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食品安全国家标准 食品中诱惑红的测定
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GB 5009.141-2016
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标准编号: GB 5009.141-2016 (GB5009.141-2016)
中文名称: 食品安全国家标准 食品中诱惑红的测定
英文名称: National food safety standard -- Determination of allura red in foods
行业: 国家标准
中标分类: X09
字数估计: 6,62
发布日期: 2016-08-31
实施日期: 2017-03-01
旧标准 (被替代): GB/T 5009.141-2003
标准依据: 国家卫生和计划生育委员会公告2016年第11号
GB 5009.141-2016: 食品安全国家标准 食品中诱惑红的测定
GB 5009.141-2016 英文名称: National food safety standard -- Determination of allura red in foods
1 范围
本标准规定了汽水、硬糖、糕点、冰淇淋中诱惑红的测定方法。
本标准适用于汽水、硬糖、糕点、冰淇淋中诱惑红的测定。
2 原理
诱惑红在酸性条件下被聚酰胺粉吸附,而在碱性条件下解吸附,再用纸色谱法进行分离后,与标准
比较定性、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。
3.1 试剂
3.1.1 甲醇(CH3OH)。
3.1.2 石油醚:沸程30℃~60℃。
3.1.3 硫酸(H2SO4):优级纯。
3.1.4 乙醇(CH3CH2OH)。
3.1.5 氨水(NH3·H2O):含量20%~25%。
3.1.6 柠檬酸(C6H8O7·H2O)。
3.1.7 钨酸钠(Na2WO4·2H2O)。
3.1.8 丁酮(C4H8O)。
3.1.9 柠檬酸钠(C6H5Na3O7)。
3.1.10 正丁醇(C4H10O)。
3.1.11 海砂。
3.1.12 甲酸(HCOOH)。
3.2 试剂配制
3.2.1 硫酸溶液(10%,体积分数):将1mL硫酸缓慢加入至8mL水中,混匀,冷却,用水定容至
10mL,混匀。
3.2.2 乙醇-氨溶液:取2mL的氨水,加70%(体积分数)乙醇至100mL。
3.2.3 乙醇溶液(50%,体积分数):量取50mL无水乙醇与50mL水混匀。
3.2.4 柠檬酸溶液(200g/L):称取20g柠檬酸,加水至100mL,溶解混匀。
3.2.5 钨酸钠溶液(100g/L):称取10g钨酸钠,加水至100mL,溶解混匀。
3.2.6 氨水溶液(1%,体积分数):量取1mL氨水,加水至100mL,混匀。
3.2.7 柠檬酸钠溶液(2.5%,体积分数):称取2.5g柠檬酸,加水至100mL,溶解混匀。
3.2.8 甲醇-甲酸溶液(6∶4,体积分数):量取甲醇60mL,甲酸40mL,混匀。
3.2.9 展开剂1:丁酮+丙醇+水+氨水(7+3+3+0.5)。
3.2.10 展开剂2:正丁醇+无水乙醇+1%氨水溶液(6+2+3)。
3.2.11 展开剂3:2.5%柠檬酸钠+氨水+乙醇(8+1+2)。
3.3 标准品
诱惑红(CAS:25956-17-6)。
3.4 标准溶液配制
3.4.1 诱惑红标准贮备液配制:准确称取诱惑红0.025g(精确到0.0001g,按诱惑红实际纯度折算为纯
品后的质量),用水溶解并定容至25mL,诱惑红浓度为1.0mg/mL。
3.4.2 诱惑红标准使用液(0.1mg/mL):吸取诱惑红的标准贮备液5.0mL于50mL容量瓶中,加水稀
释到50mL。
4 仪器和设备
4.1 可见分光光度计。
4.2 电子天平:感量为0.001g和0.0001g。
4.3 微量注射器:10μL、50μL。
4.4 展开槽。
4.5 电吹风机。
4.6 离心机。
4.7 恒温水浴锅。
5 分析步骤
5.1 试样制备
