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食品安全国家标准 食品接触材料及制品 乙二胺和己二胺迁移量的测定
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GB 31604.43-2016
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标准编号: GB 31604.43-2016 (GB31604.43-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 乙二胺和己二胺迁移量的测定
英文名称: Food contact materials -- Polymer -- Determination of 1 2-diaminoethane and 1 6-diaminohexane in food simulants -- Gas chromatography
行业: 国家标准
中标分类: X09
字数估计: 10,163
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): GB/T 23296.17-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.43-2016: 食品安全国家标准 食品接触材料及制品 乙二胺和己二胺迁移量的测定
GB 31604.43-2016 英文名称: Food contact materials -- Polymer -- Determination of 1 2-diaminoethane and 1 6-diaminohexane in food simulants -- Gas chromatography
1 范围
本标准规定了食品接触材料及制品中乙二胺和己二胺迁移量的气相色谱的测定方法。
本标准适用于食品接触材料及制品中乙二胺和己二胺迁移量的测定。
2 原理
用氯甲酸乙酯作为衍生试剂,将食品模拟物中的乙二胺和己二胺衍生转化为相应的二氨基甲酸乙
酯衍生产物,采用气相色谱柱进行分离,氢火焰离子化检测器进行检测。内标法定量,内标物为1,3-丙
二胺。
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。试验中容器及转移
器具应避免使用塑料材质。
3.1 试剂
3.1.1 氯甲酸乙酯(C3H5ClO2):纯度大于97%。
3.1.2 冰乙酸(C2H4O2)。
3.1.3 无水乙醇(C2H6O)。
3.1.4 甲苯(C7H8)。
3.1.5 乙醚(C4H10O)。
3.1.6 异辛烷(C8H18)。
3.1.7 无水硫酸钠(Na2SO4)。
3.1.8 氢氧化钠(NaOH)。
3.1.9 氨水:浓度为25%(质量分数)。
3.1.10 配制水基、酸性、酒精类、油基食品模拟物所需试剂:符合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的规定操作。
3.2.2 氨水溶液(3%,体积分数):在250mL锥形瓶中加入200mL水和30mL25%氨水溶液,混合
均匀。
3.2.3 氢氧化钠溶液(5mol/L):称取50.0g(精确到0.1g)氢氧化钠于250mL容量瓶中,用水定容。
3.2.4 乙酸溶液(4%,质量分数):称取40g(精确到0.1g)冰乙酸于1L容量瓶中,用水定容。
3.2.5 乙醇溶液(10%,体积分数):量取100mL无水乙醇于1L容量瓶中,用水定容。
3.2.6 乙醇溶液(95%,体积分数):量取475mL无水乙醇于500mL容量瓶中,用水定容。
3.3 标准品
3.3.1 乙二胺(C2H8N2,CAS号:107-15-3),纯度 >99%,或经国家认证并授予标准物质证书的标准
物质。
3.3.2 己二胺(C6H16N2,CAS号:124-09-4),纯度 >99%,或经国家认证并授予标准物质证书的标准
物质。
3.3.3 1,3-丙二胺(C3H10N2,CAS号:109-76-2),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 水配制的乙二胺储备液(1000mg/L):准确称取乙二胺50mg(精确至0.1mg)于50mL容量瓶
中,用水定容。
3.4.2 水配制的己二胺储备液(500mg/L):准确称取己二胺25mg(精确至0.1mg)于50mL容量瓶
中,用水定容。
3.4.3 水配制的丙二胺储备液(500mg/L):准确称取丙二胺25mg(精确至0.1mg)于50mL容量瓶
中,用水定容。
3.4.4 甲苯配制的乙二胺储备液(1000mg/L):准确称取乙二胺50mg(精确至0.1mg)于50mL容量
瓶中,用甲苯定容。
3.4.5 甲苯配制的己二胺储备液(500mg/L):准确称取己二胺25mg(精确至0.1mg)于50mL容量
瓶中,用甲苯定容。
3.4.6 甲苯配制的丙二胺储备液(500mg/L):准确称取丙二胺25mg(精确至0.1mg)于50mL容量
瓶中,用甲苯定容。
配制的储备液可在5℃~20℃下避光密封保存,3个月内有效。
3.5 器皿和材料
3.5.1 玻璃瓶:2mL、10mL,瓶盖带有涂覆有聚四氟乙烯的丁基橡胶或者硅橡胶密封垫。
3.5.2 容量瓶:50mL。
3.5.3 微量注射器:10μL和25μL。
3.5.4 振荡器。
4 仪器和设备
4.1 气相色谱仪:配氢火焰离子化检测器和数据自动分析软件。
4.2 分析天平:感量0.0001g和0.01g。
5 分析步骤
5.1 标准工作溶液及试样制备
5.1.1 标准工作溶液的制备
5.1.1.1 水基、酸性食品、酒精类食品模拟物和乙醇溶液(95%,体积分数)标准工作溶液
向7个10mL玻璃瓶中分别加入1mL水和10μL水配制的丙二胺储备液,依次加入0μL、1μL、
2μL、3μL、5μL、12μL和24μL水配制的乙二胺储备液和0μL、1μL、2μL、4μL、6μL、8μL、10μL
