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食品安全国家标准 食品接触材料及制品 总迁移量的测定
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GB 31604.8-2021
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标准编号: GB 31604.8-2021 (GB31604.8-2021)
中文名称:
英文名称: Methods of analysis for the evaporated rasidues in the hygienic standard of food containers of plant fibre origin
行业: 国家标准
字数估计: 18,158
发布日期: 2021-09-07
实施日期: 2022-03-07
发布机构: 中华人民共和国国家卫生健康委员会、国家市场监督管理总局
GB 31604.8-2021
Methods of analysis for the evaporated rasidues in the hygienic standard of food containers of plant fibre origin
中华人民共和国国家标准
食品安全国家标准
食品接触材料及制品 总迁移量的测定
2021-09-07发布
2022-03-07实施
中华人民共和国国家卫生健康委员会
国 家 市 场 监 督 管 理 总 局 发 布
食品安全国家标准
食品接触材料及制品 总迁移量的测定
1 范围
本标准规定了食品接触材料及制品总迁移量的测定方法。
本标准适用于食品接触材料及制品总迁移量的测定。
第一部分 水基食品模拟物、化学替代溶剂中总迁移量的测定
2 原理
试样采用水基食品模拟物、化学替代溶剂[如正己烷、异辛烷、95%(体积分数)乙醇溶液、正庚烷],
在选定的迁移试验条件下进行迁移试验,将迁移试验所得浸泡液蒸发并干燥后,扣除相应空白得到试样
向水基食品模拟物、化学替代溶剂迁移的所有非挥发性物质的总量。
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规定的二级水。
3.1 试剂
3.1.1 无水乙醇(C2H6O)。
3.1.2 乙酸(C2H4O2)。
3.1.3 三氯甲烷(CHCl3)。
3.1.4 正己烷(C6H14)。
3.1.5 异辛烷(C8H18)。
3.1.6 95%乙醇。
3.1.7 正庚烷(C7H16)。
3.2 试剂配制
水基食品模拟物的配制:GB 31604.1中水性食品或酒精饮料所对应的4%(体积分数)乙酸溶液、
10%(体积分数)乙醇溶液、20%(体积分数)乙醇溶液、50%(体积分数)乙醇溶液的配制按GB 5009.156
操作。
3.3 材料
3.3.1 蒸发皿:玻璃或陶瓷,50mL~250mL。
3.3.2 玻璃干燥器:配有硅胶或无水氯化钙等干燥剂。
3.3.3 滤纸:定性滤纸,快速。
3.3.4 无尘擦拭纸。
4 仪器和设备
4.1 天平:感量为0.1mg。
4.2 电热恒温干燥箱。
4.3 电热恒温水浴锅或其他电热设备。
5 分析步骤
5.1 迁移试验
食品接触材料及制品按照GB 31604.1和GB 5009.156的要求进行迁移试验。
5.2 水基食品模拟物、化学替代溶剂总迁移量的测定
蒸发皿在使用前,洗净并沥干水分,在100℃±5℃电热恒温干燥箱中烘干2h,然后在干燥器中冷
却0.5h后称重,重复烘干、冷却、称重,直至恒重(即前后两次称量质量差不超过0.5mg),最后一次称
量的质量即为空蒸发皿的质量。
取已恒重的空蒸发皿,向其中加入迁移试验所得浸泡液200mL(若蒸发皿规格低于200mL,则需
分次蒸干),置于不高于各浸泡液沸点温度10℃的水浴上蒸干,将蒸发皿底的水滴用滤纸或无尘擦拭纸
吸去(蒸发皿底不得残留纸纤维),再将蒸发皿置于100℃±5℃电热恒温干燥箱中干燥2h后取出,在
干燥器中冷却0.5h后称量,重复烘干、冷却、称重,直至恒重,最后一次称量的质量即为带有试样蒸发
残渣的蒸发皿质量。带有试样蒸发残渣的蒸发皿质量减去空蒸发皿的质量即为试样测定用浸泡液残渣
的质量。
5.3 三氯甲烷提取物的测定
本测定步骤适用于产品标准中规定需检测三氯甲烷提取物的食品接触材料及制品。
向5.2所得残渣中加入三氯甲烷20mL,润湿残渣,用滤纸过滤,将滤液收集到已恒重的蒸发皿中,
