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食品安全国家标准 食品接触材料及制品 复合食品接触材料中二氨基甲苯的测定
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GB 31604.23-2016
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标准编号: GB 31604.23-2016 (GB31604.23-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 复合食品接触材料中二氨基甲苯的测定
英文名称: Determination of diaminomethylbezen of complex for food packaging material
行业: 国家标准
中标分类: X09
字数估计: 10,120
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): GB/T 5009.119-2003
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.23-2016: 食品安全国家标准 食品接触材料及制品 复合食品接触材料中二氨基甲苯的测定
GB 31604.23-2016 英文名称: Determination of diaminomethylbezen of complex for food packaging material
1 范围
本标准规定了复合食品包装袋中二氨基甲苯的测定方法。
本标准适用于复合食品包装袋中二氨基甲苯的测定。
第一法 气相色谱法
2 原理
试样中二氨基甲苯用4%乙酸溶液浸出,将浸出液冷却后,在碱性条件下经二氯甲烷提取后,加七
氟丁酸酐衍生化,然后将衍生物注入带有电子捕获检测器的气相色谱仪测定,以保留时间定性,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分析纯,水为GB/T 6682规定的三级水。
3.1 试剂
3.1.1 二氯甲烷(CH2Cl2):色谱纯。
3.1.2 叔丁基甲醚(C5H12O):色谱纯。
3.1.3 七氟丁酸酐(C8F14O3):色谱纯。
3.1.4 无水硫酸钠(Na2SO4)。
3.1.5 氯化钠(NaCl)。
3.1.6 冰乙酸(C2H4O2)。
3.1.7 氢氧化钠(NaOH)。
3.2 试剂配制
3.2.1 乙酸溶液(4%):称取40g冰乙酸溶于960mL水中。
3.2.2 碳酸氢钠溶液(20g/L):称取2g碳酸氢钠溶于水中,定容至100mL。
3.2.3 氢氧化钠溶液(500g/L):称取50g氢氧化钠溶于水中,定容至100mL。
3.3 标准品
2,4-二氨基甲苯(C7H10N2,CAS号:95-80-7),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 二氨基甲苯标准储备溶液:称取二氨基甲苯10mg(精确至0.01mg)于50mL小烧杯中,加二氯
甲烷溶解,用二氯甲烷转移到100mL容量瓶中,定容,混匀,于4℃保存,其中二氨基甲苯的质量浓度
为100μg/mL。
3.4.2 二氨基甲苯标准工作溶液:吸取标准储备溶液0.50mL于50mL容量瓶中,用二氯甲烷定容至
刻度,混匀,于4℃保存,其中二氨基甲苯的质量浓度为1μg/mL。
4 仪器和设备
4.1 气相色谱仪:带电子捕获检测器。
4.2 分析天平:感量为0.01mg和0.01g。
4.3 氮吹仪。
4.4 pH计:精度为0.1。
5 分析步骤
5.1 试样制备
5.1.1 未装过食品的包装袋:用水洗3次,淋干,按2mL/cm2 计算装入乙酸溶液,热封口。
5.1.2 装过食品的包装袋:剪口,将食品全部移出,用清水冲至无污物,再用水冲洗3次,淋干后按
2mL/cm2 计算装入乙酸溶液,热封口。
5.2 迁移试验
将上述5.1.1或5.1.2热封口后的包装袋(使用温度为60℃~120℃),置于预先调至120℃±5℃
的烘箱内,恒温40min,取出自然放冷至室温,剪开封口,将提取液移入干燥的烧杯中备用。
使用温度低于60℃的包装袋,置于预先调至60℃±5℃的烘箱内,恒温2h,取出自然放冷至室
温,剪开封口,将水移入干燥的烧杯中备用。
5.3 衍生过程
量取试样50.0mL,置于分液漏斗中,用氢氧化钠溶液调节pH为8.0,混匀,再加入10g氯化钠混
匀,然后用10mL二氯甲烷分别萃取两次,每次萃取5min,静置10min。合并两次萃取液,经无水硫酸
钠脱水后在40℃下氮吹至近干,加入2mL二氯甲烷,混匀,再加入100μL七氟丁酸酐,轻轻混匀,置
于室温下进行衍生化反应15min。
将上述反应液移入60mL分液漏斗中,用2mL二氯甲烷分数次洗净浓缩瓶,洗液并入分液漏斗
中,加入5mL碳酸氢钠溶液,轻轻摇动2min,静置5min,将二氯甲烷层移入到10mL试管中,在40℃
下氮吹至近干,用叔丁基甲醚溶解并定容至5.00mL,注入气相色谱仪分析。
5.4 二氨基甲苯标准测定液的制备
分别吸取适量的二氨基甲苯工作液,加入100μL七氟丁酸酐,轻轻混匀,置于室温下进行衍生化反
应15min。将上述反应液移入60mL分液漏斗中,用2mL二氯甲烷分数次洗净浓缩瓶,洗液并入分
液漏斗中,加入5mL碳酸氢钠溶液,轻轻摇动2min,静置5min,将二氯甲烷层移入到10mL试管中,
在40℃下氮吹至近干,用叔丁基甲醚溶解并定容至5mL。
5.5 气相色谱参考条件
a) 色谱柱:HP-5MS,柱长30m,内径0.25mm,膜厚0.25μm或同等性能的色谱柱;
b) 柱温度程序:初始温度60℃保持2min,以15℃/min升温至240℃,保持5min;
c) 进样口温度:200℃;
d) 载气:氮气,纯度≥99.999%,1.0mL/min;尾吹气,30mL/min;
e) 检测器:电子捕获检测器(ECD),温度300℃;
f) 进样方式:不分流进样。
5.6 试样溶液的测定
将试样溶液注入气相色谱仪中,色谱图见图A.1,得到峰高或峰面积,以标准工作液的浓度为横坐
标,以色谱峰高或峰面积为纵坐标,绘制标准曲线。根据标准曲线得到待测液中二氨基甲苯的浓度。
6 分析结果的表述
试样中二氨基甲苯的含量按式(1)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 检出限及定量限
当取样量50.0mL,定容体积为5.00mL时,本方法的检出限为0.0005mg/L,定量限为0.001mg/L。
第二法 气相色谱-质谱法
9 原理
氟丁酸酐衍生化,然后将衍生物注入气相色谱-质谱仪测定,外标法定量。
GB 31604.23-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Contact Materials
and Articles - Determination of Diaminomethylbezen in
Complex Food Contact Materials and Articles
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 Instruments and equipment . 5
5 Analytical procedures . 6
6 Analysis results expression . 7
7 Precision. 8
8 Limits of detection and quantitation . 8
9 Principles . 8
10 Reagents and materials. 9
11 Instruments and equipment . 9
12 Analytical procedures . 9
13 Analysis results expression .. 11
14 Precision .. 11
15 Limits of detection and quantitation . 11
Appendix A Chromatograms of diaminomethylbezen standard derivatives . 12
National Food Safety Standard - Food Contact Materials
and Articles - Determination of Diaminomethylbezen in
Complex Food Contact Materials and Articles
1 Scope
This Standard specifies the method for determination of diaminomethylbezen
of complex for food packaging material.
