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食品安全国家标准 食品接触材料及制品 11-氨基十一酸迁移量的测定
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GB 31604.13-2016
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标准编号: GB 31604.13-2016 (GB31604.13-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 11-氨基十一酸迁移量的测定
英文名称: Food contact materials -- Polymer -- Determination of 11-aminoundecanoic acid in food simulants -- High performance liquid chromatography
行业: 国家标准
中标分类: X09
字数估计: 8,876
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): GB/T 23296.12-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.13-2016: 食品安全国家标准 食品接触材料及制品 11-氨基十一酸迁移量的测定
GB 31604.13-2016 英文名称: Food contact materials -- Polymer -- Determination of 11-aminoundecanoic acid in food simulants -- High performance liquid chromatography
１ 范围
本标准规定了食品接触材料及制品中１１-氨基十一酸迁移量的高效液相色谱检测方法。
本标准适用于食品接触材料及制品中１１-氨基十一酸迁移量的测定。
２ 原理
食品模拟物中１１-氨基十一酸与荧光胺反应生成衍生物，经高效液相色谱分离，用荧光检测器检测
其衍生物含量，换算得出１１-氨基十一酸的含量，采用外标法定量。
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。试验中容器及转移
应避免使用塑料材质器具。
３．１ 试剂
３．１．１ 十水合四硼酸二钠（Ｎａ２Ｂ４Ｏ７·１０Ｈ２Ｏ）。
３．１．２ 磷酸（Ｈ３ＰＯ４）。
３．１．３ 硼酸（Ｈ３ＢＯ３）。
３．１．４ 荧光胺（Ｃ１７Ｈ１０Ｏ４）。
３．１．５ 氢氧化钠（ＮａＯＨ）。
３．１．６ 磷酸二氢钠一水合物（ＮａＨ２ＰＯ４·Ｈ２Ｏ）。
３．１．７ 冰乙酸（ＣＨ３ＣＯＯＨ）。
３．１．８ 无水乙醇（ＣＨ３ＣＨ２ＯＨ）。
３．１．９ 丙酮（ＣＨ３ＣＯＣＨ３）：色谱纯。
３．１．１０ 异辛烷［（ＣＨ３）２ＣＨＣＨ２Ｃ（ＣＨ３）３］。
３．１．１１ 甲醇（ＣＨ３ＯＨ）：色谱纯。
３．１．１２ 氮气（Ｎ２）：纯度≥９９．９％。
３．２ 试剂配制
３．３ 标准品
１１-氨基十一酸（Ｃ１１Ｈ２３Ｏ２Ｎ，ＣＡＳ号：２４３２-９９-７），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 １１-氨基十一酸水溶液储备液（１．２５ｍｇ／ｍＬ）：准确称取１１-氨基十一酸标准品１２５ｍｇ（精确至０．１ｍｇ）用２ｍＬ９６％乙酸溶解后转移至１００ｍＬ容量瓶中，并以水定容至刻度，放置于４℃冰箱保存。
３．４．２ １１-氨基十一酸异辛烷储备液（０．５０ｍｇ／ｍＬ）：准确称取１１-氨基十一酸标准品２５ｍｇ（精确至０．１ｍｇ）用５ｍＬ冰乙酸溶解后转移至５０ｍＬ容量瓶中，并以异辛烷定容至刻度，放置于４℃冰箱保存。
３．４．３ １１-氨基十一酸水溶液标准中间液（２５μｇ／ｍＬ）：分别移取２ｍＬ水溶液储备液至３个不同的１００ｍＬ容量瓶中，分别用水基、酸性、酒精类食品模拟物定容。
３．４．４ 水基、酸性食品、酒精类食品模拟物标准工作溶液：分别移取１１-氨基十一酸水溶液标准中间液０ｍＬ、１．０ｍＬ、２．０ｍＬ、４．０ｍＬ、１０．０ｍＬ、２０．０ｍＬ至５０ｍＬ容量瓶中，用水定容。标准工作液的浓度分别为０μｇ／ｍＬ、０．５μｇ／ｍＬ、１．０μｇ／ｍＬ、２．０μｇ／ｍＬ、５．０μｇ／ｍＬ、１０．０μｇ／ｍＬ。采用同样方式，分别用对应酸性、酒精类食品模拟物配制同样浓度系列的１１-氨基十一酸标准工作溶液。临用时配制。
３．４．５ 油基食品模拟物标准工作溶液：分别称取５ｇ（精确至０．０１ｇ）橄榄油至６个不同的２５ｍＬ锥形瓶中。分别加入０μＬ、５μＬ、１０μＬ、２０μＬ、５０μＬ、１００μＬ的１１-氨基十一酸异辛烷储备液，充分混匀。标准工作液的浓度分别为０μｇ／ｇ、０．５μｇ／ｇ、１．０μｇ／ｇ、２．０μｇ／ｇ、５．０μｇ／ｇ、１０．０μｇ／ｇ。然后按５．２．２进行。
４ 仪器和设备
４．１ 高效液相色谱仪：配荧光检测器。
４．２ 振荡器：往复型。
５ 分析步骤
５．１ 食品模拟物试液的制备
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。
５．２ 浸泡液的处理
５．２．１ 水基、酸性、酒精类食品模拟物