再分别用20mL三氯甲烷对残渣提取两次。然后用少许三氯甲烷冲洗滤纸,滤液并入蒸发皿中,按5.2
步骤蒸干,获得试样测定用浸泡液经三氯甲烷提取的残渣质量。
5.4 空白试验
按5.1、5.2、5.3处理未与食品接触材料及制品接触的水基食品模拟物、化学替代溶剂、三氯甲烷,得
到空白浸泡液的残渣质量、空白浸泡液经三氯甲烷提取的残渣质量。
6 分析结果的表述
6.1 总迁移量计算
6.1.1 以mg/dm2 表示
6.1.1.1 非密封制品类食品接触材料及制品
除盖子、垫圈、连接件等密封制品(以下简称密封制品)以外的食品接触材料及制品,总迁移量结果
以mg/dm2 表示时,按式(1)计算。
9.1.11 硫酸(H2SO4)。
9.2 试剂配制
9.2.1 正戊烷-乙醇(95+5)混合溶液:量取950mL正戊烷,与50mL无水乙醇混匀。
9.2.2 氢氧化钾-甲醇溶液(11.0g/L):称取5.5g(精确到0.1g)氢氧化钾,溶于500mL甲醇中,混匀。
9.2.3 饱和硫酸钠溶液:称取50g(精确到0.1g)无水硫酸钠置于250mL烧杯中,加入100mL水于电
热板上加热煮沸溶解,冷却至室温后,用装有定性滤纸的漏斗过滤到烧杯中。
9.2.4 硫酸溶液(430g/L):称取215g(精确到0.1g)硫酸,缓慢加到盛有约300mL水的烧杯中,边加
边搅拌,待溶液冷却到室温后,转移到500mL容量瓶中,用少量水洗涤烧杯2次~3次,合并洗涤液到
容量瓶中,用水定容。临用现配。在温度为20℃±5℃时,此溶液置于密闭水分含量调节容器中,保持
相对湿度为50%±5%的水分含量调节环境。
9.2.5 硫酸溶液(70g/L):称取35g(精确到0.1g)硫酸,缓慢加到盛有约300mL水的烧杯中,边加边
量瓶中,用水定容。临用现配。在温度为20℃±5℃时,此溶液置于密闭水分含量调节容器中,保持相
对湿度为80%±5%的水分含量调节环境。
9.3 标准品
十七烷酸甘油三酯(C54H104O6,CAS号:2438-40-6):纯度≥98%,或经国家认证并授予标准物质证
书的标准物质。
9.4 标准溶液配制
9.4.1 内标溶液(2.0mg/mL)
准确称取1.0g(精确到0.1mg)十七烷酸甘油三酯,置于100mL烧杯中,加入环己烷溶解,移入
500mL容量瓶中,用环己烷洗涤烧杯3次,洗涤液合并入容量瓶中,用环己烷定容。在4℃冰箱中保
9.4.2 橄榄油标准储备液(100mg/mL)
称取迁移试验所得空白橄榄油5.0g(精确到0.1mg),置于50mL烧杯中,加入正庚烷溶解,移入
50mL容量瓶中,用正庚烷洗涤烧杯3次,洗涤液合并入容量瓶中,用正庚烷定容。临用现配。
9.5 材料
9.5.1 电热板。
9.5.2 密闭水分含量调节容器:如玻璃干燥器。
9.5.3 滤膜:有机相,0.22μm。
9.5.4 滤纸:定性滤纸,快速。
9.5.5 无尘擦拭纸。
10 仪器和设备
10.1 气相色谱:配有氢火焰离子化检测器(FID)。
10.2 分析天平:感量0.1mg、0.1g。
10.3 索氏萃取器。
10.4 低温循环冷凝泵。
10.5 电热恒温水浴锅。
10.6 旋转蒸发仪。
10.7 真空干燥箱。
10.8 恒温恒湿箱。
11.1 试样制备
食品接触材料及制品按GB 31604.1和GB 5009.156的要求进行迁移试验试样制备。全浸没法、填
充法试样制备面积应≥1dm2,测试池法中试样面积以试样实际接触食品模拟物的面积计算,袋装法试
样制备面积应≥2dm2,每份试样可由多个制品制备。试样数量根据以下用途确定:
a) 迁移试验:一次性使用制品至少3份试样;重复使用制品每组试样至少3份试样;
b) 挥发物测定:2份试样;
c) 适宜性判定(见附录A):2份试样;
d) 表面积测定:1份试样;
e) 水分敏感性确认:2份试样。
取2份试样按附录A所述的步骤确定方法适宜性。如果先前的测试已证实方法适宜性,则可略去
附录A步骤。
11.3 试样初始质量的称量
按照附录B或附录C所述步骤确定试样是否为水分敏感性试样。如果先前的测试已证实试样属
于非水分敏感性试样,则可略去附录B或附录C步骤。
若试样为非水分敏感性试样,直接称量初始质量;若试样为水分敏感性试样,则按照相关附录所述
步骤调节水分含量后,得到试样初始质量。若试样采用附录C所述步骤进行水分含量调节在5d内不
能达到恒重时,改用附录B进行水分含量调节。
11.4 迁移试验
同一批次测试样品制备的3组试样上进行试验,每组试样仅迁移试验时间不同。第一组试样迁移试验
