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食品安全国家标准 食品中过氧化氢残留量的测定
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GB 5009.226-2016
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标准编号: GB 5009.226-2016 (GB5009.226-2016)
中文名称: 食品安全国家标准 食品中过氧化氢残留量的测定
英文名称: Determination of hydrogen peroxide residues in foods
行业: 国家标准
中标分类: X09
字数估计: 7,757
发布日期: 2016-08-31
实施日期: 2017-03-01
旧标准 (被替代): GB/T 23499-2009
标准依据: 国家卫生和计划生育委员会公告2016年第11号
GB 5009.226-2016: 食品安全国家标准 食品中过氧化氢残留量的测定
GB 5009.226-2016 英文名称: Determination of hydrogen peroxide residues in foods
中华人民共和国国家标准
1 范围
本标准规定了食品中过氧化氢残留量的测定方法。
本标准适用于预包装牛奶、饮料、豆制品、水发产品、鸡爪等食品中过氧化氢残留量的测定。
第一法 碘量法
5 分析步骤
5.1 试样制备
5.1.1 固体样品
称取粉碎均匀的试样可食部分10g(精确到0.01g),加适量水溶解,转移入100mL容量瓶中,对蛋
白质、脂肪含量较高的样品可加入乙酸锌溶液5mL、亚铁氰化钾溶液5mL,加水定容至刻度(V1),摇
匀。浸泡30min,用滤纸过滤,滤液作为试样液备用。
5.1.2 液体样品
称取25g(精确到0.01g)试样于100mL容量瓶中,对蛋白质、脂肪含量较高的样品可加入乙酸锌
溶液5mL、亚铁氰化钾溶液5mL,加水定容至刻度(V1),摇匀,用滤纸过滤,滤液作为试样液备用。如
样品滤液有颜色,加入1g活性炭,振摇1min,用干燥滤纸过滤,弃去初滤液,滤液待用。
5.2 测定
分别吸取滤液25.0mL(V2),置于A、B两个250mL碘量瓶中,A瓶中加入0.1%过氧化氢酶溶液
0.5mL,加盖混匀,放置10min(放置过程中摇动数次)。在A、B两瓶中各加入10%硫酸溶液5.0mL、
碘化钾溶液5.0mL、3%钼酸铵溶液3滴,混匀,置暗处放置10min,各加水50mL,分别用硫代硫酸钠
标准溶液滴定,待滴至微黄色时,加淀粉指示剂0.5mL,继续滴至蓝色消失,分别记录A、B两瓶消耗硫
代硫酸钠标准溶液的毫升数。
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 其他本方法定量限为3mg/kg。
第二法 钛盐比色法
9 原理
过氧化氢在酸性溶液中,与钛离子生成稳定的橙色络合物。在430nm下,吸光度与样品中过氧化
氢含量成正比,用比色法测定样品中过氧化氢的含量。
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规定的三级水。
10.1 试剂
10.1.1 高锰酸钾(KMnO4)。
10.1.2 30%过氧化氢溶液(H2O2)。
10.1.3 硫酸(H2SO4)。
10.1.4 二氧化钛(TiO2)。
10.1.5 硫酸铵[(NH4)2SO4]。
10.1.6 盐酸(HCl)。
10.2 试剂配制
10.2.1 钛溶液:称取1.00g二氧化钛(TiO2)、4.00g硫酸铵于250mL锥形瓶,加入100mL浓硫酸,
上面放置一小漏斗,置于可控温电热套中150℃保温15h~16h,冷却后以400mL水稀释,最后用滤
纸过滤,清液备用。
10.2.2 1mol/L盐酸溶液:量取90mL盐酸,加入1000mL水中。
10.2.3 硫酸溶液(1+4):量取10mL硫酸,加入40mL水中。
10.3 标准溶液配制
10.3.1 高锰酸钾标准溶液[c(5KMnO4)=0.100mol/L]:按GB/T 601规定的方法配制和标定。
10.3.2 过氧化氢标准储备液:吸取30%过氧化氢溶液1mL于100mL容量瓶中,加水至刻度,混匀。
吸取20.00mL过氧化氢标准储备液于250mL锥形瓶中,加入10%硫酸溶液(3.2.3)25mL,用高
锰酸钾标准溶液[c(5KMnO4)=0.100mol/L]滴定至微红色
12.2 标准曲线的制作
吸取0.00mL、0.25mL、0.50mL、1.00mL、2.50mL、5.00mL、7.50mL、10.0mL过氧化氢标准使
用液(相当于0μg、5μg、10μg、20μg、50μg、100μg、150μg、200μg过氧化氢),分别置于25mL带塞
比色管中。各加入钛溶液5.0mL,用水定容至25mL,摇匀,放置10min。用5cm比色皿,以空白管调
节零点,于波长430nm处测吸光度。以标准系列的过氧化氢浓度(μg/mL)对吸光度绘制标准曲线。
12.3 试样溶液的测定
吸取10.00mL(V2)试样液于25mL带塞比色管中,各加入钛溶液5.0mL,用水定容至25mL,摇
匀,放置10min。用5cm比色皿,以空白管调节零点,于波长430nm处测吸光度。同时做试剂空白试验。
如果经过活性炭吸附后试样液仍有颜色干扰,应扣除试样液的本底色,即用5.0mL硫酸溶液(1+4)
代替钛溶液,其他按上述方法操作。
GB 5009.226-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard – Determination
of Hydrogen Peroxide Residual Quantity in Foods
ISSUED ON. AUGUST 31, 2016
IMPLEMENTED ON. MARCH 1, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
Method I -- Iodometric Method ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Instruments and Equipment ... 6
5 Analytical Procedures ... 6
6 Expression of Analysis Results ... 6
7 Precision ... 7
8 Others ... 7
Method II -- Titanium Salt Colorimetry ... 8
9 Principle ... 8
10 Reagents and Materials ... 8
11 Instruments and Equipment ... 9
12 Analytical Procedures ... 10
13 Expression of Analysis Results ... 10
14 Precision ... 11
15 Others ... 11
National Food Safety Standard – Determination
of Hydrogen Peroxide Residual Quantity in Foods
1 Scope
This Standard specifies methods of determining hydrogen peroxide residual quantity
in foods.