水配制的己二胺储备液,加盖密封,混合均匀。得到水中乙二胺浓度分别为0.00mg/L、1.00mg/L、
2.00mg/L、3.00mg/L、5.00mg/L、12.0mg/L 和24.0 mg/L;己二胺浓度分别为0.00 mg/L、
0.500mg/L、1.00mg/L、2.00mg/L、3.00mg/L、4.00mg/L和5.00mg/L。采用同样方式,分别用酸性
食品、酒精类食品模拟物和乙醇溶液(95%,体积分数)配制同样浓度系列的乙二胺和己二胺标准工作
溶液。
5.1.1.2 油基食品模拟物和异辛烷标准工作溶液
分别称取1g油基食品模拟物(精确到0.01g)于7个10mL玻璃瓶中,每个玻璃瓶中加入10μL
甲苯配制的丙二胺储备液,依次加入0μL、1μL、2μL、3μL、5μL、12μL和24μL甲苯配制的乙二胺储
备液和0μL、1μL、2μL、4μL、6μL、8μL和10μL甲苯配制的己二胺储备液,加盖密封,混合均匀。得
到油基食品模拟物中乙二胺浓度分别为0.00 mg/kg、1.00 mg/kg、2.00 mg/kg、3.00 mg/kg、
5.00mg/kg、12.0mg/L和24.0mg/kg;己二胺浓度分别为0.00mg/kg、0.500mg/kg、1.00mg/kg、
2.00mg/kg、3.00mg/kg、4.00mg/kg和5.00mg/kg。采用同样方式,用异辛烷配制同样浓度系列的
乙二胺和己二胺标准工作溶液。
5.1.2 食品模拟物试液的制备
食品模拟物试液应按照GB 31604.1和GB 5009.156的要求从迁移试验中获取,应避光于冰箱中冷
藏保存。
当食品接触材料及制品与橄榄油在10d、20℃或者10d、40℃条件下长期接触时,食品接触材料
及制品中迁移出的乙二胺和己二胺会与橄榄油发生反应,导致检测结果偏低,应采用乙醇溶液(95%,体
积分数)或异辛烷替代油基食品模拟物进行检测。
5.1.2.2 水基、酸性食品、酒精类食品模拟物
准确量取迁移试验中得到的水基、酸性食品、酒精类食品模拟物1mL于10mL玻璃瓶中,加入
10μL水配制的丙二胺储备液,加盖密封,混合均匀。
5.1.2.3 油基食品模拟物
甲苯配制的丙二胺储备液,加盖密封,混合均匀。
5.1.2.4 乙醇溶液(95%,体积分数)
准确量取迁移试验中得到的乙醇溶液(95%,体积分数)1.0mL于10mL样品瓶中,加入10μL水
配制的丙二胺储备液,加盖密封,混合均匀。
5.1.2.5 异辛烷
准确量取迁移试验中得到的异辛烷1.0mL于10mL样品瓶中,加入10μL甲苯配制的丙二胺储
备液,加盖密封,混合均匀。
5.1.3 空白试液的制备
按照5.1.2的操作处理未与食品接触材料及制品接触的食品模拟物。
5.2.1 水基、酸性食品、酒精类食品模拟物和乙醇溶液(95%,体积分数)
向盛有水基、酸性食品、酒精类食品模拟物试液的玻璃瓶中加入1mL氨水溶液(3%,体积分数)、
3mL氢氧化钠溶液(5mol/L)、2mL甲苯和200μL氯甲酸乙酯,密封,室温下往复振荡30min。静置
分层后,转移1mL上层甲苯清液于2mL玻璃进样瓶中,加入少许无水硫酸钠,离心后取上层清液供气
相色谱分析。乙醇溶液(95%,体积分数)按照同样程序处理。
5.2.2 油基食品模拟物
向盛有油基食品模拟物试液的玻璃瓶中加入5mL乙醚和1mL乙酸溶液(4%,质量分数),加盖密
封,充分摇匀,静置分层。用移液器转移下层水相于10mL玻璃瓶中,再次用1mL乙酸溶液(4%,质量
分数)重复提取,合并两次提取液。在提取液中加入4mL乙醚进行清洗,移去醚层,再重复用4mL乙
处理。
5.2.3 异辛烷
向盛有异辛烷试液的玻璃瓶中加入1mL乙酸溶液(4%,质量分数),密封,充分摇匀,静置分层。
用移液器转移下层水相于10mL玻璃瓶中,再次用1mL乙酸溶液(4%,质量分数)重复提取,合并两次
提取液。在提取液中加入4mL乙醚进行清洗,移去醚层,再重复用4mL乙醚清洗,最终异辛烷试液中
的乙二胺和己二胺被萃取到水相中,按5.2.1操作步骤进行衍生处理。
5.3 空白试液衍生化处理
按照5.2的操作处理5.1.3中制备的空白试液。
5.4 测定
仪器参考条件列出如下:
a) 色谱柱:100%二甲基硅氧烷柱,长30m,内径0.32mm,膜厚5μm,或相当者;
b) 进样口温度:280℃;
c) 检测器温度:300℃;
d) 炉温:100℃保持1min,以25℃/min上升到270,保持7min;
e) 载气:氮气,流速1.8mL/min;
f) 进样方式:分流进样,分流比10∶1;
g) 进样量:1μL。
5.4.2 标准曲线的制作
品模拟物标准工作溶液中乙二胺或己二胺的浓度为横坐标,以对应的乙二胺衍生物或己二胺衍生物与
内标物丙二胺衍生物之间的峰面积比值为纵坐标,绘制标准工作曲线,得到线性方程。标准溶液的色谱
图参见附录A。
5.4.3 定量测定
对经衍生化处理的食品模拟物试液和空白试液依次进样,分别得到乙二胺衍生物或己二胺衍生物
与内标物丙二胺衍生物峰面积对应比值;根据标准曲线得到试样溶液中乙二胺或己二胺的含量,扣除空
白值。
6 分析结果的表述
由标准曲线得到试样溶液中乙二胺或己二胺的浓度,按照GB 5009.156进行迁移量的计算,得到食
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%。
GB 31604.43-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard - Food contact materials
and products - Determination of migration quantity of
ethylenediamine and hexamethylene diamine
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of the PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principles ... 4