时间为按相关标准要求确定的迁移试验时间,第二组试样迁移试验时间为第一组的2倍,第三组试样迁
移试验时间为第一组的3倍。迁移试验平行样数量应满足11.1a)的要求。
11.5 试样最终质量的称量
迁移试验完成后尽快将试样从橄榄油中取出,冷却到室温。将试样放在两张滤纸或无尘擦拭纸中
间,轻轻按压,吸去试样表面的橄榄油。重复按压步骤,直到纸上不出现油斑为止,试样表面不得残留纸
纤维。非水分敏感性试样,直接称量最终质量;水分敏感性试样按11.3中相同的方法进行水分含量调
节后称量最终质量。
11.6 试样挥发物的测定
所述步骤进行迁移试验,非水分敏感性试样,直接称量最终质量;水分敏感性试样按11.3中相同的方法
进行水分含量调节后称量最终质量。
每份平行试样单位面积挥发物质量由试样初始质量与最终质量之差除以相应的取样面积来计算。
如果按附录B所述步骤对试样进行水分含量调节,则可略去此步骤。
11.7 空白试验
按11.4的步骤处理未与食品接触材料及制品接触的橄榄油,用于配制橄榄油标准储备液。
11.8 被试样吸收橄榄油的测定
11.8.1 橄榄油的第一次萃取
萃取溶剂按食品接触材料及制品的食品接触面主体聚合物材质进行选择,主体材质为非极性聚合
采用正戊烷-乙醇(95+5)混合溶液。
向索氏萃取器的收集瓶中加入10.0mL内标溶液(2.0mg/mL)和萃取溶剂,并加入沸石或玻璃珠
以防暴沸。将试样裁切成合适的尺寸,用定性滤纸包好或装入玻璃纤维套桶中(包括裁切过程中产生的
试样碎屑、颗粒等),放入索氏萃取器,回流萃取7h~8h,每小时至少循环6次,并确保每次循环中试样
都完全浸没在溶剂中且保持相互分离。
11.8.2 第一次萃取橄榄油的甲酯化
11.8.2.1 萃取液的转移
所得萃取溶液用旋转蒸发仪或蒸馏装置蒸发至10mL左右并转移至50mL烧瓶中,用萃取溶剂分
3次洗涤收集瓶,并将3次洗涤液合并到烧瓶中,在旋转蒸发仪上蒸干。
移取10.0mL正庚烷将残渣溶解或完全分散,向烧瓶中加入10.0mL氢氧化钾-甲醇溶液
(11.0g/L),并加入沸石或玻璃珠以防暴沸,连接冷凝器,煮沸回流10min±1min。通过冷凝器加入
5.0mL三氟化硼甲醇溶液,回流2min±0.25min。冷却至室温,向烧瓶中加入15mL~20mL饱和硫
酸钠溶液,充分振荡,静置分层后取上层溶液经滤膜过滤,得到待测试液。
11.8.3 橄榄油的第二次萃取和甲酯化
按11.8.1的步骤改用乙醚对试样进行第二次萃取,对乙醚萃取出的橄榄油按11.8.2的步骤进行甲
酯化,得到待测试液。
11.8.4 其他注意事项
若试样第一次萃取出橄榄油质量≤2.0mg,则试样无须用乙醚进行萃取。如果试样用乙醚萃取所
量>10.0mg,则试样需用乙醚再次萃取,或用合适的溶剂将试样溶解或溶胀,必要时用沉淀剂将聚合物
沉淀后取清液,按11.8.2步骤进行甲酯化,得到待测试液。
11.8.5 测定
11.8.5.1 气相色谱参考条件
11.8.5.1.1 非极性柱参考条件
a) 色谱柱:5%苯基-聚二甲基硅氧烷石英毛细管柱,30.0m×250μm×0.25μm,或性能类似的分
析柱;
b) 载气:氮气,流速1.0mL/min;
c) 进样口温度:280℃;
e) 进样体积:1.0μL;
f) 升温程序:初始温度180℃,以20℃/min升温至240℃,再以80℃/min升温至300℃;
g) 检测器温度:250℃;
h) 氢气流速:35mL/min;
i) 空气流速:460mL/min;
j) 尾吹气:氮气,流速25mL/min。
11.8.5.1.2 极性柱参考条件
a) 色谱柱:聚乙二醇石英毛细管柱,30.0m×250μm×0.25μm,或性能类似的分析柱;
b) 载气:氮气,流速1.0mL/min;
d) 进样方式:分流进样,分流比10∶1;
e) 进样体积:1.0μL;
f) 升温程序:初始温度120℃,保持1min,以20℃/min升温至220℃,保持10min;
g) 检测器温度:250℃;
h) 氢气流速:30mL/min;
i) 空气流速:350mL/min;
j) 尾吹气:氮气,流速20mL/min。
11.8.5.2 标准曲线的制作
分别准确移取0.02mL、0.10mL、0.20mL、0.50mL、1.0mL、2.0mL、5.0mL橄榄油标准储备液
按11.8.2.2进行甲酯化获得待测试液。各待测试液中对应的橄榄油质量分别以2.0mg、10mg、20mg、