This Standard is applicable to the determination of hydrogen peroxide residual quantity
in foods, such as prepackaged milk, beverage, soy product, waterish logged product
and chicken feet, etc.
Method I -- Iodometric Method
2 Principle
Strong oxide in foods oxidizes potassium iodide in diluted sulfuric acid and generates
quantitative iodine. In the generated iodine, starch is taken as the indicator; sodium
thiosulfate standard solution is titrated to obtain the total quantity of strong oxide. Add
catalase decomposition to remove hydrogen peroxide in the sample; sodium
thiosulfate standard solution is titrated to remove the content of other oxides other than
hydrogen peroxide. The difference of the result of two titrations can be adopted to
obtain the content of hydrogen peroxide in the sample.
3 Reagents and Materials
Unless otherwise indicated, the reagents adopted under this method are of analytical
purity. The water is third-grade water as specified in GB/T 6682.
3.1 Reagents
3.1.1 Sodium thiosulfate (Na2S2O3).
3.1.2 Soluble starch [(C6H10O5)n].
3.1.3 Potassium iodide (KI).
3.1.4 Sulfuric acid (H2SO4).
3.1.5 Ammonium molybdate [(NH4)6Mo7O24.4H2O].
3.1.6 Catalase (unit vitality>200,000 U/mL). store under -20 °C.
4 Instruments and Equipment
4.1 Electronic balance. division value. 0.01 g.
4.2 High-speed grinder.
5 Analytical Procedures
5.1 Preparation of Samples
5.1.1 Solid sample
Weigh-take 10 g (accurate to 0.01 g) of edible part from grinded and homogenized
sample, add an appropriate amount of water to dissolve it, then, transfer it into 100 mL
volumetric flask. 5 mL of zinc acetate solution and 5 mL of potassium ferrocyanide
solution can be added to samples with relatively high content of protein and fat; add
water to dilute to the constant volume (V1), shake it up. Soak it for 30 min, use filter
paper to filter it. Reserve the filtrate as sample solution for later usage.
5.1.2 Liquid sample
Weigh-take 25 g (accurate to 0.01 g) of sample and place it in 100 mL volumetric flask.
added to samples with relatively high content of protein and fat; add water to dilute to
the constant volume (V1), shake it up. Use filter paper to filter it. Reserve the filtrate as
sample solution for later usage. If any color shows up in the sample filtrate, add 1 g of
activated carbon, shake it for 1 min; use dry filter paper to filter it, remove the primary
filtrate and reserve the filtrate for later usage.
5.2 Determination
Respectively take 25.0 mL (V2) of the filtrate and place it in two 250 mL iodine
volumetric flasks (A and B); add 0.5 mL of 0.1% catalase solution to volumetric flask A,
put on the lid and mix it up; place it evenly for 10 min (shake it for several times during
potassium iodide to volumetric flask A and B, and 3 drops of 3% ammonium molybdate
solution. Mix it up, place it in the dark for 10 min. Respectively add 50 mL of water, and
adopt sodium thiosulfate standard solution to titrate it, till it turns yellowish. Add 0.5 mL
of starch indicator and continue the titration, till blue vanishes. Respectively record the
volume of sodium thiosulfate standard solution consumed in volumetric flask A and B.
6 Expression of Analysis Results
The content of hydrogen peroxide in the sample shall be calculated in accordance with
10.3.1 Potassium permanganate standard solution [c(ଵହKMnO4)=0.100 mol/L]. prepare
and calibrate in accordance with the method stipulated in GB/T 601.
peroxide solution and place it in 100 mL volumetric flask; add water to the constant
volume, mix it up.
Take 20.00 mL of hydrogen peroxide standard stock solution and place it in 250 mL
conical flask; add 25 mL of 10% sulfuric acid solution (3.2.3); adopt potassium
permanganate standard solution [c(ଵହKMnO4)=0.100 mol/L] to titrate it till it turns reddish.
The concentration of hydrogen peroxide standard stock solution shall be calculated in
accordance with Formula (2).
Where.
X - The concentration of hydrogen peroxide standard stock solution, expressed in
17.01 - The mass of hydrogen peroxide equivalent with potassium permanganate
standard solution [c(ଵହKMnO4)=0.100 mol/L] per mL, expressed in (mg);
c - The concentration of potassium permanganate standard solution [c(ଵହKMnO4)=0.100
mol/L], expressed in (mol/L);
V - The volume of potassium permanganate standard solution [c(ଵହ KMnO4)=0.100
mol/L] for titration, expressed in (mL).
10.3.3 Hydrogen peroxide standard working solution. dilute hydrogen peroxide
standard stock solution to 20 μg/mL in accordance with the calibration result in 10.3.2.
11 Instruments and Equipment
11.2 High-speed grinder.
11.3 Spectrophotometer. equipped with 5 cm colorimetric ware.
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