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食品安全国家标准 食品接触材料及制品 己内酰胺的测定和迁移量的测定
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GB 31604.19-2016
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标准编号: GB 31604.19-2016 (GB31604.19-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 己内酰胺的测定和迁移量的测定
英文名称: Determination of 6-caprolactam in nylon 6 resin and its products
行业: 国家标准
中标分类: X09
字数估计: 8,886
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2283-2009; GB/T 5009.125-2003; GB/T 23296.20-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.19-2016: 食品安全国家标准 食品接触材料及制品 己内酰胺的测定和迁移量的测定
GB 31604.19-2016 英文名称: Determination of 6-caprolactam in nylon 6 resin and its products
1 范围
本标准规定了食品接触材料及制品中己内酰胺的测定方法和迁移量的测定方法。
本标准适用于食品接触材料及制品中己内酰胺的测定和迁移量的测定。
己内酰胺的测定
2 原理
试样经水提取后,己内酰胺溶解在提取液中,经滤膜过滤后用配有紫外检测器的高效液相色谱仪进
行检测,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
乙腈(C2H3N,CAS号:75-05-8):色谱纯。
3.2 标准品
3.2.1 己内酰胺(C6H11NO,CAS号:105-60-2):纯度≥99%,或经国家认证并授予标准物质证书的标
准物质。
3.3 标准溶液配制
3.3.1 己内酰胺标准储备液
称取100mg(精确至0.0001g)己内酰胺,用水溶解后,定容至100mL,配制成浓度为1000mg/L
的储备液。溶液在4℃下避光密封储存,有效期为1个月。
3.3.2 己内酰胺中间标准溶液
用刻度吸量管吸取0.05mL、0.25mL、0.5mL、1.0mL、2.5mL、5.0mL己内酰胺标准储备液于6
个10mL容量瓶中,用水定容,得到己内酰胺浓度为5.0mg/L、25.0mg/L、50.0mg/L、100.0mg/L、
250.0mg/L、500.0mg/L的中间标准溶液。溶液储存方式同3.3.1。
3.3.3 己内酰胺标准工作溶液
分别准确吸取1.0mL己内酰胺中间标准溶液于6支10mL具塞玻璃试管中,分别加入4.0mL水
混匀,获得己内酰胺标准工作溶液。其中,己内酰胺浓度分别为1.0mg/L、5.0mg/L、10.0mg/L、
20.0mg/L、50.0mg/L、100.0mg/L。溶液储存方式同3.3.1。
4 仪器和设备
4.1 高效液相色谱仪:配备紫外检测器(UV)。
4.2 冷冻研磨仪。
4.3 分析天平:感量0.0001g。
4.4 具塞玻璃试管:10mL。
4.5 0.45μm微孔滤膜。
4.6 恒温水浴锅。
5 分析步骤
5.1 试样处理
先将试样用冷冻研磨仪或剪刀等其他切割工具将其破碎成粒径小于1mm×1mm后再称量。切
割样品时,不可使其发热变软。
5.2 试样溶液的制备
称取粉碎样品1.0g(精确到0.0001g)于具塞玻璃试管中,加入10mL水后在沸水浴中提取
40min,放冷至室温,然后取上层清液置于25mL容量瓶中。再用10mL水按照上述方式提取1次,并
合并两次清液后,用水定容至刻度,取1mL提取液通过0.45μm滤膜过滤后供高效液相色谱进样。若
样品溶液浓度超出线性范围,使用水适当稀释,使其浓度处于线性范围内。
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 色谱参考条件
5.4.1 色谱柱:C18柱,柱长250mm,内径4.6mm,粒径5μm。
5.4.2 检测器:紫外检测波长210nm。
5.4.3 流动相:乙腈-水(20+80)。
5.4.4 流速:1.0mL/min。
5.4.5 进样体积:10μL。
5.5 标准曲线的制作
按照5.4所列测定条件,分别将己内酰胺标准工作溶液进液相色谱仪测定。以标准工作溶液中己
内酰胺浓度为横坐标,单位为毫克每升(mg/L),以对应己内酰胺峰面积为纵坐标,制作标准工作曲线。
标准色谱图参见图A.1。
5.6 试样溶液的测定
按照5.4所列条件,将试样溶液(5.2)及空白溶液(5.3)进液相色谱仪测定,得到己内酰胺峰面积,扣
除空白值。
6 分析结果的表述
试样中己内酰胺含量按式(1)计算:
X=ρ×
V×f×10-3
m×10-3
(1)
式中:
X ---试样中己内酰胺的含量,单位为毫克每千克(mg/kg);