This Standard applies to the determination of diaminomethylbezen of complex
for food packaging material.
Method I Gas chromatography
2 Principles
USE 4% acetic acid solution to leach the diaminomethylbezen in the sample;
after the leaching solution is cooled and extracted with dichloromethane under
alkaline conditions, ADD heptafluorobutyric anhydride to derivatize; then,
INJECT the derivatives into a gas chromatograph with electron capture detector
for determination; USE retention time to determine the quality, and the external
standard method to quantify.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are analytically pure.
The water is the Grade III water specified in GB/T 6682.
3.1 Reagents
3.1.1 Dichloromethane (CH2CI2). chromatographically pure.
3.1.2 Tert-butyl methyl ether (C5H12O). chromatographically pure.
3.1.3 Heptafluorobutyric anhydride (C8F14O3). chromatographically pure.
3.1.4 Anhydrous sodium sulfate (Na2SO4).
5 Analytical procedures
5.1 Preparation of samples
5.1.1 Packaging material which does not contain food ever. USE water to wash
for 3 times; DRY it; at 2 mL/cm2, FILL it with acetic acid solution; and heat seal.
5.1.2 Packaging material which contains food ever. SNIP the seal; REMOVE
all the food; USE clean water to rinse until there is no dirt; and USE water to
wash for 3 times; after drying it, at 2 mL/cm2, FILL it with acetic acid solution;
and heat seal.
5.2 Migration test
PUT the above 5.1.1 or 5.1.2 heat-sealed packaging material (The operating
temperature is 60 °C~120 °C) in an oven pre-adjusted to 120 °C±5 °C; KEEP it
at constant temperature for 40 min; TAKE it out and COOL naturally to room
temperature; then SNIP the seal; and REMOVE the extract into a dry beaker;
SET aside.
PUT the packaging material (The operating temperature is less than 60 °C) in
an oven pre-adjusted to 60 °C±5 °C; KEEP it at constant temperature for 2 h;
TAKE it out and COOL naturally to room temperature; then SNIP the seal; and
REMOVE the water into a dry beaker; SET aside.
MEASURE 50.0 mL of the sample; PLACE it in a separatory funnel; USE
sodium hydroxide solution to adjust the pH to 8.0; MIX well; and ADD 10 g of
sodium chloride and MIX well; then USE 10 mL of dichloromethane to extract
twice, 5 min each time; LET it stand for 10 min. COMBINE the two extracts;
after being dehydrated with anhydrous sodium sulfate, at 40°C, BLOW nitrogen
until nearly dry; ADD 2 mL of dichloromethane and MIX well; and ADD 100 μL
of heptafluorobutyric anhydride, MIX gently; at room temperature, CARRY out
derivatization reaction for 15 min.
TRANSFER the above reaction solution into a 60 mL separatory funnel; USE 2
INCORPORATE the washing liquor into the separatory funnel; ADD 5 mL of
sodium bicarbonate solution; gently SHAKE it for 2 min; LET it stand for 5 min;
TRANSFER the dichloromethane layer into a 10 mL test tube; at 40°C, BLOW
nitrogen until nearly dry; USE tert-butyl methyl ether to dissolve and dilute to
5.00 mL; and INJECT it into gas chromatograph for analysis.
5.4 Preparation of standard determination solution of
10 Reagents and materials
Same as those under 3.
11 Instruments and equipment
11.2 Analytical balance. The sensitivity is 0.01 mg and 0.01 g.
11.3 Nitrogen blowing concentrator.
11.4 pH meter. The precision is 0.1.
12 Analytical procedures
12.1 Preparation of samples
Same as that under 5.1.
12.2 Migration test
Same as that under 5.2.
12.3 Derivatization process
12.4 Preparation of standard determination solution of
diaminomethylbezen
Same as that under 5.4.
12.5 Reference conditions for gas chromatography-mass spectrometry
a) Chromatographic column. HP-5 MS. The column length is 30 m. The inner
diameter is 0.25 mm. The film thickness is 0.25 μm. Or chromatographic
column with equivalent performance;
b) Column temperature program. The initial temperature is 60 °C and
maintained for 2 min. At 15 °C/min, the temperature is raised to 240 °C
c) Inlet temperature. 200 °C;
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