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食品安全国家标准 食品接触材料及制品1,4-丁二醇迁移量的测定
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GB 31604.51-2021
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标准编号: GB 31604.51-2021 (GB31604.51-2021)
中文名称: 食品安全国家标准 食品接触材料及制品1,4-丁二醇迁移量的测定
英文名称: National food safety standard - Food-contact materials and articles - Determination of migration of 1,4-butanediol
行业: 国家标准
中标分类: C53
字数估计: 8,896
发布日期: 2021-02-22
实施日期: 2021-08-22
标准依据: 国家卫生健康委员会公告2021年第3号
GB 31604.51-2021
National food safety standard - Food-contact materials and articles - Determination of migration of 1,4-butanediol
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
1,4-丁二醇迁移量的测定
2021-02-22发布
2021-08-22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
1,4-丁二醇迁移量的测定
1 范围
本标准规定了食品接触材料及制品中1,4-丁二醇迁移量的测定方法。
本标准适用于塑料、涂层、使用粘合剂和油墨的食品接触材料及制品中1,4-丁二醇迁移量的测定。
2 原理
食品接触材料及制品采用食品模拟物或替代溶剂浸泡,1,4-丁二醇迁移到食品模拟物中,测定食品
模拟物中1,4-丁二醇的迁移量。水性、酸性和酒精类食品模拟物经甲醇稀释后检测,油脂类食品模拟
物经甲醇萃取后检测。试液通过气相色谱柱分离,采用配置氢火焰离子化检测器(FID)的气相色谱仪
检测,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规定的一级水。
3.1 试剂
3.1.1 橄榄油:须符合GB 5009.156中附录A的要求。
3.1.2 乙酸 (C2H4O2)。
3.1.3 乙醇 (C2H6O)。
3.1.4 甲醇 (CH4O)。
3.1.5 丙酮 (C3H6O)。
3.2 试剂配制
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
醇溶液和95%(体积分数)乙醇溶液的配制按GB 5009.156操作。
3.3 标准品
1,4-丁二醇(C4H10O2,CAS号:110-63-4),纯度大于99%,经国家认证并授予标准物质证书的标准品。
3.4 标准溶液配制
3.4.1 储备液(1000mg/L)
准确称取50mg(精确到0.1mg)的1,4-丁二醇标准物质,甲醇溶解后转移到50mL容量瓶中,甲
醇准确定容至刻度,充分摇匀后,静置,存储于玻璃试剂瓶中。此溶液在0℃~4℃冰箱中保存,有效期
为3个月。
3.4.2 标准中间液1(10mg/L)
准确移取1.00mL1,4-丁二醇标准储备液(3.4.1)到100mL容量瓶中,甲醇定容到刻度,摇匀,静
置,现配现用。
3.4.3 标准中间液2
分别准确移取0.40mL、0.80mL、1.20mL、1.60mL、2.00mL和4.00mL储备液(3.4.1)于6个
10mL容量瓶中,丙酮定容,摇匀,静置,得到质量浓度分别为40 mg/L、80 mg/L、120 mg/L、
160mg/L、200mg/L和400mg/L的标准中间液,现配现用。
3.4.4 标准工作溶液
3.4.4.1 标准工作溶液[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
和50%(体积分数)乙醇溶液]
分别准确移取标准中间溶液1(3.4.2)0.20mL、0.40mL、0.60mL、0.80mL、1.00mL和2.00mL于
6个10mL容量瓶中,分别准确加入2.0mL对应的食品模拟物,甲醇准确定容至刻度,充分摇匀后,静
置。得到质量浓度分别为0.20mg/L、0.40mg/L、0.60mg/L、0.80mg/L、1.00mg/L和2.00mg/L的
标准工作溶液,现配现用。
3.4.4.2 标准工作溶液(油脂类食品模拟物)
分别准确称取2.0g(精确到0.001g)油脂类食品模拟物橄榄油于6个具塞离心管中,分别加入6个
不同质量浓度的油脂类食品模拟物标准中间溶液2(3.4.3)各50μL,充分摇匀后静置,得到质量浓度分