准确移取１．０ｍＬ从迁移试验中获得的水基、酸性、酒精类食品模拟物至１０ｍＬ反应管中，当模拟物为４％乙酸时应同时加入１５０μＬ氢氧化钠溶液以调节ｐＨ。余下步骤按５．４进行衍生，平行制样２份。
５．２．２ 油基食品模拟物
称取５ｇ（精确至０．０１ｇ）从迁移试验中得到的橄榄油介质食品模拟物至２５ｍＬ锥形瓶中，加入５ｍＬ异辛烷，混匀。准确移入５．０ｍＬ９６％乙酸，将锥形瓶放置在振荡器上振荡３０ｍｉｎ。待两相分离后，准确移取１．０ｍＬ下层的乙酸提取液转移至１０ｍＬ反应管中，用氮气浓缩器于４０℃将乙酸提取液吹干。向吹干后的反应管中准确移入１．０ｍＬ水，置于涡旋振荡器上处理１０ｓ，充分混匀。余下步骤按５．４进行衍生，平行制样２份。
５．３ 空白试液的制备
按５．２处理未与食品接触材料接触的食品模拟物，余下步骤按５．４进行衍生。
５．４ １１-氨基十一酸的衍生
准确移取１．０ｍＬ硼酸缓冲溶液加入到制备的水基、酸性、酒精类、油基食品模拟物试液及制备的
空白溶液中，置于涡旋振荡器上处理１０ｓ，充分混匀。混匀过程中，加入１．０ｍＬ荧光胺溶液。将所得衍生物溶液过微孔滤膜，滤液待测。
５．５ 仪器参考条件
ａ） 色谱柱：Ｃ１８柱（柱长２５０ｍｍ，内径４．６ｍｍ，粒径５μｍ），或同等性能的色谱柱。
ｂ） 流动相：甲醇-磷酸盐缓冲溶液（７０＋３０，体积比）。
ｃ） 流速：１．０ｍＬ／ｍｉｎ。
ｄ） 进样量：１０μＬ。
ｅ） 柱温：室温。
ｆ） 荧光检测器：激发波长３９０ｎｍ，发射波长４８０ｎｍ。
５．６ 标准工作曲线的制作
分别吸取上述标准系列的衍生溶液注入液相色谱仪中，按照５．５仪器参考条件测定相应的峰面积
（１１-氨基十一酸标准物质衍生物色谱图见附录 Ａ），以标准工作液中１１-氨基十一酸浓度为横坐标，以１１-氨基十一酸峰面积为纵坐标，绘制标准工作曲线。
５．７ 试样溶液的测定
按照５．５仪器参考条件，将试样的衍生溶液注入液相色谱仪中，以保留时间定性，同时记录峰面积，根据标准曲线得到待测液中１１-氨基十一酸的浓度。
６ 分析结果的表述
由标准曲线得到食品模拟物试液中１１-氨基十一酸的浓度，按GB ５００９．１５６进行迁移量计算，得到食品接触材料及制品中１１-氨基十一酸的迁移量。计算结果保留至小数点后两位。
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１０％。
８ 其他
本标准的定量限：水基、酸性、酒精类食品模拟物中１１-氨基十一酸定量限为０．８ｍｇ／Ｌ，油基食品模拟物中１１-氨基十一酸定量限为０．８ｍｇ／ｋｇ。
GB 31604.13-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Food contact materials and products - Determination
of 11-amino undecanoic acid migration quantity
ISSUED ON. OCTOBER 19, 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 . 6
5 Analytical procedures . 7
6 Analysis results expression . 8
7 Precision . 9
8 Others . 9
Appendix A 11-amino undecanoic acid standard substance derivative
chromatogram . 10
Foreword
This standard replaces GB/T 23296.12-2009 "Food contact materials – Polymer
- Determination of 11-aminoundecanoic acid in food simulants - High
performance liquid chromatography"
Compared with GB/T 23296.12-2009, the main changes of this standard are as
follows.
--- The standard name is changed to “National food safety standard - Food
contact materials and products - Determination of 11-amino undecanoic
acid migration quantity”;
--- Modify the preparation of food simulant test solution;
--- Modify the expression of analysis results.
National food safety standard -
Food contact materials and products - Determination
of 11-amino undecanoic acid migration quantity
1 Scope
This standard specifies the test method of high performance liquid
chromatography of 11-amino undecanoic acid migration quantity in food contact
materials and products.
