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食品安全国家标准 食品中羰基价的测定
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GB 5009.230-2016
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标准编号: GB 5009.230-2016 (GB5009.230-2016)
中文名称: 食品安全国家标准 食品中羰基价的测定
英文名称: National Food Safety Standard -- Determination of carbonyl value
行业: 国家标准
中标分类: X09
字数估计: 5,525
发布日期: 2016-08-31
实施日期: 2017-03-01
旧标准 (被替代): GB/T 5009.37-2003部分
标准依据: 国家卫生和计划生育委员会公告2016年第11号
GB 5009.230-2016: 食品安全国家标准 食品中羰基价的测定
GB 5009.230-2016 英文名称: National Food Safety Standard -- Determination of carbonyl value
中华人民共和国国家标准
1 范围
本标准规定了食品中羰基价的测定。
本标准适用于油炸小食品、坚果制品、方便面、膨化食品以及食用植物油等食品中羰基价的测定。
5 分析步骤
5.1 取样方法
称取含油脂较多的试样0.5kg,含脂肪少的试样取1.0kg,在玻璃研钵中研碎,混合均匀后,按四分
法对角取样,放置广口瓶内保存于4℃以下冰箱中。
液态油脂类试样根据试样情况取有代表性试样后,放置广口瓶内保存于4℃以下冰箱中。
5.2 非油脂类试样处理
5.2.1 含油脂高的试样,如油炸花生、坚果等:称取混合均匀的试样50g,置于250mL带盖广口瓶中,
加入50mL石油醚,放置14h~18h,用快速滤纸过滤后,室温下,用旋转蒸发器旋蒸15min,减压回收
溶剂,得到油脂以供测定。用前保存于4℃以下冰箱中。
5.2.2 含油脂中等的试样,如蛋糕、江米条等:称取混合均匀的试样100g,置于500mL带盖广口瓶中,
加入100mL~200mL石油醚,放置14h~18h,用快速滤纸过滤后,室温下,用旋转蒸发器旋蒸
15min,减压回收溶剂,在50℃鼓风干燥箱中挥发石油醚1h,得到油脂以供测定。用前保存于4℃以下冰箱中。
5.2.3 含油脂少的试样,如面包、饼干等:称取混合均匀的试样250g~300g于500mL带盖广口瓶,
加入适量石油醚浸泡试样,放置14h~18h,用快速滤纸过滤后,室温下,用旋转蒸发器旋蒸15min,
减压回收溶剂,在50℃鼓风干燥箱中挥发石油醚1h,得到油脂以供测定。用前保存于4℃以下冰箱中。
5.2.4 含水量较高样品,可加入适量无水硫酸钠,使样品成粒状;易结块样品,可加入4倍~6倍量的海砂,混合均匀后再提取油脂。
5.3 测定
称取0.025g~0.5g油样(精确至0.1mg):羰基价低于30meq/kg的油样称取0.1g,羰基价
30meq/kg~60meq/kg的油样称取0.05g,羰基价高于60meq/kg的油样,称取0.025g;置于25mL
具塞试管中,加5mL苯溶解油样,加3mL三氯乙酸溶液及5mL2,4-二硝基苯肼溶液,仔细振摇混匀。
在60°C水浴中加热30min,反应后取出用流水冷却至室温,沿试管壁缓慢加入10mL氢氧化钾-
乙醇溶液,使成为二液层,涡旋振荡混匀后,放置10min。
以1cm比色杯,用试剂空白调节零点,于波长440nm处测吸光度。
GB 5009.230-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Determination of Carbonyl Value 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
2 Principle ... 4
3 Reagents and Materials ... 4
4 Instruments and Equipment ... 5
5 Analytical Procedures ... 5
6 Expression of Analysis Results ... 6
7 Precision ... 7
National Food Safety Standard -
Determination of Carbonyl Value in Foods
1 Scope
This Standard specifies the method of determining carbonyl value in foods.
This Standard is applicable to the determination of carbonyl value in foods, such as
fried food, nut, instant noodle, puffed food and edible vegetable oil, etc.
2 Principle
In alkaline solution, the reaction product of carbonyl compound and
2,4-dinitrophenylhydrazine generates maroon or wine red. Determine absorbance at
the wavelength of 440 nm and calculate carbonyl value.
3 Reagents and Materials
3.1 Reagents
3.1.1 Ethanol (C2H6O). analytical purity.
3.1.2 Benzene (C6H6). spectral purity or chromatographic purity.
3.1.3 2,4-dinitrophenylhydrazine (C6H6N4O4). analytical purity.
3.1.4 Trichloroacetic acid (C2H6Cl3O2). analytical purity.
3.1.5 Potassium hydroxide (KOH). analytical purity.
3.1.6 Petroleum ether (C5H12O2). analytical purity, boiling range. 30 °C~60 °C.
3.1.7 Aluminum powder (Al). analytical purity.
3.2 Preparation of Reagents
3.2.1 Refined ethanol. take 1,000 mL of ethanol and place it in 2,000 mL round-bottom
flask; add 5 g of aluminum powder, zeolite and 10 g of potassium hydroxide; connect
with the reflux condenser of standard grinding mouth; start heating and reflux for 1 h in
water bath, then, adopt all-glass distillation unit to distill and gather the distillate.
3.2.2 Trichloroacetic acid solution. weigh-take 4.3 g of solid trichloroacetic acid, add
100 mL of benzene to dissolve it.
evaporator under the room temperature; decompress and recover the reagent; use
air-blowing drying oven to volatilize petroleum ether for 1 h under 50 °C, then, obtain
grease for later determination. Store it in the refrigerator under 4 °C before usage.
5.2.3 Samples with low content of grease, such as bread and biscuit. weigh-take 250
g~300 g of mixed sample and place it in 500 mL wide-mouth bottle with a lid; add an
appropriate amount of petroleum ether to soak the sample and place it for 14 h~18 h.
Take quick filter paper to filter it; start rotary evaporation for 15 min with a rotary
evaporator under the room temperature; decompress and recover the reagent; use
air-blowing drying oven to volatilize petroleum ether for 1 h under 50 °C, then, obtain
grease for later determination. Store it in the refrigerator under 4 °C before usage.
5.2.4 Samples with high content of water. add an appropriate amount of anhydrous
sodium sulfate to make the sample granular; easily agglomerated sample. add 4
times~6 times of sea sand, mix it up, then, extract grease.
5.3 Determination
Weigh-take 0.025 g~0.5 g (accurate to 0.1 mg) of grease sample. weigh-take 0.1 g of
grease sample with carbonyl value < 30 meq/kg; weigh-take 0.05 g of grease sample
with carbonyl value 30 meq/kg~60 meq/kg; weigh-take 0.025 g of grease sample with
carbonyl value >60 meq/kg; place it in 25 mL tube with a plug, then, add 5 mL of
benzene to dissolve the grease sample; add 3 mL of trichloroacetic acid solution and
5 mL of 2,4-dinitrophenylhydrazine solution; meticulously shake it and mix it up.
Heat it up for 30 min in water bath at 60 °C; after reaction, take it out and use running
water to cool it down to the room temperature. Slowly add 10 mL of potassium
hydroxide-ethanol solution along the tube wall to turn it into two-liquid layer. Start
vortex oscillation and mix it up, then, place it evenly for 10 min.
Take 1 cm colorimetric cup and adjust the zero point with reagent blank; measure
6 Expression of Analysis Results
Carbonyl value in the sample shall be calculated in accordance with Formula (1).
Where.
X - Carbonyl value (calculated by grease) of the sample, expressed in (meq/kg);
A - The absorbance of the sample during determination;
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