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食品安全国家标准 食品接触材料及制品 1，3-苯二甲胺迁移量的测定
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GB 31604.11-2016
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标准编号: GB 31604.11-2016 (GB31604.11-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 1，3-苯二甲胺迁移量的测定
英文名称: Food contact materials -- Polymer -- Determination of 1 3-benzenedimethanamine in food simulants -- High performance liquid chromatography
行业: 国家标准
中标分类: X09
字数估计: 8,865
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2550-2010; GB/T 23296.25-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.11-2016: 食品安全国家标准 食品接触材料及制品 1，3-苯二甲胺迁移量的测定
GB 31604.11-2016 英文名称: Food contact materials -- Polymer -- Determination of 1 3-benzenedimethanamine in food simulants -- High performance liquid chromatography
本标准规定了食品接触材料及制品中1,3-苯二甲胺迁移量的高效液相色谱测定方法。
本标准适用于食品接触材料及制品中1,3-苯二甲胺迁移量的测定。
2 原理
食品接触材料进行迁移试验后,对水基、酸性、酒精类食品模拟物中1,3-苯二甲胺进行荧光胺衍
生,然后通过高效液相色谱进行分离,采用荧光检测器检测,外标法定量;油性模拟物中1,3-苯二甲胺
经4%乙酸溶液萃取后采用同样方法检测。
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规定的一级水且用氮气饱和。
3.1 试剂
3.1.1 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。
3.1.2 甲醇(CH4O,CAS号:67-56-1):色谱纯。
3.1.3 四氢呋喃(C4H8O,CAS号:109-99-9):色谱纯。
3.1.4 丙酮(C3H6O,CAS号:67-64-1)。
3.1.5 庚烷(C7H16,CAS号:142-82-5)。
3.1.6 乙酸(C2H4O2,CAS号:64-19-7)。
3.1.7 荧光胺(C17H10O4,CAS号:38183-12-9):纯度≥98%。
3.1.8 十水合四硼酸钠(Na2B4O7·10H2O,CAS号:1330-43-4)。
3.1.9 氢氧化钠(NaOH,CAS号:1310-73-2)。
3.1.10 氮气:99.999%。
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 四氢呋喃溶液(体积分数为90%):量取90mL四氢呋喃于100mL容量瓶中,用水定容至刻度。
3.2.3 荧光胺溶液(2mg/mL):称取50mg(精确至0.0001g)荧光胺,用丙酮溶解后,定容至25mL。
该溶液在5℃下避光储存,有效期一周。
3.2.4 氢氧化钠溶液(5mol/L):称取20g氢氧化钠,用水溶解后,定容至100mL。
3.2.5 硼酸缓冲溶液(0.15mol/L,pH=9.2):称取14.3g十水四硼酸钠,用水溶解后,定容至250mL。
在使用溶液前,如果由于温度下降而导致沉淀则需要重新溶解。
3.2.6 乙酸溶液(质量浓度为4%):称取乙酸20g,用水溶解后,定容至500mL。
3.2.7 硼酸缓冲溶液(0.02mol/L,pH=9.2):吸取133mL的0.15mol/L硼酸缓冲溶液(3.2.5),用水
稀释定容至1L。
3.2.8 高效液相色谱流动相[硼酸缓冲液∶水∶甲醇(18∶37∶45)]:吸取180mL的0.02mol硼酸缓
冲溶液(3.2.7)、370mL水、450mL甲醇混合。
3.3 标准品
1,3-苯二甲胺标准品(C8H12N2,CAS号:1477-55-0):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 1,3-苯二甲胺标准储备液
称取50mg(精确至0.0001g)1,3-苯二甲胺,用水溶解后,定容至50mL,浓度为1000mg/L。该
溶液在5℃下避光储存,有效期3个月。
3.4.2 用于水基(酸性、酒精类)食品模拟物的1,3-苯二甲胺标准工作溶液
用刻度吸量管吸取0.20mL的1,3-苯二甲胺标准储备液(3.4.1)于100mL容量瓶中,用水基(酸
性、酒精类)食品模拟物稀释至刻度,获得浓度为2.0mg/L的用于水基(酸性、酒精类)食品模拟物的1,
3-苯二甲胺标准工作溶液。该溶液在5℃下避光储存,有效期为1个月。
3.4.3 用于油基模拟物的1,3-苯二甲胺标准工作溶液
用刻度吸量管吸取2.0mL的1,3-苯二甲胺标准储备液(3.4.1)于100mL容量瓶中,用水稀释至刻
度,得浓度为20.0mg/L的溶液。吸取10mL该溶液于100mL容量瓶中,用四氢呋喃溶液(3.2.2)稀
释至刻度,得浓度为2.0mg/L的用于油基模拟物的1,3-苯二甲胺标准工作溶液。该溶液在5℃下避
光储存,有效期为1个月。
3.4.4 水基(酒精类)食品模拟物的1,3-苯二甲胺标准工作溶液