5.1.1 汽水:将样品加热去二氧化碳后,称取10g(精确到0.001g)样品于烧杯中,然后用20%柠檬酸
调pH呈酸性,加入0.5g~1.0g聚酰胺粉吸附色素,将吸附色素的聚酰胺粉全部转到漏斗中过滤,用
pH4的酸性热水洗涤多次(约200mL),以洗去糖等物质。若有天然色素,用甲醇-甲酸溶液洗涤1次~
3次,每次20mL,至洗液无色为止。再用70℃的水多次洗涤至流出液中性。洗涤过程应充分搅拌然后
用乙醇-氨水溶液分次解吸色素,收集全部解吸液,于水浴上驱除氨,蒸发至2mL左右,转入5mL的容
量瓶中,用50%的乙醇分次洗涤蒸发皿,洗涤液并入5mL的容量瓶中,用50%的乙醇定容至刻度。此
液留作纸色谱用。
5.1.2 硬糖:称取10g(精确到0.001g)的已粉碎的样品,加30mL的水,温热溶解,若样品溶液的pH
较高,用柠檬酸溶液(3.2.4)调至pH4左右。加入0.5g~1.0g聚酰胺粉吸附色素,将吸附色素的聚酰
胺粉全部转到漏斗中过滤,用pH4的酸性热水洗涤多次(约200mL),以洗去糖等物质。若有天然色
素,用甲醇-甲酸溶液洗涤1次~3次,每次20mL,至洗液无色为止。再用70℃的水多次洗涤至流出液
中性。洗涤过程应充分搅拌然后用乙醇-氨水溶液分次解吸色素,收集全部解吸液,于水浴上驱除氨,蒸
发至2mL左右,转入5mL的容量瓶中,用50%的乙醇分次洗涤蒸发皿,洗涤液并入5mL的容量瓶
中,用50%的乙醇定容至刻度。此液留作纸色谱用。
5.1.3 糕点:称取10g(精确到0.001g)已粉碎的样品,加入30mL石油醚提取脂肪,共提三次,然后用
电吹风吹干,倒入漏斗中,用乙醇-氨解吸色素,解吸液于水浴上蒸发至20mL,加入1mL的钨酸钠溶液
沉淀蛋白,真空抽滤,用乙醇-氨解吸滤纸上的诱惑红,然后将滤液于水浴上挥去氨,调pH呈酸性,加
入0.5g~1.0g聚酰胺粉吸附色素,将吸附色素的聚酰胺粉全部转到漏斗中过滤,用pH4的酸性热水
洗涤多次(约200mL),以洗去糖等物质。若有天然色素,用甲醇-甲酸溶液洗涤1次~3次,每次
20mL,至洗液无色为止。再用70℃的水多次洗涤至流出液中性。洗涤过程应充分搅拌然后用乙醇-
氨水溶液分次解吸色素,收集全部解吸液,于水浴上驱除氨,蒸发至2mL左右,转入5mL的容量瓶中,
用50%的乙醇分次洗涤蒸发皿,洗涤液并入5mL的容量瓶中,用50%的乙醇定容至刻度。此液留作
纸色谱用。
5.1.4 冰淇淋:称取10g(精确到0.001g)已均匀的试样于烧杯中,加入20g海沙15mL石油醚提取脂
肪,提取2次,倾去石油醚,然后在50℃的水浴上挥去石油醚,再加入乙醇-氨解吸液解吸诱惑红,解吸
液倒入100mL的蒸发皿中,直至解吸液无色。将解吸液在水浴上挥去乙醇,使体积约为20mL时,加
入1mL硫酸(1+10),1mL钨酸钠溶液沉淀蛋白,放置2min,然后用乙醇-氨调至pH呈碱性,将溶液
性,加入0.5g~1.0g聚酰胺粉吸附色素,将吸附色素的聚酰胺粉全部转到漏斗中过滤,用pH4的酸性
热水洗涤多次(约200mL),以洗去糖等物质。若有天然色素,用甲醇-甲酸溶液洗涤1次~3次,每次
20mL,至洗液无色为止。再用70℃的水多次洗涤至流出液中性。洗涤过程应充分搅拌然后用乙醇-
氨水溶液分次解吸色素,收集全部解吸液,于水浴上驱除氨,蒸发至2mL左右,转入5mL的容量瓶中,
用50%的乙醇分次洗涤蒸发皿,洗涤液并入5mL的容量瓶中,用50%的乙醇定容至刻度。此液留作
纸色谱用。
5.2 定性
取层析纸,在距底边2cm起始线上分别点3μL~10μL的样品处理液、1μL诱惑红标准使用液,
分别挂于盛有展开剂1、展开剂2、展开剂3的展开槽中,用上行法展开,待溶剂前沿展至15cm处,将滤
5.3 定量
5.3.1 标准曲线的制备
吸取0.0mL、0.2mL、0.4mL、0.6mL、0.8mL、1.0mL诱惑红标准使用液,分别置于10mL比色
管中,各加水稀释到刻度,浓度分别为0μg/mL、2μg/mL、4μg/mL、6μg/mL、8μg/mL、10μg/mL。
用1mL比色杯,以零管调零点,于波长500nm处,测定吸光度,绘制标准曲线。
5.3.2 样品的测定
取色谱用纸,在距离底边2cm的起始线上,点0.20mL样品处理液,从左到右点成条状。纸的右
边点诱惑红的标准溶液1μL,依法展开,取出晾干。将样品的色带剪下,用少量热水洗涤数次,洗液移
