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食品安全国家标准 食品接触材料及制品 醋酸乙烯酯迁移量的测定
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GB 31604.20-2016
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标准编号: GB 31604.20-2016 (GB31604.20-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 醋酸乙烯酯迁移量的测定
英文名称: Food contact materials -- Polymer materials -- Determination of vinyl acetate in food stimulants by gas chromatography/mass spectrometry
行业: 国家标准
中标分类: X09
字数估计: 8,838
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2333-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.20-2016: 食品安全国家标准 食品接触材料及制品 醋酸乙烯酯迁移量的测定
GB 31604.20-2016 英文名称: Food contact materials -- Polymer materials -- Determination of vinyl acetate in food stimulants by gas chromatography/mass spectrometry
1 范围
本标准规定了食品接触材料及其制品醋酸乙烯酯迁移量的测定方法。
本标准适用于食品接触材料及制品中醋酸乙烯酯迁移量的测定。
2 原理
试样中醋酸乙烯酯经食品模拟浸泡液浸出后,用丙酮定容,最后气相色谱测定,外标法定量。样本
一经检出需要气相色谱-质谱法确证。
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 丙酮(C3H6O):不含醋酸乙烯酯。
3.1.2 甲醇(C2H4O)。
3.1.3 水基、酸性、酒精类、油基食品模拟物:所用试剂依据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操作。
3.2.2 甲醇-水混合液(1+1):量取100mL甲醇和100mL水,混匀。
3.3 标准品
醋酸乙烯酯(C4H6O2,CAS号:108-05-4):纯度≥99%,或经国家认证并授予标准物质证书的标准
物质。
3.4 标准溶液配制
3.4.1 醋酸乙烯酯标准贮备溶液(1000mg/L):准确称取醋酸乙烯酯标准品10mg(精确至0.01mg)
于10mL容量瓶中,用丙酮溶解稀释到刻度线,-10℃密封保存。
3.4.2 醋酸乙烯酯标准中间溶液(100mg/L):吸取1.0mL醋酸乙烯酯贮备液于10mL容量瓶中,用
丙酮稀释到刻度线,使用当天配制。
4 仪器和设备
4.1 气相色谱仪:配有FID检测器。
4.2 气相色谱-质谱仪:配有EI离子源。
4.3 分析天平:感量0.1mg、0.01g。
4.4 微量注射器:10μL、50μL、1000μL。
4.5 超声振荡器。
4.6 0.2μm尼龙滤膜针式过滤器。
5 分析步骤
5.1 样品迁移试验
按照GB 5009.156及GB 31604.1的要求,对样品进行迁移试验,得到食品模拟物试液。如果得到
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。
应将所得食品模拟物试液冷却或恢复至室温后进行下一步试验。
5.2 水基、酸性食品、酒精、油基类食品模拟物标准工作溶液的制备
准确吸取醋酸乙烯酯标准中间溶液0mL、0.01mL、0.05mL、0.1mL、0.5mL、1.0mL于10mL容
量瓶中,用丙酮定容,得到醋酸乙烯酯浓度分别为0.00mg/L、0.1mg/L、0.5mg/L、1.0mg/L、
5.0mg/L、10.0mg/L的标准工作液。采用同样方式,分别得到对应水基、酸性食品、酒精类、油基类食
品模拟物标准工作溶液。
5.3 气相色谱仪器参考条件
气相色谱仪器参考条件列出如下:
a) 色谱柱:DB-5石英毛细管柱,柱长30m,内径0.32mm,膜厚0.25μm,或相当者;
b) 程序升温:35 ℃(保持5min),以5 ℃/min升至50 ℃,以40 ℃/min升至250 ℃(保
持2min);
c) 进样口温度:250℃;
d) 进样方式:分流进样(10∶1),进样量为1μL;
e) 检测器温度:300℃;
f) 载气(N2)流速:0.5mL/min;
g) 氢气流速:30mL/min;
h) 空气流速:400mL/min。
5.4 测定
5.4.1 试样测定
取干净、干燥的25mL容量瓶,加入1g(精确至0.0001g)经过迁移实验的模拟食品浸泡液,用丙
酮定容至刻度,充分混匀后备用。
用微量注射器分别吸取一定量的上述试液注入气相色谱仪中,按照上述气相色谱条件,各重复测定
两次,醋酸乙烯酯的气相色谱图参见图A.1。
5.4.2 空白试验
空白试验系指除不加试样外,采用完全相同的分析步骤、试剂和用量,进行平行操作。
6 分析结果的表述
由标准曲线得到试样溶液中醋酸乙烯酯的浓度,按GB 5009.156进行迁移量计算,得到食品接触材
料及制品中醋酸乙烯酯的迁移量。计算结果保留至小数点后两位。
7 确证试验
当上述结果超过特定迁移量值(SML)时,可采用气相色谱-质谱联用法或其他有效方法进行确证。
气相色谱-质谱联用法分析参考条件及色谱图参见附录B和附录C。
8 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%。
9 其他
方法检出限为0.1mg/kg,定量限为0.5mg/kg。
GB 31604.20-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Food contact materials and products -
Determination of vinyl acetate migration quantity
ISSUED ON. OCTOBER19, 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 .. 5
5 Analytical procedures .. 5
6 Analysis results expression . 7
7 Confirmatory test .. 7
8 Precision . 7
9 Others .. 7
Appendix A Vinyl acetate gas chromatogram .. 8
Appendix B Gas chromatography-mass spectrometry confirmation reference
conditions .. 9
Appendix C Vinyl acetate chromatography-mass spectrometry diagram .. 11
National food safety standard -
Food contact materials and products -
Determination of vinyl acetate migration quantity
1 Scope
This standard specifies determination method of vinyl acetate migration
quantity in food contact materials and products.