3 Reagents and materials ... 4
4 Instrument and equipment ... 6
5 Analytical procedures ... 7
6 Analysis results expression ... 10
7 Precision ... 10
8. Others ... 11
Appendix A Chromatograms of ethylenediamine and hexamethylene diamine
derivatives in food simulant standard solution ... 12
Foreword
This standard replaces GB/T 23296.17-2009 "Food contact materials -
Polymer - Determination of 1,2-diaminoethane and 1,6-diaminohexane in food
simulants - Gas chromatography"
Compared with GB/T 23296.17-2009, the main changes of this standard are as
follows.
---The standard name has been changed to “National food safety standard -
Food contact materials and products - Determination of migration
quantity of ethylenediamine and hexamethylene diamine”.
National food safety standard - Food contact materials
and products - Determination of migration quantity of
ethylenediamine and hexamethylene diamine
1 Scope
This standard specifies the determination methods for gas chromatography of
migration quantity of ethylenediamine and hexamethylene diamine in food
contact materials and products.
This standard applies to the determination of migration quantity of
ethylenediamine and ethylenediamine in food contact materials and products.
2 Principles
Use ethyl chloroformate as derivatizing reagent; derivatively convert
ethylenediamine and hexamethylene diamine in food simulants to the
corresponding dicarbamate derivatives; use gas chromatography column to
separate; use hydrogen flame ionization detector to test. Use internal standard
method for quantification; the internal standard substance is 1,3-propane
diamine.
3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are analytical
grade, the water is the grade-1 water specified in GB/T 6682. Containers and
transfer implements in the test shall avoid the use of plastic materials.
3.1 Reagents
3.1.1 Ethyl chloroformate (C3H5ClO2). Purity is greater than 97%.
3.1.2 Glacial acetic acid (C2H4O2).
3.1.3 Anhydrous ethanol (C2H6O).
3.1.4 Toluene (C7H8).
3.4 Standard solution preparation
3.4.1 Ethylenediamine stock solution prepared by water (1000mg/L).
Accurately WEIGH 50mg (accurate to 0.1mg) of ethylenediamine; PLACE it
into 50mL volumetric flask; USE water to dilute it.
3.4.2 Hexamethylene diamine stock solution prepared by water (500mg/L).
Accurately WEIGH 25mg (accurate to 0.1mg) of hexamethylene diamine;
PLACE it into 50mL volumetric flask; USE water to dilute it.
3.4.3 Propane diamine stock solution prepared by water (500mg/L). Accurately
WEIGH 25mg (accurate to 0.1mg) of propane diamine; PLACE it into 50mL
volumetric flask; USE water to dilute it.