别为1.0mg/kg、2.0mg/kg、3.0mg/kg、4.0mg/kg、5.0mg/kg和10.0mg/kg的标准工作溶液,分别加
入2.00mL甲醇溶液萃取,混匀,离心分层,取上层溶液通过0.45μm滤膜后待测。
3.4.4.3 标准工作溶液[替代溶剂(95%乙醇)]
分别准确移取标准中间溶液1(3.4.2)0.20mL、0.40mL、0.60mL、0.80mL、1.00mL和2.00mL于
6个10mL容量瓶中,分别准确加入2.0mL95%乙醇食品模拟物,甲醇准确定容至刻度,充分摇匀后,
静置,得到质量浓度分别为0.20mg/L、0.40mg/L、0.60mg/L、0.80mg/L、1.00mg/L和2.00mg/L的
标准工作溶液,现配现用。
4 仪器和设备
4.1 气相色谱仪:配置氢火焰离子化检测器(FID)。
4.2 分析天平:感量0.1mg和感量1mg。
4.3 有机相微孔滤膜:0.45μm。
4.4 离心机:最高转速>3000r/min。
5 分析步骤
5.1 试液的制备
5.1.1 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。迁移试验所得浸泡
液如不能立即测试,应置于4℃冰箱中避光保存。若进行下一步试验,应将浸泡液恢复至室温后使用。
5.1.2 浸泡液的处理
5.1.2.1 浸泡液的处理[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)]
准确移取迁移试验中得到的浸泡液5.00mL于25mL容量瓶中,加入甲醇准确定容至刻度,充分
摇匀后,静置待测。
5.1.2.2 油脂类食品模拟物的处理
准确称取迁移试验中得到的油脂类食品模拟物橄榄油2.0g(精确到0.001g)于具塞试管中,加入
5.1.2.3 替代溶剂(95%乙醇)浸泡液的处理
准确移取迁移试验中得到的替代溶剂(95%乙醇)浸泡液5.00mL于25mL容量瓶中,加入甲醇准
确定容至刻度,充分摇匀后,静置,待测。
5.1.3 空白试液的制备
按5.1.1和5.1.2处理未与食品接触材料及制品接触的食品模拟物、替代溶剂。
5.2 仪器参考条件
5.2.1 色谱柱:聚乙二醇气相色谱柱:30m×0.32mm×0.25μm(或等效色谱柱)。
5.2.2 进样口温度:250℃(不分流进样)。
5.2.3 进样量:1μL。
5.2.5 流速:1mL/min。
5.2.6 检测器(FID)温度:260℃;氢气流量:30mL/min;空气流量:400mL/min。
5.3 标准曲线的绘制
按照5.2所列的仪器参考条件,对标准工作溶液进行测定。以标准工作溶液中1,4-丁二醇的质量
浓度为横坐标,以对应的峰面积的响应值为纵坐标,绘制标准曲线。1,4-丁二醇在食品模拟物标准溶液
的参考色谱图见附录A。
5.4 试液的测定
按照5.3所列的仪器参考条件,分别将试样溶液(5.1.2)和空白溶液(5.1.3)进行测定,得到目标物峰
面积,从标准曲线计算试样溶液、空白溶液中1,4-丁二醇的含量c、c0。空白溶液中1,4-丁二醇的含量
注:由于试样含少量水,建议根据实际检测情况定期维护设备。
6 分析结果的表述
6.1 食品接触材料及制品1,4-丁二醇特定迁移量的计算(以mg/kg表示)
食品接触材料及制品1,4-丁二醇特定迁移量以mg/kg表示时,按式(1)计算。
X=
c-c0()×V1
S1 ×
S2
V2
式中:
X ---1,4-丁二醇的特定迁移量,单位为毫克每千克(mg/kg);
c ---试样浸泡液中1,4-丁二醇的含量,单位为毫克每升(mg/L)或毫克每千克(mg/kg);
c0 ---空白浸泡液中1,4-丁二醇的含量,单位为毫克每升(mg/L)或毫克每千克(mg/kg);
V1 ---迁移试验使用模拟物的体积或质量,单位为升(L)或千克(kg);
S1 ---迁移试验中试样与模拟物接触的面积,单位为平方分米(dm2);
S2 ---试样实际使用中与食品接触的面积,单位为平方分米(dm2);
V2 ---试样实际使用中接触食品的体积或质量,单位为千克(kg);各种液态食品通常按密度为
1kg/L将其体积换算为相应的质量。
进行计算。
结果至少保留2位有效数字。
6.2 密封用制品类食品接触材料及制品1,4-丁二醇特定迁移量的计算(以mg/件表示)
当预期用途未知时,密封制品类食品接触材料及制品1,4-丁二醇特定迁移量以 mg/件表示时,按
式(2)计算,需注明采用的迁移试验方法、迁移试验中单个密封制品与食品模拟物接触的面积。
X=
(c-c0)×V
(2)
式中:
c ---试样浸泡液中1,4-丁二醇的含量,单位为毫克每升(mg/L)或毫克每千克(mg/kg);
c0 ---空白浸泡液中1,4-丁二醇的含量,单位为毫克每升(mg/L)或毫克每千克(mg/kg);
V ---试样浸泡液的体积或质量,单位为升(L)或千克(kg);
n ---浸泡用密封制品的数量,单位为件。
结果至少保留2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20%。
8 其他
