标准编号:	GB 31604.18-2016
中文名称:	食品安全国家标准 食品接触材料及制品 丙烯酰胺迁移量的测定
英文名称:	National Food Safety Standard - Food Contact Materials and Articles - Determination of Migration of Acrylamide
行业分类:	GB    国家标准
发布机构:	国家卫生和计划生育委员会
发布日期:	2016-10-19
实施日期:	2017-4-19
标准状态:	valid
替代旧标准:	GB/T 23296.9-2009 食品接触材料 高分子材料 食品模拟物中丙烯酰胺的测定 高效液相色谱法
翻译语言:	英文
文件格式:	PDF
中文字符数:	6000 字
翻译价格(元):	200.0
交付时间:	付款后 1 个工作日

Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative. This standard replaces GB/T 23296.9-2009 Food Contact Materials - Polymer - Determination of Acrylamide in Food Simulants - High Performance Liquid Chromatography. The following main changes have been made with respect to GB/T 23296.9-2009 (the previous edition): ——This standard is renamed as National Food Safety Standard - Food Contact Materials and Articles - Determination of Migration of Acrylamide; ——Application scope is added; ——Preparation of food simulants is modified; ——Treatment process of oil-based food simulant test solution is modified. National Food Safety Standard Food Contact Materials and Articles Determination of Migration of Acrylamide 1 Scope This standard specifies the determination of migration of acrylamide in food contact materials and articles. This standard is applicable to the detection of migration of acrylamide in food contact materials and articles by liquid chromatography. 2 Principle Detect the food simulants of food contact materials and articles by liquid chromatography, directly inject the sample of water-based, acidic and alcoholic food simulants, inject the sample of oil-based food simulant after water extraction, separate through high performance liquid chromatograph (with ion exclusion column), detect with ultraviolet detector, and carry out quantitative determination by external standard peak area method. 3 Reagents and Materials Unless otherwise specified, analytically-pure reagents and Class-I water (defined in GB/T 6682) are adopted for the purpose of this method. Containers and transfer appliances in test shall not be made of plastic materials. 3.1 Reagents 3.1.1 Water-based, acidic, alcoholic and oil-based food simulants: the reagents used shall be in accordance with the requirements of GB 31604.1. 3.1.2 Acetonitrile (C2H3N): chromatographically pure. 3.1.3 Methanol (CH3OH): chromatographically pure. 3.1.4 Sulfuric acid (H2SO4): guaranteed reagent. 3.2 Reagent preparation 3.2.1 Water-based, acidic, alcoholic and oil-based food simulants: prepare according to GB 5009.156 as well as the intended use and service conditions of to-be-tested sample. 3.2.2 Sulphuric acid solution (0.0036 mol/L): measure 0.1 mL sulfuric acid, scale the volume with water to 500 mL and mix well. 3.3 Standard product Acrylamide (C3H5NO): with purity≥99%. 3.4 Preparation of standard solutions 3.4.1 Acrylamide standard stock solution (1000 mg/L): accurately weigh 10 mg (accurate to 0.1 mg) acrylamide standard, scale the volume to 10 mL with methanol, keep the stock solution in 0℃~4℃ refrigerator. 3.4.2 Acrylamide standard intermediate solution (10 mg/L): pipet 1.0 mL acrylamide stock solution and scale the volume to 100 mL with methanol. 4 Instruments and Apparatus 4.1 High performance liquid chromatograph: equipped with ultraviolet detector. 4.2 Analytical balance: with sensibility of 0.1 mg and 0.01 g. 4.3 Microporous filter membrane: 0.2 μm. 4.4 Colorimetric tube with stopper: 25 mL. 5 Analysis Steps 5.1 Preparation of test solutions 5.1.1 Preparation of food simulant test solution Carry out migration test according to the intended use and service conditions of to-be-tested sample and the migration test methods and conditions specified in GB 5009.156 and GB 31604.1. After completion of the migration test, mix the simulants obtained from migration test sufficiently well for the next analysis. 