50mg、100mg、200mg、500mg计。分别吸取上述系列标准待测试液注入气相色谱仪中,按照11.8.5.1
仪器参考条件进行测定,典型色谱图参见附录D。
采用内标法绘制标准曲线,标准待测试液中脂肪酸甲酯与内标峰的峰面积比值为纵坐标,对应橄榄
油质量为横坐标。用极性柱时,纵坐标采用橄榄油所有脂肪酸甲酯(C16∶0、C16∶1、C18∶0、C18∶1、C18∶2)峰
面积之和与内标峰面积的比值;使用非极性柱时,纵坐标采用橄榄油C16、C18峰面积之和与内标峰面积
的比值。
迁移试验温度≥100℃,或迁移试验时间≥10d时,其标准曲线只适用于与迁移试验空白橄榄油在
同一检测周期内、相同迁移试验条件下试样的定量分析。其他迁移试验条件下,当所用橄榄油为同一生
11.8.5.3 试样吸收橄榄油质量的测定
按照11.8.5.1仪器参考条件,将试样待测试液(11.8.2~11.8.4)注入气相色谱仪进行测定。根据标
准曲线计算试样待测试液中橄榄油的质量。
试样吸收的橄榄油总质量为11.8.1~11.8.4所获得的各待测试液中橄榄油质量之和。
11.8.5.4 试样吸收的橄榄油成分变化的判定
使用极性柱时,以C16∶0与内标峰面积的比值对橄榄油质量绘制标准曲线,计算试样每次萃取的橄
榄油质量;以C18∶1与内标峰面积的比值对橄榄油质量绘制标准曲线,计算试样每次萃取的橄榄油质量,
两条标准曲线计算得到的同一试样待测试液中橄榄油质量的差值应≤2mg/dm2。否则,橄榄油不适宜
作为该试样的油脂类食品模拟物。使用非极性柱时,分别采用C16、C18的峰面积按上述方法确认橄榄油
12 分析结果的表述
12.1 以mg/dm2 表示
12.1.1 非密封制品类食品接触材料及制品
非密封制品类食品接触材料及制品的总迁移量结果以mg/dm2 表示时,按式(8)计算。
X8=
m5-(m6-m7)
S -Xb
(8)
式中:
m5---迁移试验前试样的初始质量,单位为毫克(mg);
m6---迁移试验后试样的最终质量,单位为毫克(mg);
m7---迁移试验后试样吸收的橄榄油总质量,单位为毫克(mg);
S ---试样与橄榄油接触的面积,单位为平方分米(dm2);
Xb---迁移试验前后2份试样单位面积挥发物质量平均值,单位为毫克每平方分米(mg/dm2)。
注:假定浸没在橄榄油中的试样单位面积的挥发物质量等于试样单位面积挥发物平均质量。当Xb≤2mg/dm2
时,试样挥发物质量以0计;当Xb>2mg/dm2 时,试样挥发物质量以实际测定值计,以下所有公式同此处。
12.1.2 密封制品类食品接触材料及制品
密封制品类食品接触材料及制品的总迁移量结果以mg/dm2 表示时,按式(9)计算。
m5-(m6-m7)
S -Xb
×
S0+S3
(9)
式中:
X9---密封制品类食品接触材料及制品的总迁移量,单位为毫克每平方分米(mg/dm2);
m5---迁移试验前试样的初始质量,单位为毫克(mg);
m6---迁移试验后试样的最终质量,单位为毫克(mg);
m7---迁移试验后试样吸收的橄榄油总质量,单位为毫克(mg);
S ---试样与橄榄油接触的面积,单位为平方分米(dm2);
Xb---迁移试验前后2份试样单位面积挥发物质量平均值,单位为毫克每平方分米(mg/dm2);
S3---密封制品实际适配容器与食品接触的面积,单位为平方分米(dm2)。
12.2 以mg/kg表示
12.2.1 非密封制品类食品接触材料及制品
非密封制品类食品接触材料及制品的总迁移量结果以mg/kg表示时,按式(10)计算。
X10=X8×F (10)
式中:
X10---非密封制品类食品接触材料及制品的总迁移量,单位为毫克每千克(mg/kg);
X8 ---非密封制品类食品接触材料及制品的总迁移量,单位为毫克每平方分米(mg/dm2);
F ---在可预见使用情形下,食品接触材料及制品实际接触食品的面积与食品质量之间的比值
换算成相应的食品质量。当实际S/V 已知时,F 即为可预见使用情形下的最大S/V;当实
际S/V 未知时,F 采用6dm2/kg,即6dm2 食品接触材料及制品接触1kg食品。
12.2.2 密封制品类食品接触材料及制品
密封制品类食品接触材料及制品的总迁移量结果以mg/kg表示时,按式(11)计算。
X11=
m5-(m6-m7)
S -Xb
×
S0
V3
(11)
式中:
X11---密封制品类食品接触材料及制品的总迁移量,单位为毫克每千克(mg/kg);
m6 ---迁移试验后试样的最终质量,单位为毫克(mg);