入10mL的比色管中,加水稀释至刻度,混匀后,与标准管同时在500nm处,测定吸光度。
GB 5009.141-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Determination of allura red in foods
ISSUED ON. AUGUST 31, 2016
IMPLEMENTED ON. MARCH 01, 2017
Issued by. National Health and Family Planning commission
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle... 4
3 Reagents and materials ... 4
4 Instruments and equipment ... 6
5 Analytical procedures ... 6
6 Expression of analytical results ... 9
7 Precision... 9
8 Others ... 9
National food safety standard -
Determination of allura red in foods
1 Scope
This standard specifies the determination method of allura red in soft drinks,
hard candy, cakes and ice cream.
This standard applies to the determination of allura red in soft drinks, hard candy,
cakes and ice cream.
2 Principle
The allura red is adsorbed by the polyamide powder under acidic conditions,
and desorbed under alkaline conditions, then it is separated by paper
chromatography, and qualitatively and quantitatively compared with the
standard.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are of analytical
grade and the water is the grade I water as specified in GB/T 6682.
3.1 Reagents
3.1.1 Methanol (CH3OH).
3.1.2 petroleum ether. boiling range 30 °C ~ 60 °C.
3.1.3 Sulfuric acid (H2SO4). excellent grade pure.
3.1.4 Ethanol (CH3CH2OH).
3.1.5 Ammonia (NH3 • H2O). 20% ~ 25%.
3.1.6 Citric acid (C6H8O7 • H2O).
3.1.7 Sodium tungstate (Na2WO4 • H2O).
3.1.8 Butanone (C4H8O).
3.1.9 Sodium citrate (C6H5Na3O7).
converted in accordance with the actual purity of allura red), USE water to
dissolve and make its volume reach to 25 mL, the allura red concentration is
1.0 mg/mL.
3.4.2 Allura red standard use solution (0.1 mg/mL). PIPETTE 5.0 mL of allura
red standard stock solution in a 50 mL volumetric flask, ADD water to dilute it
to 50 mL.