ρ ---依据校准曲线获得的试样溶液中己内酰胺的浓度,单位为毫克每升(mg/L);
V ---试样溶液体积,单位为毫升(mL);
f ---浓度稀释因子;
10-3---单位换算因子;
m ---试样称样量,单位为克(g)。
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其算术平均值的10%。
8 其他
方法检出限为10mg/kg、方法定量限为25mg/kg。
己内酰胺迁移量的测定
9 原理
样品经浸泡后,水基、酒精、酸性食品模拟物中的己内酰胺直接通过高效液相色谱分离,采用紫外检
10 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。
10.1 试剂
10.1.1 乙腈(C2H3N,CAS号:75-05-8):色谱纯。
10.1.2 乙醇(C2H6O,CAS号:64-17-5)。
10.1.3 正己烷(C6H14,CAS号:110-54-3)。
10.1.4 水基、酸性、酒精、油基食品模拟物:所用试剂依据GB 31604.1规定。
10.2 试剂配制
10.2.1 乙醇-水溶液(1+2):量取100mL乙醇和200mL水,混匀。
10.3 标准品
10.3.1 己内酰胺(C6H11NO,CAS号:105-60-2):纯度≥99%,或经国家认证并授予标准物质证书的标
准物质。
10.4 标准溶液配制
10.4.1 己内酰胺标准储备液
称取100mg(精确至0.0001g)己内酰胺,用水溶解后,定容至100mL,配制成浓度为1000mg/L
的储备液。溶液在4℃下避光密封储存,有效期为1个月。
10.4.2 己内酰胺标准溶液
用刻度吸量管吸取0.05mL、0.25mL、0.5mL、1.0mL、2.5mL、5.0mL己内酰胺储备液于10mL
250.0mg/L、500.0mg/L的标准溶液。溶液储存方式同10.4.1。
10.4.3 水基、酸性、酒精类食品模拟物标准工作溶液
用刻度吸量管吸取1.0mL己内酰胺标准溶液于6支10mL具塞玻璃试管中,分别加入4.0mL水
基食品模拟物,混匀,获得水基食品模拟物标准工作溶液。其中,己内酰胺浓度分别为1.0mg/L、
5.0mg/L、10.0mg/L、20.0mg/L、50.0mg/L、100.0mg/L。采用同样方式,分别用酸性、酒精类食品
模拟物配制同样浓度的己内酰胺标准工作溶液。
10.4.4 油基食品模拟物标准工作溶液
分别称取8.0g橄榄油(精确到0.01g),置于6个分液漏斗中,分别加入1.6mL己内酰胺标准溶
液,混匀,使得油基模拟物中己内酰胺浓度为1.0mg/kg、5.0mg/kg、10.0mg/kg、20.0mg/kg、
10min,静置30min使两相分层,移取5mL下层水溶液,经脱脂棉与0.45μm微孔滤膜过滤后待测。
11 仪器和设备
11.1 高效液相色谱法:配备紫外检测器(UV)。
11.2 分析天平:感量0.0001g。
11.3 具塞玻璃试管:10mL。
11.4 0.45μm微孔滤膜。
11.5 恒温水浴锅。
12 分析步骤
12.1 试样迁移试验
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。
GB 31604.19-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Food contact materials and products -
Determination of caprolactam and migration quantity
ISSUED ON. OCTOBER19, 2016
IMPLEMENTED ON. APRIL19, 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 .. 5
5 Analytical procedures .. 5
6 Analysis results expression . 7
7 Precision . 7
8 Others .. 7
9 Principles .. 7
10 Reagents and materials . 8
11 Instrument and equipment .. 9
12 Analytical procedures .. 9
13 Analysis results expression .. 11
14 Precision .. 11
15 Others . 11
Appendix A Liquid chromatogram of standard solution .. 12
National food safety standard -
Food contact materials and products -
Determination of caprolactam and migration quantity
1 Scope
This standard specifies determination method of caprolactam and migration
quantity in food contact materials and products.