m7 ---迁移试验后试样吸收的橄榄油总质量,单位为毫克(mg);
S ---试样与橄榄油接触的面积,单位为平方分米(dm2);
Xb ---迁移试验前后2份试样单位面积挥发物质量平均值,单位为毫克每平方分米(mg/dm2);
S0 ---密封制品实际使用中与食品接触的面积,单位为平方分米(dm2);
V3 ---密封制品实际使用容器盛装食品的质量,各种液态食品密度通常以1kg/L计,将其体积
换算成相应的食品质量,单位为千克(kg)。
12.3 以mg/件表示
密封制品类食品接触材料及制品总迁移量结果以 mg/件表示,按式(12)计算,需注明采用的迁移
X12=
m5-(m6-m7)-Xb×S
(12)
式中:
X12---密封制品类食品接触材料及制品的总迁移量,单位为毫克每件(mg/件);
m5 ---迁移试验前试样的初始质量,单位为毫克(mg);
m6 ---迁移试验后试样的最终质量,单位为毫克(mg);
m7 ---迁移试验后试样吸收的橄榄油总质量,单位为毫克(mg);
Xb ---迁移试验前后2份试样单位面积挥发物质量平均值,单位为毫克每平方分米(mg/dm2);
n ---浸泡密封制品的数量,单位为件。
GB 31604.8-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
Food safety national standard - Food contact materials and products - Determination of total migration
ISSUED ON: SEPTEMBER 07, 2021
IMPLEMENTED ON: MARCH 07, 2022
Issued by: National Health Commission of the People's Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword ... 3
1 Scope ... 4
Part One -- Determination of overall migration in water-based food simulants,
chemical alternative solvents ... 4
2 Principle ... 4
3 Reagents and materials ... 4
4 Instruments and equipment... 5
5 Analysis steps ... 5
6 Expression of analysis results ... 7
7 Precision ... 11
Part Two -- Determination of total migration in olive oil ... 11
8 Principle ... 11
9 Reagents and materials ... 12
10 Instruments and equipment... 14
11 Analysis steps ... 14
12 Expression of analysis results ... 20
13 Precision ... 23
Annex A Suitability Judgment ... 25
Annex B Confirmation of moisture-sensitive specimens and adjustment of
moisture content -- Vacuum drying method ... 26
Annex C Confirmation of moisture-sensitive specimens and adjustment of
moisture content -- Constant humidity method ... 28
Annex D Typical chromatogram ... 30
National Food Safety Standard - Food Contact
Materials and Articles Determination of Overall
Migration
1 Scope
This Standard specifies the methods for determination of overall migration for
food contact materials and articles.