本方法的检出限为0.3mg/kg,定量限1.0mg/kg。当迁移试验中S/V 与实际使用情形下S/V 相
1.0mg/kg;当迁移试验中S/V 与实际使用情形下S/V 不同时,本方法1,4-丁二醇对各食品模拟物、化
学替代溶剂中1,4-丁二醇的检出限和定量限按第6章进行计算。
GB 31064.51-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard - Food contact material
and products - Determination of migration of 1,4-
butanediol
ISSUED ON: FEBRUARY 22, 2021
IMPLEMENTED ON: AUGUST 22, 2021
Issued by: National Health Commission of PRC;
State Administration for Market Regulation.
Table of Contents
1 Scope ... 3
2 Principle ... 3
3 Reagents and materials ... 3
4 Instrument and equipment ... 5
5 Analytical procedures ... 5
6 Expression of analysis results ... 7
7 Precision ... 9
8 Others ... 9
Appendix A Chromatogram of 1,4-butanediol standard solution ... 10
National food safety standard - Food contact material
and products - Determination of migration of 1,4-
butanediol
1 Scope
This standard specifies the method for determining the migration of 1,4-
butanediol in food contact materials and products.
This standard applies to the determination of migration of 1,4-butanediol, in
plastics, coatings, food contact materials and products, which use adhesives
and inks.
2 Principle
Food contact materials and products are immersed in food simulants OR
alternative solvents. The 1,4-butanediol migrates into the food simulants. The
migration amount of 1,4-butanediol in the food simulants is determined. For the
water-based, acidic and alcoholic food simulants, it is tested after being diluted
by methanol. For the oily food simulants, it is tested after being extracted by
methanol. The test solution is separated by a gas chromatographic column;
detected by a gas chromatograph, which is equipped with a flame ionization
detector (FID). The retention time is used for qualitative, whilst the external
standard method is used for quantification.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are all analytically
pure; the water is the grade 1 water, as specified in GB/T 6682.
3.1 Reagents
3.1.1 Olive oil: It must meet the requirements of Appendix A in GB 5009.156.
3.1.2 Acetic acid (C2H4O2).
3.1.3 Ethanol (C2H6O).
standard intermediate solution 1 (3.4.2), into six 10 mL volumetric flasks.