5.1.2 Preparation of water-based, acidic and alcoholic food simulants test solution Filter the food simulant test solution with 0.2 μm microporous filter membrane for determination. 5.1.3 Preparation of oil-based food simulant test solution Weigh 10 g (accurate to 0.01 g) oil-based food simulant test solution into the colorimetric tube, add 10.0 mL water, violently oscillate for 1 min, and keep it still until layering. Filter the lower water solution with 0.2 μm filter membrane for determination. 5.1.4 Preparation of blank solution 5.1.4.1 Water-based, acidic and alcoholic food simulants blank solution Transfer the food simulant not in contact with the sample and filter with 0.2 μm microporous filter membrane for determination. 5.1.4.2 Oil-based food simulant blank solution Transfer 10 g (accurate to 0.01 g) food simulant not in contact with the sample and operate according to 5.1.3. 5.1.5 Water-based, acidic and alcoholic food simulants standard working solution Accurately pipet 0.00 mL, 0.03 mL, 0.05 mL, 0.08 mL, 0.1 mL and 0.5 mL acrylamide standard intermediate solutions into 10mL-volumetric flasks, then scale the volume with food simulant not in contact with the sample to obtain the standard working solutions with the concentrations of acrylamide of 0.00 mg/L, 0.03 mg/L, 0.05 mg/L, 0.08 mg/L, 0.10 mg/L and 0.50 mg/L respectively. In the same way, prepare acrylamide standard working solution with the same concentration series with corresponding water-based, acidic and alcoholic food simulants respectively. 5.1.6 Oil-based food simulant standard working solution Weigh 10 g (accurate to 0.01 g) oil-based food simulants and put into five colorimetric tubes respectively, pipet 0.00 mL, 0.03 mL, 0.05 mL, 0.08 mL, 0.1 mL and 0.5 mL acrylamide standard intermediate solutions (10 mg/L) into the colorimetric tubes and mix well, add 10.0 mL water, violently oscillate for 1 min and keep it still until layering to obtain the standard working solutions with the concentrations of acrylamide of 0.00 mg/kg, 0.03 mg/kg, 0.05 mg/kg, 0.08 mg/kg, 0.10 mg/kg and 0.50 mg/kg. Filter the lower water solution with 0.2 μm filter membrane for determination. 5.2 Determination 5.2.1 Liquid chromatographic conditions a) Chromatographic column: Venusil CIS ion-exclusion chromatographic column with length of 250 mm, inside diameter of 4.6 mm and particle size of 5 μm, or equivalent; b) Mobile phase: sulfuric acid solution: acetonitrile (91+9); c) Flow rate: 0.5 mL/min; d) Column temperature: 50℃; e) Ultraviolet detector: with wavelength of 198 nm; f) Sample injection amount: 20 μL. 5.2.2 Chromatographic determination Inject the standard solution and sample solution in sequence for determination, plot the standard curve with the concentration of acrylamide in the standard working solution as x-axis (in mg/L or mg/kg) and the corresponding peak area of acrylamide as y-axis. Carry out the qualitative determination by retention time and quantitative determination by external standard method. Under the above chromatographic conditions, the retention time of acrylamide is 11.6 min, see Annex A for the chromatogram of acrylamide. The regression parameter is calculated according to Formula (1): y=a×x+b (1) Where, y——the peak area of acrylamide in food simulant standard working solution; a——the slope of regression curve; x——the concentration of acrylamide in the food simulant standard working solution, mg/L or mg/kg; b——the intercept of regression curve.