分别用刻度吸量管吸取0.5mL、2.0mL、3.0mL、4.0mL、5.0mL的1,3-苯二甲胺标准工作溶液
(3.4.2)于5个100mL容量瓶中,用相应的食品模拟物(水基、酒精食品模拟物)定容至刻度,得到浓度
分别为0.010mg/L、0.040mg/L、0.060mg/L、0.080mg/L、0.10mg/L标准工作溶液。用刻度吸量管
分别吸取上述溶液2.0mL于5个5mL试管中,分别加入0.4mL硼酸缓冲溶液(3.2.5),充分混匀。分
别加入300μL荧光胺溶液(3.2.3)衍生试剂,振荡1min,静置10min。衍生溶液过0.45μm滤膜后供
高效液相色谱进样。
3.4.5 酸性食品模拟物的1,3-苯二甲胺标准工作溶液
分别用刻度吸量管吸取0.5mL、2.0mL、3.0mL、4.0mL、5.0mL酸性食品模拟物中的1,3-苯二甲
胺标准工作溶液(3.4.2)于5个100mL容量瓶中,用酸性食品模拟物定容至刻度,得到浓度分别为
0.010mg/L、0.040mg/L、0.060mg/L、0.080mg/L、0.10mg/L标准工作溶液。准确吸取上述溶液中
各10.0mL于5个25mL烧杯中,在第一个烧杯中滴加5mol/L氢氧化钠溶液(3.2.4),调节pH至9.2,
计算所需氢氧化钠溶液的体积,准确至0.01mL。在另外4个烧杯中,准确加入上述滴加体积的氢氧化
钠溶液(3.2.4),充分混匀(各溶液pH应在8.0~9.9范围内)。以下按3.4.4中“用刻度吸量管分别吸取
上述溶液2.0mL供高效液相色谱进样”操作。
3.4.6 油基食品模拟物标准工作溶液
称取20.0g(精确至0.01g)油基模拟物,置于5个125mL分液漏斗中,分别用刻度吸量管吸取加
入0.2mL、0.4mL、0.6mL、0.8mL、1.0mL的1,3-苯二甲胺标准工作溶液(3.4.3)于该5个125mL分
液漏斗中。分别准确加入0.8mL、0.6mL、0.4mL、0.2mL和0mL的四氢呋喃溶液(3.2.2)和5.0mL
庚烷,充分混匀,再加入20.0mL乙酸溶液(3.2.6),振荡5min,静置15min,待两相完全分离后,收集水
相萃取物,得到浓度分别为0.02mg/kg、0.04mg/kg、0.06mg/kg、0.08mg/kg、0.10mg/kg油基食品模
拟物标准工作溶液。准确移取上述工作溶液中各10mL于5个25mL烧杯中,在第一个烧杯中滴加
5mol/L氢氧化钠溶液(3.2.4),调节pH至9.2,计算所需氢氧化钠溶液的体积,准确至0.01mL。在另
外4个烧杯中,准确加入上述滴加体积的氢氧化钠溶液(3.2.4),充分混匀(各溶液pH应在8.0~9.9范
围内)。以下按3.4.4中“用刻度吸量管分别吸取上述溶液2.0mL供高效液相色谱进样”操作。
4 仪器和设备
4.1 高效液相色谱仪:配荧光检测器(FLD)。
4.2 分析天平:感量为0.0001g。
4.3 涡旋混匀器。
4.4 机械振荡器。
4.6 恒温水浴。
5 分析步骤
5.1 试样迁移试验
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。
所得食品模拟物试液应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 水基和酒精类食品模拟物的制备
用刻度吸量管吸取从迁移试验中得到的水基(酒精类)食品模拟物2.0mL于5mL试管中,加入
液过0.45μm滤膜后供高效液相色谱进样。
5.2.2 酸性食品模拟物的制备
用刻度吸量管吸取从迁移试验中获得的10.0mL酸性食品模拟物于25mL烧杯中,滴加入
5mol/L氢氧化钠溶液(3.2.4),体积同3.4.5中氢氧化钠溶液体积,充分混匀(溶液pH应在8.0~9.9范
围内)。用刻度吸量管吸取上述溶液2.0mL于5mL试管中,以下按5.2.1中“加入0.4mL硼酸缓冲液
供高效液相色谱进样”操作。
5.2.3 油基食品模拟物的制备
称取20.0g(精确至0.01g)橄榄油模拟物置于125mL分液漏斗中,分别加入1mL的四氢呋喃溶
液和5.0mL庚烷。充分混匀后,加入20mL乙酸溶液,振荡5min,静置15min,待两相完全分离后,收
(3.2.4),体积同3.4.6中氢氧化钠溶液体积,充分混匀(溶液pH应在8.0~9.9范围内)。用刻度吸量管
吸取上述溶液2.0mL于5mL试管中,以下按5.2.1中“加入0.4mL硼酸缓冲液供高效液相色谱
进样”操作。
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 色谱柱:C18,柱长150mm,内径4.6mm,粒径5μm。
5.4.2 流动相:高效液相色谱流动相[硼酸缓冲液∶水∶甲醇(18∶37∶45)]。
5.4.3 流速:1.0mL/min。
5.4.5 荧光检测器:激发波长394nm,发射波长480nm。
5.4.6 进样量:20μL。
5.5 绘制标准工作曲线
按5.4所列测定条件,分别将水基、酸性、酒精类、油基食品模拟物标准工作溶液(3.4.4、3.4.5、
3.4.6)进高效液相色谱仪器测定。以食品模拟物中1,3-苯二甲胺浓度为横坐标,单位为“mg/L(水基、
酸性、酒精类食品模拟物)或mg/kg(油基食品模拟物)”,以1.3-苯二甲胺峰面积为纵坐标,绘制标准工
作曲线。标准溶液色谱图见图A.1。
5.6 试样溶液的测定
按5.4所列条件,分别将模拟物溶液(5.2)、空白溶液(5.3)依次进液相色谱仪测定,得到目标物峰面
6 分析结果的表述
由标准曲线得到试样溶液中1,3-苯二甲胺的浓度,按GB 5009.156进行迁移量计算,得到食品接触
材料及制品中1,3-苯二甲胺的迁移量。计算结果保留两位有效数字。
7 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%。
8 其他