3.4.4 Ethylenediamine stock solution prepared by toluene (1000mg/L).
Accurately WEIGH 50mg (accurate to 0.1mg) of ethylenediamine; PLACE it
into 50mL volumetric flask; USE toluene to dilute it.
3.4.5 Hexamethylene diamine stock solution prepared by toluene (500mg/L).
PLACE it into 50mL volumetric flask; USE toluene to dilute it.
3.4.6 Propane diamine stock solution prepared by toluene (500mg/L).
Accurately WEIGH 25mg (accurate to 0.1mg) of propane diamine; PLACE it
into 50mL volumetric flask; USE toluene to dilute it.
The prepared stock solution can be stored in dark place at 5°C~20°C, and it is
valid within 3 months.
3.5 Vessels and materials
3.5.1 Glass bottle. 2mL, 10mL, the caps are coated with Teflon-coated butyl
rubber or silicone rubber gaskets.
3.5.3 Micro-syringes. 10μL and 25μL.
3.5.4 Oscillator.
4 Instrument and equipment
4.1 Gas chromatograph. equipped with hydrogen flame ionization detector and
data automatic analysis software.
4.2 Analytical balance. Sensitivity is 0.0001g and 0.01g.
When food contact materials and products are contacted with olive oil at 10d,
20°C or 10d, 40°C for a long period of time, ethylenediamine and
hexamethylene diamine that have migrated from food contact materials and
(95%, volume fraction) or isooctane shall be used to replace oil-based food
simulants for testing.
5.1.2.2 Water-based, acidic food, alcoholic food simulants
Accurately MEASURE 1mL of the water-based, acidic food, and alcoholic food
simulants obtained from the migration test; PLACE it into 10mL glass bottle;
ADD 10μL of propane diamine stock solution prepared by water; COVER and
SEAL it; MIX it uniformly.
5.1.2.3 Oil-based food simulant
Accurately WEIGH 1.0g (accurate to 0.01g) of the oil-based food simulant
of propane diamine stock solution prepared by toluene; COVER and SEAL it;
MIX it uniformly.
5.1.2.4 Ethanol solution (95%, volume fraction)
Accurately MEASURE 1.0mL of the ethanol solution (95%, volume fraction)
obtained from the migration test; PLACE it into 10mL sample bottle; ADD 10μL
of propane diamine stock solution prepared by water; COVER and SEAL it;
MIX it uniformly.
5.1.2.5 Isooctane
Accurately MEASURE 1.0mL of the isooctane obtained from the migration test;
solution prepared by toluene; COVER and SEAL it; MIX it uniformly.
5.1.3 Preparation of blank test solution
Handle the food simulants that have not been in contact with food contact
materials and products in accordance with the operation of 5.1.2.
5.2 Derivatization of food simulant test solution
5.2.1 Water-based, acidic food, alcoholic food simulant and ethanol
solution (95%, volume fraction)
ADD 1mL of ammonia solution (3%, volume fraction), 3mL of sodium
hydroxide solution (5mol/L), 2mL of toluene, and 200μL of ethyl chloroformate
c) Detector temperature. 300°C;
d) Furnace temperature. keep for 1min at 100°C, rise to 270 at 25°C/min,
keep for 7min;
e) Carrier gas. nitrogen, flow rate 1.8mL/min;
f) Sample injection mode. split injection, split ratio 10.1;
g) Injection volume. 1μL.
5.4.2 Drawing of standard curve
Conduct derivatization for the standard working solution prepared in 5.1.1
according to 5.2; TEST it under the instrument parameters listed in 5.4.1. With
standard working solution of food simulants as abscissa, AND the ratio of the
peak area between the corresponding ethylenediamine derivative or
hexamethylene diamine derivative and internal standard substance propane
diamine derivative as vertical axis, DRAW a standard working curve; OBTAIN
a linear equation. See Appendix A for the chromatograms of standard solution.
5.4.3 Quantitative determination
After the sequential sample injection of derivatized food simulant test solution
and blank test solution, OBTAIN the corresponding ratio of the peak area of
ethylenediamine derivative or hexamethylene diamine derivative and internal
content of ethylenediamine or hexamethylene diamine in the sample solution
according to the standard curve; DEDUCT blank value.
6 Analysis results expression
OBTAIB the concentration of ethylenediamine or hexamethylene diamine in
the sample solution from the standard curve; CALCULATE the migration
quantity according to GB 5009.156; OBTAIN the migration quantity of
ethylenediamine or hexamethylene diamine in food contact materials and
products. The calculation result is retained with three significant figures.
7 Precision
under repeatability conditions shall not exceed 10% of the arithmetic mean.
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