Respectively, accurately add 2.0 mL of corresponding food simulants. Use
methanol to make its volume accurately reach to the mark. Shake well. Let
stand. It gets the standard working solutions, which have mass concentrations
of 0.20 mg/L, 0.40 mg/L, 0.60 mg/L, 0.80 mg/L, 1.00 mg/L, 2.00 mg/L. Prepare
it before use.
3.4.4.2 Standard working solution (oily food simulant)
Respectively, accurately weigh 2.0 g (accurate to 0.001 g) of oily food simulant
(olive oil) into six centrifuge tubes with stoppers. Respectively add 50 μL of 6
standard intermediate solution 2 (3.4.3) of oily food simulant, at different mass
concentrations. Shake well. Let it stand, to obtain standard working solutions,
which have mass concentrations of 1.0 mg/kg, 2.0 mg/kg, 3.0 mg/kg, 4.0 mg/kg,
5.0 mg/kg, 10.0 mg/kg. Respectively add 2.00 mL of methanol solution for
extraction. Mix well. Centrifuge for layering. Take the upper layer solution. Make
it pass through a 0.45 μm filter membrane. Prepare for testing.
3.4.4.3 Standard working solution [Alternative solvent (95% ethanol)]
Accurately pipette 0.20 mL, 0.40 mL, 0.60 mL, 0.80 mL, 1.00 mL, 2.00 mL of
standard intermediate solution 1 (3.4.2), into six 10 mL volumetric flasks.
Respectively, accurately add 2.0 mL of 95% ethanol food simulant. Use
methanol to make its volume reach accurately to the mark. Shake it well. Let it
stand, to obtain the standard working solution, which has mass concentrations
of 0.20 mg/L, 0.40 mg/L, 0.60 mg/L, 0.80 mg/L, 1.00 mg/L, 2.00 mg/L,
respectively. Prepare it before use.
4.1 Gas chromatograph: It is equipped with hydrogen flame ionization detector
(FID).
4.2 Analytical balance: The sensitivity is 0.1 mg and 1 mg.
4.3 Organic phase microporous filter membrane: 0.45 μm.
4.4 Centrifuge: The maximum speed is > 3000 r/min.
5 Analytical procedures
5.1 Preparation of test solution
5.1.1 Migration test
5.2.5 Flow rate: 1 mL/min.
flow rate: 400 mL/min.
5.3 Drawing of standard curve
Determine the standard working solution, in accordance with the instrument
reference conditions, which are listed in 5.2. Use the mass concentration of 1,4-
butanediol in the standard working solution, as the abscissa, AND the response
value of the corresponding peak area, as the ordinate, to draw the standard
curve. Refer to Appendix A for the reference chromatogram of 1,4-butanediol,
in the food simulant standard solution.
5.4 Determination of test solution
solution (5.1.2) and the blank solution (5.1.3) are respectively determined, to
obtain the peak area of the target object. From the standard curve, calculate
the content of the 1,4-butanediol, c and c0, in the sample solution and the blank
solution. The content of the 1,4-butanediol, c0, in the blank solution shall not be
higher than the mass concentration of the method detection limit.
Note: As the specimen contains a small amount of water, it is recommended to
maintain the equipment regularly, based on actual testing conditions.
6 Expression of analysis results
6.1 Calculation of specific migration of 1,4-butanediol in food contact
When the specific migration of 1,4-butanediol in food contact materials and
products is expressed in mg/kg, it is calculated according to formula (1).
Where:
X - The specific migration of 1,4-butanediol, in milligrams per kilogram
(mg/kg);
c - The content of 1,4-butanediol in the specimen soaking solution, in
milligrams per liter (mg/L) or milligrams per kilogram (mg/kg);
c0 - The content of 1,4-butanediol in the blank soaking solution, in milligrams
per liter (mg/L) or milligrams per kilogram (mg/kg);
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