水基、酸性、酒精类食品模拟物中1,3-苯二甲胺的方法检出限为0.004mg/L、定量限为0.01mg/L;
油基食品模拟物中1,3-苯二甲胺的方法检出限为0.006mg/kg、定量限为0.02mg/kg。
GB 31604.11-2016
GB
NATIONAL STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Contact
Materials and Articles - Determination of Migration of
1,3-benzenedimethanamine
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 Instruments and equipment ... 7
5 Analysis steps ... 8
6 Expression of analysis results ... 9
7 Precision... 10
8 Other ... 10
Annex A Liquid chromatogram ... 11
Foreword
This Standard replaces GB/T 23296.25-2009 Food contact materials - Polymer
- Determination of 1 3-benzenedimethanamine in food simulants - High
performance liquid chromatography and SN/T 2550-2010 Food contact
materials. Polymer materials. Determination of 1,3-benzenedimethanamine in
food simulants.
Compared with GB/T 23296.25-2009, the main change in this Standard is as
follow.
- modified the standard’s name to “National Food Safety Standard - Food
Contact Materials and Articles - Determination of Migration of 1,3-
benzenedimethanamine”.
National Food Safety Standard - Food Contact
Materials and Articles - Determination of Migration of
1,3-benzenedimethanamine
1 Scope
This Standard specifies the high-performance liquid chromatography method
for determination of migration of 1,3-benzenedimethanamine.
This Standard is applicable to the determination of migration of 1,3-
benzenedimethanamine in food contact materials and articles.
2 Principle
After the migration test of food contact materials, 1,3-benzenedimethylamine in
water-based, acidic and alcohol food simulants shall be subjected to fluorescent
amine derivatization, then separation by high performance liquid
chromatography. Using fluorescence detector detection, external standard
method to quantify.
3 Reagents and materials
Unless otherwise specified, the reagents used in this method are of analytical
grade, water is of grade one specified in GB/T 6682 and saturated with nitrogen.
3.1 Reagents
3.1.1 Water-based, acidic, alcohol-based, oil-based food simulants. reagents
used in accordance with the provisions of GB 31604.1
3.1.2 Methanol (CH4O, CAS No.. 67-56-1). chromatographic pure
3.1.3 Tetrahydrofuran (C4H8O, CAS No. 109-99-9). chromatographic pure
3.1.4 Acetone (C3H6O, CAS No. 67-64-1)
3.1.5 Heptane (C7H16, CAS No.. 142-82-5)
3.1.6 Acetic acid (C2H4O2, CAS No.. 64-19-7)
Weigh 50 mg (nearest to 0.0001 g) of 1,3-benzenedimethylamine. Dissolve with
water. Set volume to 50 mL. The concentration shall be 1000 mg/L. This
solution shall be stored in the darkness at 5°C for three months.
