundance K /% >50 20~50 10~20 ≤10
DEHA concentration of 2mg/mL is obtained. Store the solution in the
refrigerator for validity period of 1 month.
10.4.2 DEHA standard intermediate solution (Water, acidic, alcohol
Draw 2.5mL DEHA standard reserve solution (10.4.1) with graduated pipette
to 50mL volumetric bottle, dilute to the scale with n-hexane. The standard
intermediate solution of DEHA is obtained with the concentration of
100.0mg/L. The storage method of the solution is the same as that of 10.4.1.
10.4.3 DEHA standard working solution (for water, acidic, alcohol based
food simulants analysis)
Draw with graduated pipette and micro-syringe respectively 50μL, 0.2mL,
0.5mL, 1.0mL, 2.0mL, 5.0mL of the DEHA standard intermediate solution
(10.4.2), place them in 6 10mL volumetric bottles, dilute with n-hexane, meter
obtained with concentration of 0.5mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L,
20.0mg/L, 50.0mg/L. The storage method is the same as that of 10.4.1.
10.4.4 DEHA standard reserve solution (for oil-based food simulants
analysis)
Weigh DEHA 50mg (precision to 0.0001g) and put it into the 50mL beaker.
Add oil-based food simulant 50g (precision to 0.0001g), dissolve and mix
evenly. The concentration of the standard reserve solution is 1000mg/kg.
Store the solution in the refrigerator for validity period of 1 month.
10.4.5 DEHA standard intermediate solution (for oil-based food
Weigh 1.0g (precision to 0.01g) of DEHA standard reserve solution (10.4.4),
put into the 10mL volumetric bottle. Weigh accurately 9.0g (precision to
0.0001g) of oil-based food simulant and put into the same bottle. Mix to obtain
the DEHA standard intermediate solution with the concentration of 100mg/kg.
The storage method of the solution is the same as that of 10.4.4.
10.4.6 DEHA standard working solution (for oil-based food simulants
analysis)
Weigh respectively 0.2g, 0.5g, 1.0g, 2.0g, 4.0g, 5.0g (precision to 0.01g) of
the DEHA standard intermediate solution (10.4.5), place them into 6 10mL
(precision to 0.0001g) of oil-based food simulant, shake to mix and obtain the
standard working solution of DEHA with concentration of 2mg/kg, 5mg/kg,
10mg/kg, 20mg/kg, 40mg/kg, 50mg/kg respectively. Weigh respectively the
e) Determination method. select the ion monitoring mode, the monitoring
ion range(m/z) of DEHA. 40~370, the DEHA characteristic ions of are.
129, 147, 112, 71, of which 129 is the quantitative ion;
f) Solvent delay by. 5 min.
12.5 Making of standard curve
In accordance with the determination conditions listed in 12.4, determine
working solution (10.4.3, 10.4.6). Draw the standard curve using the DEHA
concentration in the standard working solution as the horizontal coordinate, in
unit of “milligram per liter(mg/L) (water, acid, alcohol-based food simulant), or
milligrams per kilogram (mg/kg) (oil-based food simulant)", and the peak area
of corresponding DEHA as the vertical coordinate.
12.6 Determination of sample solution
12.6.1 Qualitative determination
In accordance with the determination conditions listed in 12.4, inject the
sample solution (12.2) and the blank solution (12.3) into gas chromatography
5.6.1.
12.6.2 Quantitative determination
When determine the sample and blank solution, deduct the blank value to
obtain the peak area of DEHA.
13 Expression of the analytic result
Obtain the concentration of DEHA in the sample solution from the standard
curve. Calculate according to GB 5009.156 to obtain the migration amount of
DEHA in food contact materials and products. Retain two-digit valid numbers
for the results of calculation.
The absolute difference between the two independent measurements
obtained under repetitive conditions shall not exceed 10% of the arithmetic
average.
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