This Standard is applicable to the determination of overall migration for food
contact materials and articles.
Part One -- Determination of overall migration in
water-based food simulants, chemical alternative
solvents
2 Principle
The specimen uses water-based food simulants and chemical alternative
solvents [such as n-hexane, isooctane, 95% (volume fraction) ethanol solution,
n-heptane]. Perform migration test under selected migration test conditions.
Evaporate and dry the soaking liquid obtained from the migration test. After
deducting the corresponding blanks, the total amount of all non-volatile
substances migrated from the specimen to water-based food simulants and
chemical substitute solvents is obtained.
3 Reagents and materials
Unless otherwise specified, the reagents used in this method are analytically
pure, and the water is grade two water specified in GB/T 6682.
3.1 Reagents
3.1.1 Absolute ethanol (C2H6O).
3.1.2 Acetic acid (C2H4O2).
chemical substitute solvents
Wash and drain the evaporating dish before use. Dry for 2h in a 100°C±5°C
electric heating constant temperature drying oven. Then weigh it after cooling
for 0.5h in a desiccator. Repeat drying, cooling, and weighing until constant
weight (that is, the difference in mass between the two weighings does not
exceed 0.5mg). The last weighed mass is the mass of the empty evaporating
dish.
Take an empty evaporating dish with constant weight. Add 200mL of the
soaking solution obtained from the migration test to it (if the evaporating dish
specification is < 200mL, it needs to be evaporated to dryness in batches).
Place it in a water bath that is not higher than the boiling point of each soaking
solution 10°C and evaporate to dryness. Use filter paper or dust-free wipes to
remain at the bottom of the evaporating dish). Then put the evaporating dish in
a 100°C±5°C electric heating constant temperature drying box to dry for 2h.
Take it out. Cool in a desiccator for 0.5h. Weigh it. Repeat drying, cooling, and
weighing until constant weight. The last weighed mass is the mass of the
evaporating dish with specimen evaporation residue. The mass of the
evaporating dish with the evaporation residue of the specimen minus the mass
of the empty evaporating dish is the mass of the soaking solution residue for
the specimen determination.
5.3 Determination of trichloromethane extract
that require the detection of chloroform extracts in the product standard.
Add 20mL of chloroform to the residue obtained in 5.2. Wetting the residue. Use
the filter paper to filter. Collect the filtrate into an evaporating dish with constant
weight. Then use 20mL of chloroform to extract the residue twice respectively.
Use a little chloroform to rinse the filter paper. The filtrate is incorporated into
the evaporating dish. Steam to dry according to step 5.2. Obtain the mass of
the residue extracted with chloroform from the soaking solution for the
specimen determination.
5.4 Blank test
chloroform that are not in contact with food contact materials and articles
according to 5.1, 5.2, and 5.3. Obtain the residue mass of the blank soaking
solution and the residue mass of the blank soaking solution extracted with
chloroform.
X6 - Total migration of product contact materials and articles after chloroform
extraction, in milligrams per square decimeter (mg/dm2);
F - Under foreseeable use cases, the ratio between the area of food contact
materials and articles that actually contact the food and the mass of the food
(S/V), in square decimeter per kilogram (dm2/kg). The density of various liquid
food mass. When the actual S/V is known, F is the maximum S/V under the
foreseeable use case. When the actual S/V is unknown, F uses 6dm2/kg, that
is, 6dm2 of food contact materials and articles contact 1kg of food.
6.3 Correction of results
When GB 31604.1 stipulates the correction factor for fat-containing food
simulants, the determination results of the chemical solvent substitution test
shall be divided by the corresponding correction factor.
6.4 Expression of results
The calculation result of the total migration amount is expressed as the
repeatability condition. The calculation result is accurate to one decimal place.
7 Precision
When the total migration result is ≤ 10.0mg/dm2 or 60.0mg/kg, the difference
between the two independent determination results obtained under
repeatability conditions and the arithmetic mean shall not exceed 1.0mg/dm2 or
6.0mg/kg. The determination result after applying the correction factor shall also
meet this requirement.