Foreword i 1 Scope 2 Principle 3 Reagents and Materials 4 Instruments and Apparatus 5 Analysis Steps 6 Expression of Analysis Results 7 Accuracy 8 Other Annex A Chromatogram of Standard Solution

中华人民共和国国家标准 GB 31604.18—2016 食品安全国家标准 食品接触材料及制品 丙烯酰胺迁移量的测定 2016—10—19发布 2017—04—19实施 中华人民共和国 国家卫生和计划生育委员会 发布 前言 本标准代替GB/T 2329 6.9--2009《食品接触材料 高分子材料 食品模拟物中丙烯酰胺的测定高效液相色谱法》。 本标准与GB/T 23296.9--2009相比，主要变化如下： ——标准名称修改为“食品安全国家标准 食品接触材料及制品 丙烯酰胺迁移量的测定”； ——增加了适用范围； ——修改了食品模拟物制备； ——修改了油基食品模拟物试液的处理过程。 食品安全国家标准 食品接触材料及制品 丙烯酰胺迁移量的测定 1范围 本标准规定了食品接触材料及制品中丙烯酰胺迁移量的测定。 本标准适用于食品接触材料及制品中丙烯酰胺迁移量的液相色谱法检测。 2原理 对于食品接触材料及其制品的食品模拟物采用液相色谱进行检测，其中水基、酸性、酒精类食品模拟物直接进样，油基食品模拟物通过水萃取后进样，通过高效液相色谱(色谱柱为离子排斥柱)进行分离，采用紫外检测器进行检测，方法采用外标峰面积法定量。 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。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。 3.1.2 乙腈(C2H3N)：色谱纯。 3.1.3甲醇(CH3OH)：色谱纯。 3.1.4硫酸(H2SO4)：优级纯。 3.2试剂配制 3.21水基、酸性、酒精类、油基食品模拟物：根据待测样品的预期用途和使用条件，按GB 5009.156操作。 3.22硫酸溶液(0.003 6 mol/L)：量取0.1 mL硫酸，用水定容至500 mL，混匀。 3.3标准品 丙烯酰胺(C3H5NO)：纯度≥99％。 3.4标准溶液配制 3.4.1丙烯酰胺标准储备溶液(1 000 mg/L)：准确称取丙烯酰胺标准品10 mg(精确至0.1 mg)，用甲醇定容至10 mL，该储备液储存于0℃～4℃冰箱中。 3.4.2丙烯酰胺标准中间溶液(10 mg/L)：吸取1.0 mL丙烯酰胺贮备液用甲醇定容至100 mL。 4仪器和设备 4.1 高效液相色谱仪：配有紫外检测器。 4.2分析天平：感量0.1 mg和0.01 g。 4.3微孔滤膜：0.2 μm。 4.4具塞比色管：25 mL。 5分析步骤 5.1试液制备 5.1.1食品模拟物试液的制备 根据待测样品的预期用途和使用条件，按照GB 5009.156和GB 31 604.1规定的迁移试验方法及试验条件进行迁移试验。迁移试验结束后，将迁移试验所得模拟物充分混匀后，用于以下分析。 5.1.2水基、酸性、酒精类食品模拟物试液的制备 将食品模拟物试液通过0.2 μm微孔滤膜过滤后供测定用。 5.1.3油基食品模拟物试液的制备 称取10 g(精确至0.01 g)油基食品模拟物试液至比色管中，加入10.0 mL水，剧烈振荡1 min，静置分层。取下层水溶液，通过0.2 μm滤膜过滤后供测定用。 5.1.4空白溶液的制备 5.1.4.1水基、酸性、酒精类食品模拟物空白溶液 移取未与样品接触过的食品模拟物，通过0.2 μm微孔滤膜过滤后供测定用。 5.1.4.2油基食品模拟物空白溶液 移取10 g(精确至0.01 g)未与样品接触过的食品模拟物，按照5.1.3操作。 