3.4.2 1,3-benzenedimethylamine standard working solution used for
water-based (acidic, alcoholic) food simulants
Pipette 0.20 mL of 1,3-benzenedimethanamine standard stock solution (3.4.1)
in a 100mL volumetric flask with a graduated pipette. Dilute to scale with a
water-based (acidic, alcoholic) food simulant to obtain a 1,3-
benzenedimethanamine standard working solution for water-based (acidic,
alcoholic) food simulants with a concentration of 2.0 mg/L. This solution shall
be stored in the darkness at 5°C for one month.
3.4.3 1,3-benzenedimethylamine standard working solution used for oil-
Pipette 2.0 mL of 1,3-xylylenediamine standard stock solution (3.4.1) in a 100
mL volumetric flask with a graduated pipette. Dilute to scale with water to obtain
a solution with a concentration of 20.0 mg/L. Pipette 10 mL of this solution in a
100 mL volumetric flask. Dilute to scale with tetrahydrofuran solution (3.2.2) to
obtain 1,3-benzenedimethylamine standard working solution for oil-based
simulants with a concentration of 2.0 mg/L. This solution shall be stored in the
darkness at 5°C for one month.
3.4.4 1,3-benzenedimethylamine standard working solution of water-
based (alcoholic) food simulants
mL, 5.0 mL of 1,3-benzenedimethylamine standard working solution (3.4.2) in
five 100 mL volumetric flasks. Use corresponding food simulants (water-based,
alcohol food simulants) to set volume to scale and obtain standard working
solutions with concentrations of 0.010 mg/L, 0.040 mg/L, 0.060 mg/L, 0.080
mg/L, 0.10 mg/L. Pipette 2.0 mL of the above solution into 5 5-mL tubes with a
graduated pipette. Separately add 0.4 mL of boric acid buffer solution (3.2.5),
mix well. Add 300 μL of fluorescein solution (3.2.3) derivatization reagent
separately, oscillating 1min, placing still 10min. The derivative solution is filtered
through a 0.45 μm filter for high performance liquid chromatography injection.
food simulants
Respectively using a graduated pipette to pipette 0.5 mL, 2.0 mL, 3.0 mL, 4.0
mL, 5.0 mL of 1,3-benzenedimethylamine standard working solution (3.4.2) in
acidic food simulants into five 100 mL volumetric flasks. Use acidic food
simulants to set volume to scale to obtain standard working solutions with
concentrations of 0.010 mg/L, 0.040 mg/L, 0.060 mg/L, 0.080 mg/L, 0.10 mg/L.
5 Analysis steps
5.1 Sample migration test
In accordance with the requirements of GB 5009.156 and GB 31604.1, carry
resulting food simulant test solution cannot be immediately used for the next
test, the food simulant test solution shall be stored in a 4°C refrigerator from
light.
The resulting food simulant test solution shall be cooled or returned to room
temperature before proceeding to the next test.
5.2 Preparation of test solution
5.2.1 Preparations of water-based and alcohol food simulants
Pipette 2.0 mL of a water-based (alcoholic) food simulant obtained from the
migration test in a 5-mL tube with a graduated pipette. Add 0.4 mL of borate
reagent, oscillating 1min, placing still 10min. The derivative solution is filtered
through a 0.45 μm filter for high performance liquid chromatography injection.
5.2.2 Preparation of acidic food simulants
Pipette 10.0 mL of acidic food simulants from the migration test in a 25-mL
beaker by using a graduated pipette. Drop 5 mol/L sodium hydroxide solution
(3.2.4) with same volume as sodium hydroxide solution in 3.4.5, well mixing
(solution pH shall be within 8.0~9.9). Pipette 2.0 mL of the above solution in a
5-mL tube with a graduated pipette. The rest shall follow “add 0.4 mL of borate
buffer.for high performance liquid chromatography injection” in 5.2.1.
Weigh 20.0g (nearest to 0.01 g) olive oil mimics placing in a 125-mL separating
funnel. Separately add 1 mL of tetrahydrofuran solution and 5.0 mL of heptane.
After thoroughly mixing, add 20 mL of acetic acid solution, oscillating 5min,
placing still 15min. After the two phases are completely separated, collect the
aqueous phase. Pipette 10.0 mL of the above solution in a 25-mL beaker by
using a graduated pipette. Drop 5 mol/L sodium hydroxide solution (3.2.4) with
same volume as sodium hydroxide solution in 3.4.6, well mixing (solution pH
shall be within 8.0~9.9). Pipette 2.0 mL of the above solution in a 5-mL tube
with a graduated pipette. The rest shall follow “add 0.4 mL of borate buffer.for
5.3 Preparation of blank solution
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