This standard applies to determination of caprolactam and migration quantity in
food contact materials and products.
Determination of caprolactam
2 Principles
After the sample is extracted by water, the caprolactam is dissolved in extracting
solution; after filtered through filter membrane, it is detected by a high-
performance liquid chromatograph (HPLC) that is equipped with an ultraviolet
detector; use external standard method to quantify.
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.
3.1 Reagents
Acetonitrile (C2H3N, CAS No. 75-05-8). Chromatographically pure.
3.2 Standards
3.2.1 Caprolactam (C6H11NO, CAS number. 105-60-2). Purity ≥ 99%, or
standard substance which is identified by national authentication and awarded
a reference material certificate.
3.3 Standard solution preparation
5.2 Preparation of sample solution
WEIGH 1.0 g (accurate to 0.0001g) of crushed samples; PLACE it into a
stoppered glass tube; after adding 10 mL of water, EXTRACT for 40 min in a
boiling water bath; when cooling to room temperature, TAKE the supernatant
into 25 mL volumetric flask. Then USE 10 mL of water to extract once again as
above; COMBINE the twice-supernatant; USE water to dilute it to the mark;
TAKE 1 mL of extracting solution through 0.45 μm filter membrane; after filtering,
it is for sample injection of high performance liquid chromatography. If the
concentration of the sample solution is beyond linear range, use water to dilute
it so that the concentration is within linear range.
5.3 Preparation of blank solution
Except for not adding sample, use the same analytical procedures, reagents
and dosage as 5.2.
5.4 Reference conditions of chromatography
5.4.1 Chromatographic column. C18-column, column-length 250 mm, inner-
diameter 4.6 mm, particle-size 5 μm.
5.4.2 Detector. UV detection wavelength 210 nm.
5.4.3 Mobile phase. acetonitrile-water (20+80).
5.4.5 Injection volume. 10 μL.
5.5 Drawing of standard curve
According to the measurement conditions listed in 5.4, respectively PLACE
caprolactam standard working solution into liquid chromatograph to determine.
With the caprolactam concentration of standard working solution as abscissa,
in milligrams per liter (mg/L), AND the corresponding peak area of caprolactam
as vertical axis, DRAW a standard working curve. See Figure A.1 for the
standard chromatogram.
5.6 Determination of sample solution
the blank solution (5.3) into liquid chromatograph to determine; OBTAIN the
peak area of caprolactam; DEDUCT blank value.
simulant test solution can not be immediately carried out the next test, the food
simulant test solution shall be stored in refrigerator at 4 °C.
The resulting food simulant test solution shall be cooled or returned to room
temperature before proceeding to the next test.
12.2 Preparation of sample solution
12.2.1 Processing of food simulants that are water-based, acidic and
alcoholic
acidic and alcoholic obtained from the migration test; FILTER through 0.45 μm
microporous membrane to wait for determining.
12.2.2 Processing of oil-based food simulants
WEIGH 8.0 g (accurate to 0.01g) of olive oil obtained from the migration test;
PLACE it into separatory funnel; ADD 1.6 mL of water; MIX it uniformly; ADD
15 mL of n-hexane; MIX it uniformly; ADD 8 mL of ethanol-water solution (1+2);
VIBRATE it for 10 min; LET it stand for 30 min to separate the two-phase; MOVE
5 mL of lower-layer water solution; FILTER through cotton wool and 0.45 μm
microporous membrane to wait for determining.
Except for not adding sample, use the same analytical procedures, reagents
and dosage as 12.2.
12.4 Reference conditions of chromatography
12.4.1 Chromatographic column. C18-column, column-length 250 mm, inner-
diameter 4.6 mm, particle-size 5 μm.
12.4.2 Detector. UV detection wavelength 210 nm.
12.4.3 Mobile phase. acetonitrile-water (20+80).
12.4.4 Flow rate. 1.0 mL/min.
12.4.5 Injection volume. 10 μL.
According to the conditions listed in 12.4, respectively PLACE standard working
solution of food simulants that are water-based, acidic and alcoholic, and
standard working solution of oil-based food simulants into liquid chromatograph
to determine. With the caprolactam concentration of food simulants as abscissa,
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