5.1.5水基、酸性、酒精类食品模拟物标准工作溶液 准确吸取丙烯酰胺标准中间溶液0.00 mL、0.03 mL、0.05 mL、0.08 mL、0.1 mL、0.5 mL于10 mL容量瓶中，用未与样品接触过的食品模拟物定容，得到丙烯酰胺浓度分别为0.00 mg/L、0.03 mg/L、0.05 mg/L、0.08 mg/L、0.10 mg/L、0.50 mg/L的标准工作液。采用同样方式，分别用对应水基、酸性、酒精类食品模拟物配制同样浓度系列的丙烯酰胺标准工作溶液。 5.1.6油基食品模拟物标准工作溶液 分别称取10 g(精确至0.01 g)油基食品模拟物至5个比色管中，分别吸取丙烯酰胺标准中间溶液(10 mg/L)0.00 mL、0.03 mL、0.05 mL、0.08 mL、0.1 mL、0.5 mL于比色管中，混匀，加入10.0 mL水，剧烈振荡1 min，静置分层。得到丙烯酰胺浓度分别为0.00 mg/kg、0.03 mg/kg、0.05 mg/kg、0.08 mg/kg、0.10 mg/kg、0.50 mg/kg的标准工作液。取下层水溶液，通过0.2 μm滤膜过滤后供测定用。 5.2测定 5.21液相色谱条件 a) 色谱柱：Venusil CIS，离子排斥色谱柱，柱长250 mm，内径4.6 mm，粒径5 μm，或相当者； b)流动相：硫酸溶液：乙腈(91+9)； c)流速：0.5 mL/min； d)柱温：50℃； e)紫外检测器：波长198 nm； f)进样量：20 μL。 5.22色谱测定 对标准溶液及样液依次进样测定，以标准工作溶液中丙烯酰胺浓度为横坐标，单位以“mg/L或mg/kg”表示；以对应的峰面积为纵坐标，绘制标准曲线。用保留时间定性，外标法定量。在上述色谱条件下丙烯酰胺保留时间为11.6 min，色谱图见附录A。 回归参数按式(1)计算： y=a×x+b ………………………(1) 式中： y——食品模拟物标准工作溶液中丙烯酰胺的峰面积； a——回归曲线的斜率； x——食品模拟物标准工作溶液中丙烯酰胺的浓度，单位为毫克每升或毫克每千克(mg/L或mg/kg)； b——回归曲线的截距。 6分析结果的表述 由标准曲线得到试样溶液中丙烯酰胺的浓度，按GB 5009.156进行迁移量计算，得到食品接触材料及制品中丙烯酰胺的迁移量。计算结果保留至小数点后两位。 7精密度 在重复的条件下获得的两次独立测定结果的绝对差值不得超过10％。 8其他 本方法对水基、酸性、酒精类食品模拟物中丙烯酰胺的检出限为0.01 mg/L，油基食品模拟物中丙烯酰胺的检出限为0.01 mg/kg。 本方法对水基、酸性、酒精类食品模拟物中丙烯酰胺的定量限为0.03 mg/L，油基食品模拟物中丙烯酰胺的定量限为0.03 mg/kg。 附 录 A 标准溶液色谱图 A.1 正己烷模拟物中丙烯酰胺标准液相色谱图 正己烷模拟物中丙烯酰胺标准液相色谱图见图A.1。 丙烯酰胺 图A.1 正己烷模拟物中丙烯酰胺标准液相色谱图(0.05 mg/L) A.2 10％乙醇模拟物中丙烯酰胺标准液相色谱图 10％乙醇模拟物中丙烯酰胺标准液相色谱图见图A.2。 丙烯酰胺 图A.2 10％乙醇模拟物中丙烯酰胺标准液相色谱图(0.05 mg/L) A.3 20％乙醇模拟物中丙烯酰胺标准液相色谱图 20％乙醇模拟物中丙烯酰胺标准液相色谱图见图A.3。 丙烯酰胺 图A.3 20％乙醇模拟物中丙烯酰胺标准液相色谱图(0.05 mg/L) A.4 50％乙醇模拟物中丙烯酰胺标准液相色谱图 50％乙醇模拟物中丙烯酰胺标准液相色谱图见图A.4。 丙烯酰胺 图A.4 50％乙醇模拟物中丙烯酰胺标准液相色谱图(0.05 mg/L) A.5 4％乙酸模拟物中丙烯酰胺标准液相色谱图 4％乙酸模拟物中丙烯酰胺标准液相色谱图见图A.5。 丙烯酰胺 图A.5 4％乙酸模拟物中丙烯酰胺标准液相色谱图(0.05 mg/L)