4 Instruments and equipment
4.1 Visible spectrophotometer.
4.2 Electronic balance. The sensitivity is 0.001 g and 0.0001 g.
4.3 Microinjector. 10 μL, 50 μL.
4.4 Developer tank
4.5 Electric blower.
4.6 Centrifuge.
4.7 Constant temperature water bath.
5 Analytical procedures
5.1 Specimen preparation
5.1.1 Soft water. After heating the sample to remove carbon dioxide, WEIGH
10 g (accurate to 0.001 g) of sample in a beaker, then USE 20% citric acid to
adjust the pH to acidity, ADD 0.5 g ~ 1.0 g of polyamide powder to absorb the
pigment, TRANSFER polyamide powder adsorbing the pigment into a funnel
for filtration, USE acidic hot water at pH4 to rinse it for many times (about 200
mL), to wash away sugar and the like. If there is a natural pigment, USE
methanol-formic acid solution to rinse it for 1 ~ 3 times, 20 mL for each rinsing,
until the rinsing solution is colorless. Then USE water at 70 °C to make multiple
rinsing until the flowing out solution is neutral. In the rinsing process, it shall fully
mix it and then use ethanol-ammonia solution to desorb the pigment for many
bath, EVAPORATE it to about 2 mL, TRANSFER it to a 5 mL volumetric flask,
USE 50% ethanol to rinse the evaporating dish for many times. CONTAIN the
rinsing solution into a 5 mL volumetric flask, USE 50% ethanol to make its
volume to the mark. This solution is retained for paper chromatography.
5.1.2 Hard candy. WEIGH 10 g (accurate to 0.001g) of the pulverized sample,
ADD 30 mL of water, HEAT to dissolve it. If the pH of the sample solution is
to precipitate the protein, LET it be standing for 2 min, then USE ethanol-
ammonia to adjust pH to alkaline. TRANSFER the solution into a centrifuge
tube, CENTRIFUGE it at 5000 r/min for 15 min, POUR out the supernatant,
adjust pH to acidity, ADD 0.5 g ~ 1.0 g of polyamide powder to absorb the
pigment, TRANSFER polyamide powder adsorbing the pigment into a funnel
for filtration, USE acidic hot water at pH4 to rinse it for many times (about 200
mL), to wash away sugar and the like. If there is a natural pigment, USE
methanol-formic acid solution to rinse it for 1 ~ 3 times, 20 mL for each rinsing,
until the rinsing solution is colorless. Then USE water at 70 °C to make multiple
rinsing until the flowing out solution is neutral. In the rinsing process, it shall fully
mix it and then use ethanol-ammonia solution to desorb the pigment for many
times, COLLECT all the desorption solution, REMOVE the ammonia on a water
USE 50% ethanol to rinse the evaporating dish for many times. CONTAIN the
rinsing solution into a 5 mL volumetric flask, USE 50% ethanol to make its
volume to the mark. This solution is retained for paper chromatography.
5.2 Qualitative
TAKE the chromatographic paper, ADD 3 μL ~ 10 μL of sample treatment
solution and 1 μL of allura red standard use solution on the 2 cm starting line
from the bottom edge, respectively, HANG it on the developer tank containing
the developer 1, the developer 2, and the developer 3. USE the up-rising
method to extend it, when the front edge of the reagent reaches to the position
the standard spot for qualitative.
5.3 Quantification
5.3.1 Preparation of standard curve
PIPETTE 0.0 mL, 0.2 mL, 0.4 mL, 0.6 mL, 0.8 mL, 1.0 mL allura red standard
use solution, respectively, PLACE it in a 10 mL colorimetric tube respectively,
ADD water to each tube to dilute it to the mark, the concentration is respectively
0 μg/mL, 2 μg/mL, 4 μg/mL, 6 μg/mL, 8 μg/mL, and 10 μg/mL. USE a 1 mL
cuvette, USE a zero tube to adjust the zero point, at the wavelength of 500 nm,
DETERMINE the absorbance and DRAW the standard curve.
TAKE the chromatographic paper and ADD 0.20 mL of sample treatment
solution on the starting line 2 cm from the bottom edge, in the shape of a strip
from left to right. ADD 1 μL of allura red standard solution at the right side of the
paper, UNFLOD it as required, TAKE it out and DRY it naturally. CUT off the
color strip of the sample, USE a small amount of hot water to rinse it for many
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