This standard applies to the determination of 11-amino undecanoic acid
migration quantity in food contact materials and products.
2 Principles
11-amino undecanoic acid in food simulants reacts with fluorescamine to form
derivative, which is separated by high performance liquid chromatography; use
fluorescence detector to test the derivative content; obtain the content of 11-
amino undecanoic acid by conversion; 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. The containers
and transfer apparatuses in the test shall avoid using plastic materials.
3.1 Reagents
3.1.1 Disodium tetraborate decahydrate (Na2B4O7·10H2O).
3.1.2 Phosphoric acid (H3PO4).
3.1.3 Boric acid (H3BO3).
3.1.4 Fluorescent amine (C17H10O4).
3.1.5 Sodium hydroxide (NaOH).
11-amino undecanoic acid (C11H23O2N, CAS No.. 2432-99-7), purity ≥ 99%, or
standard substance which is identified by national authentication and awarded
a reference material certificate.
3.4 Standard solution preparation
3.4.1 11-amino undecanoic acid aqueous-solution stock solution (1.25mg/mL).
Accurately WEIGH 125mg (accurate to 0.1mg) of 11-amino undecanoic acid
standards; USE 2mL of 96% acetic acid to dissolve it; TRANSFER it into 100mL
volumetric flask; USE water to dilute it to the mark; STORE it in a refrigerator at
4 °C.
3.4.2 11-amino undecanoic acid isooctane stock solution (0.50mg/mL).
Accurately WEIGH 25mg of 11-amino undecanoic acid standards (accurate to
0.1mg); USE 5mL of glacial acetic acid to dissolve it; TRANSFER it into 50mL
volumetric flask; USE isooctane to dilute it to the mark; STORE it in a
3.4.3 11-amino undecanoic acid aqueous-solution standard intermediate
solution (25μg/mL). Respectively MOVE 2mL of aqueous solution stock solution
into 3 different 100mL volumetric flasks; USE water-based, acidic, alcoholic
food simulants to dilute it, respectively.
3.4.4 Water-based, acidic food, alcoholic food simulants standard working
solution. Respectively MOVE 0mL, 1.0mL, 2.0mL, 4.0mL, 10.0mL, 20.0mL of
11-amino undecanoic acid aqueous solution standard intermediate solution into
50mL volumetric flask; USE water to dilute it. The concentration of the standard
working solution is 0μg/mL, 0.5μg/mL, 1.0μg/mL, 2.0μg/mL, 5.0μg/mL and
alcoholic food simulants to prepare 11-amino undecanoic acid standard working
solution with the same concentration series. PREPARE it when in use.
3.4.5 Oil-based food simulant standard working solution. WEIGH 5g (accurate
to 0.01g) of olive oil respectively; PLACE it into 6 different 25mL conical flasks.
Respectively ADD 0μL, 5μL, 10μL, 20μL, 50μL and 100μL of 11-amino
undecanoic acid isooctane stock solution; MIX it uniformly. The concentration
of standard working solution is 0μg/g, 0.5μg/g, 1.0μg/g, 2.0μg/g, 5.0μg/g and
10.0μg/g, respectively. Then operate according to 5.2.2.
4 Instrument and equipment
detector.
4.2 Oscillator. Reciprocating-type.
Accurately MOVE 1.0mL of boric acid buffer solution into the prepared water-
based, acidic, alcoholic, oil-based food simulant test solution and the prepared
blank solution; PLACE it on vortex oscillator for 10s; MIX it uniformly. During the
mixing process, ADD 1.0mL of fluorescamine solution. The resulting derivative
solution is passed through microfiltration membrane; the filtrate is waiting for
determination.
5.5 Instrument reference conditions
diameter 4.6mm, particle-size 5μm), or the chromatographic column with
equivalent performance.
b) Mobile phase. methanol-phosphate buffer solution (70+30, volume ratio).
c) Flow rate. 1.0mL/min.
d) Injection volume. 10μL.
e) Column temperature. room temperature.
f) Fluorescence detector. excitation wavelength 390nm, emission
wavelength 480nm.
5.6 Drawing of standard working curve
liquid chromatograph; DETERMINE the corresponding peak area according to
5.5 instrument reference conditions (see Appendix A for the chromatogram of
11-amino undecanoic acid standard substance derivative). With the 11-amino
undecanoic acid concentration of standard working solution as abscissa, AND
the corresponding peak area of 11-amino undecanoic acid as vertical axis,
DRAW a standard working curve.
5.7 Determination of sample solution
According to 5.5 instrument reference conditions, INJECT the sample derivative
solution into liquid chromatograph; DETERMINE the nature based on the
concentration of 11-amino undecanoic acid in the solution-under-test according
to the standard curve.
6 Analysis results expression
OBTAIN 11-amino undecanoic acid concentration of food stimulant sample
solution from standard curve; CALCULATE migration quantity according to GB
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