This standard applies to determination of vinyl acetate migration quantity in food
contact materials and products.
2 Principles
In the sample, after the vinyl acetate is leached from the food simulation soaking
solution, use acetone to dilute it, and finally use gas chromatography to
determine and external standard method to quantify. Once the sample is
detected, it must be confirmed by gas chromatography - mass spectrometry.
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. The containers
and transfer apparatuses in the test shall avoid using plastic materials.
3.1 Reagents
3.1.1 Acetone (C3H6O). It does not contain vinyl acetate.
3.1.2 Methanol (C2H4O).
3.1.3 Water-based, acidic, alcoholic, oil-based food simulants. The reagents
used are in accordance with the provisions of GB 31604.1.
3.2 Reagent preparation
3.2.1 Water-based, acidic, alcoholic, oil-based food simulants. Operate
according to GB 5009.156.
5.2 Preparation of standard working solution of food simulants that are
water-based, acidic food, alcoholic, and oil-based
Accurately PIPETTE 0 mL, 0.01 mL, 0.05 mL, 0.1 mL, 0.5 mL, 1.0 mL of vinyl
acetate standard intermediate solution into 10 mL volumetric flask; USE
acetone to dilute it; OBTAIN standard working solution with vinyl acetate
concentration of 0.00 mg/L, 0.1 mg/L, L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 10.0
mg/L, respectively. In the same way, OBTAIN standard working solution of food
simulants that are water-based, acidic food, alcoholic, and oil-based.
5.3 Gas chromatograph (GC) reference conditions
The GC reference conditions are listed below.
a) Chromatographic column. DB-5 quartz capillary column, column length 30
m, inner diameter 0.32 mm, film thickness 0.25 μm, or equivalent;
b) Temperature programming. 35 °C (keep for 5 min), rising from 5 °C/min to
50 °C, rising from 40 °C/min to 250 °C (keep for 2 min);
c) Inlet temperature. 250 °C;
d) Injection mode. split injection (10.1), injection volume is 1 μL;
e) Detector temperature. 300 °C;
f) Carrier gas (N2) flow rate. 0.5 mL/min;
g) Hydrogen flow rate. 30 mL/min;
h) Air flow rate. 400 mL/min.
5.4.1 Sample determination
TAKE a clean and dry 25 mL volumetric flask; ADD 1 g (accurate to 0.0001 g)
of simulated food soaking solution after migration experiment; USE acetone to
dilute it to the mark; MIX it uniformly for spare-use. USE micro-syringe to pipette
respectively a certain amount of the above test solution; INJECT it into gas
chromatograph. According to the above gas chromatographic conditions,
REPEAT the determination twice. The gas chromatogram of vinyl acetate is
shown in Figure A.1.
5.4.2 Blank Test
analytical procedure, reagents and dosage, carry out parallel operation.
Appendix B
Gas chromatography-mass spectrometry confirmation reference
conditions
B.1 Gas chromatographic conditions
The gas chromatographic conditions are listed below.
a) Chromatographic column. Capillary column. DB-5 ms 30 m × 0.25 mm
(inner diameter) × 0.25 μm, or equivalent;
b) Temperature programming. 30 °C (keep for 4 min), rising from 5 °C/min to
c) Inlet temperature. 250 °C;
d) GC-MS interface temperature. 280 °C;
e) Carrier gas (He). 0.55 mL/min;
f) Injection mode. split injection, split ratio is 10.1.
B.2 Mass Spectrometry Conditions
The mass spectrometry conditions are listed below.
a) Ion source temperature. 230 °C;
b) Quadrupole rod temperature. 150 °C;
c) Ion source. EI source, ionization energy 70 eV;
e) Qualitative ion. 86,44 m/z.
Note. For different mass spectrometers, the instrument parameters may be different.
Before the determination, the mass spectrometry parameters shall be optimized to the
best.
B.3 Qualitative determination
When determining the sample, dilute the sample solution appropriately, and
determine the sample solution and standard working solution according to gas
chromatography-mass spectrometry conditions. If it is confirmed that the
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