When the total migration result is > 10.0mg/dm2 or 60.0mg/kg, the difference
between the two independent determination results obtained under
arithmetic mean. The determination result after applying the correction factor
shall also meet this requirement.
Part Two -- Determination of total migration in olive oil
8 Principle
The specimen uses olive oil as a food simulant. The migration test is carried
out under the selected conditions. The total migration is determined by the
(accurate to 0.1g) potassium hydroxide and dissolve it in 500mL of methanol.
Mix well.
9.2.3 Saturated sodium sulfate solution: Weigh 50g (accurate to 0.1g) of
electric hot plate and boil to dissolve. After cooling to room temperature, use a
funnel equipped with qualitative filter paper to filter into a breaker.
9.2.4 Sulfuric acid solution (430g/L): Weigh 215g (accurate to 0.1g) of sulfuric
acid. Add slowly to a beaker containing about 300mL of water. Stir while adding.
After the solution has cooled to room temperature, transfer to a 500mL
volumetric flask. Wash the beaker with a small amount of water 2 to 3 times.
Combine the washing liquid into the volumetric flask. Use water to set volume.
Prepare it when it is required. When the temperature is 20°C±5°C, the solution
is placed in a closed moisture content adjustment container. Maintain a
9.2.5 Sulfuric acid solution (70g/L): Weigh 35g (accurate to 0.1g) of sulfuric acid.
Add slowly to a beaker containing about 300mL of water. Stir while adding. After
the solution is cooled to room temperature, transfer to a 500mL volumetric flask.
Wash the beaker with a small amount of water 2 to 3 times. Combine the
washing liquid into the volumetric flask. Use water to set volume. Prepare it
when it is required. When the temperature is 20°C±5°C, the solution is placed
in a closed moisture content adjustment container. Maintain a moisture content
adjustment environment with a relative humidity of 80% ± 5%.
9.3 Standard product
≥98%, or standard material certified by the country and awarded with a standard
material certificate.
9.4 Preparation of standard solution
9.4.1 Internal standard solution (2.0mg/mL)
Accurately weigh 1.0g (accurate to 0.1mg) of heptadecanoic acid triglyceride.
Place in a 100mL beaker. Add cyclohexane to dissolve. Transfer to a 500mL
volumetric flask. Wash the beaker 3 times with cyclohexane. The washing liquid
is combined into the volumetric flask. Use cyclohexane to set volume. Store in
a refrigerator at 4°C. The validity period is 1 month.
Weigh 5.0g of blank olive oil obtained from migration test (accurate to 0.1mg).
Place in a 50mL beaker. Add n-heptane to dissolve. Transfer to a 50mL
volumetric flask. Wash the beaker 3 times with n-heptane. The washing liquid
multiple products. The number of specimens is determined according to the
following purposes:
a) Migration test: At least 3 specimens of disposable products; At least 3
specimens per set of specimens for repeated use of articles;
b) Volatile matter determination: 2 specimens;
c) Suitability judgment (see Annex A): 2 specimens;
e) Confirmation of moisture sensitivity: 2 specimens.
11.2 Suitability Judgment
Take 2 specimens to determine the suitability of the method according to the
steps described in Annex A. If the previous test has confirmed the suitability of
the method, it can omit the steps in Annex A.
11.3 Weighing of the initial mass of the specimen
Determine whether the specimen is moisture sensitive according to the steps
described in Annex B or Annex C. If the previous test has confirmed that the
specimen is a non-moisture-sensitive specimen, it can omit the steps in Annex
If the specimen is a non-moisture sensitive specimen, directly weigh the initial
mass. If the specimen is moisture sensitive, after adjusting the moisture content
according to the steps described in the relevant appendix, the initial mass of
the specimen is obtained. If the specimen adopts the steps described in Annex
C to adjust the moisture content and cannot reach a constant weight within 5d,
use Annex B to adjust the moisture content.
11.4 Migration test
The migration test of food contact materials and articles shall be conducted in
accordance with the requirements of GB 31604.1 and GB 5009.156. For
test specimens. Each group of specimens differs only in the migration test time.
The migration test time of the first group of specimens is the migration test time
determined according to the requirements of relevant standards. The migration
test time of the second group of specimens is twice that of the first group. The
migration test time of the third group of specimens is 3 times that of the first
group. The number of parallel specimens for migration test should meet the
requirements of 11.1a).
11.5 Weighing the final mass of the specimen
Remove the specimen from the olive oil as soon as possible after the migration
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