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GB 5009.149-2016

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GB 5009.149-2016 英文版 500 购买 现货,9秒内自动发货PDF,有增值税发票。 食品安全国家标准 食品中栀子黄的测定 有效

   
标准编号: GB 5009.149-2016 (GB5009.149-2016)
中文名称: 食品安全国家标准 食品中栀子黄的测定
英文名称: Determination of crocin in foods
行业: 国家标准
中标分类: X09
发布日期: 2016-12-23
实施日期: 2017-06-23
旧标准 (被替代): GB/T 5009.149-2003
标准依据: National Health and Family Planning Commission Notice No.17 of 2016

GB 5009.149-2016
Determination of crocin in foods
中华人民共和国国家标准
食品安全国家标准
食品中栀子黄的测定
2016-12-23发布
2017-06-23实施
中华人民共和国国家卫生和计划生育委员会
国 家 食 品 药 品 监 督 管 理 总 局 发 布
前言
本标准代替GB 5009.149-2003《食品中栀子黄的测定》。
本标准与GB 5009.149-2003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中栀子黄的测定”;
---原标准第一法高效液相色谱法测定栀子苷修改为高效液相色谱法测定藏花素和藏花酸;
---改进了样品前处理分析方法;
---扩大了方法适用范围;
---删除了第二法 薄层色谱法。
食品安全国家标准
食品中栀子黄的测定
1 范围
本标准规定了食品中栀子黄的代表性成分:藏花素、藏花酸的测定方法。
本标准适用于冰淇淋、蜜饯、腌菜、干杏仁、巧克力、糕点、熟肉、酱油、果汁、配制酒、果冻、薯片中藏
花素和藏花酸的测定。
2 原理
试样用甲醇超声提取后,通过C18反相色谱柱分离,用高效液相色谱/可见光检测器于440nm下检
测栀子黄的主要显色成分藏花素和藏花酸,以保留时间定性,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。
3.1 试剂
3.1.1 甲醇(CH3OH):色谱纯。
3.1.2 乙腈(CH3CN):色谱纯。
3.1.3 冰乙酸(CH3COOH)。
3.1.4 乙酸铵(CH3COONH4)。
3.2 试剂配制
3.2.1 乙酸-乙酸铵溶液(pH=4):准确称取0.77g乙酸铵置于1L容量瓶内,加900mL水溶解,用冰
乙酸调节pH=4.0,加水定容至1L,混匀,经0.45μm微孔滤膜过滤后使用。
3.3 标准品
3.3.1 藏花素标准品(C44H64O24,CAS号:42553-65-1),纯度≥90.0%。
3.3.2 藏花酸标准品(C20H24O4,CAS号:27876-94-4),纯度≥90.0%。
3.4 标准溶液配制
3.4.1 藏花素标准储备液:准确称取5.00mg(精确至0.01mg)藏花素标准品,用甲醇溶解,转移到10mL
容量瓶中,用甲醇定容,混匀,藏花素浓度为0.5mg/mL,于4℃保存。
3.4.2 藏花酸标准储备液:准确称取1.00mg(精确至0.01mg)藏花酸标准品,用甲醇溶解,转移到10mL
容量瓶中,用甲醇定容,混匀,藏花酸浓度为0.1mg/mL,于4℃保存。
3.4.3 藏花素、藏花酸混合标准曲线工作液:分别均吸取藏花素标准储备液、藏花酸标准储备液0.05mL、
0.1mL、0.2mL、0.5mL、1.0mL于10mL容量瓶中,用甲醇定容,混匀,藏花素系列标准工作液浓度分
别均为2.5μg/mL、5μg/mL、10μg/mL、25μg/mL、50μg/mL,藏花酸系列标准工作液浓度分别均为
0.5μg/mL、1μg/mL、2μg/mL、5μg/mL、10μg/mL,于4℃保存。
4 仪器和设备
4.1 高效液相色谱仪,配置可见检测器。
4.2 分析天平:感量为0.01mg和0.01g。
4.3 离心机:转速≥5000r/min。
4.4 酸度计。
4.5 超声波清洗仪。
4.6 食品粉碎机。
4.7 有机相型微孔滤膜:孔径0.45μm。
5 分析步骤
5.1 试样制备及保存
5.1.1 液体样品
将饮料、酒类、酱油等样品摇匀分装,密闭常温或冷藏保存。
5.1.2 半固态样品
对果冻等样品取可食部分匀浆后,搅拌均匀,分装,密闭冷藏或冷冻保存。
5.1.3 固体样品
饼干、糕点、熟肉制品、可可制品等低含水量样品,经高速粉碎机粉碎、分装,于室温下避光密闭
保存。
5.2 试样处理
5.2.1 液体样品
称取2g(精确至0.01g)均匀试样(若试样中含二氧化碳应先超声除去)置于烧杯中,用适量甲醇溶
解并转移至25mL容量瓶中,加甲醇定容,摇匀。吸取1mL溶液过0.45μm有机滤膜,待测。
5.2.2 半固体试样及固体试样
称取2g(精确至0.01g)均匀试样于50mL离心管中,准确量取25mL甲醇溶液加入其中,超声
20min后涡旋2min,4000r/min离心10min,吸取1mL上清液过0.45μm有机滤膜,待测。
5.2.3 酱油
称取1g(精确至0.01g)均匀试样置于烧杯中,用适量甲醇溶解并转移至50mL容量瓶中,加甲醇
定容,摇匀。吸取1mL溶液过0.45μm有机滤膜,待测。
注:5.2过程应在避免强光照射的环境下进行。
5.3 仪器参考条件
仪器参考条件列出如下:
a) 色谱柱:C18色谱柱,柱长250mm,内径4.6mm,粒径5μm,或同等性能的色谱柱;
b) 流动相:A:乙酸-乙酸铵缓冲溶液,B:乙腈,梯度洗脱见表1;
d) 流速:1.0mL/min;
e) 检测波长:440nm。
表1 流动相及梯度洗脱条件
时间
min
流速
mL/min
流动相A
流动相B
1 1.0 80 20
8 1.0 40 60
8.1 1.0 30 70
13 1.0 2 98
15 1.0 80 20
20 1.0 80 20
5.4 标准曲线的制作
将混合标准工作液分别注入高效液相色谱仪中,测定藏花素和藏花酸相应的峰面积,以标准工作液
的浓度为横坐标,以色谱峰面积为纵坐标,绘制标准曲线(标准图谱见图A.1)。
将试样溶液注入高效液相色谱仪中,得到藏花素和藏花酸的峰面积,根据标准曲线得到待测液中藏
花素和藏花酸的浓度。
6 分析结果的表述
试样中藏花素和藏花酸的含量按式(1)计算:
X= ρ×
V×1000
m×1000×1000×
F (1)
式中:
ρ ---由标准曲线求得试样溶液中藏花素或藏花酸的浓度,单位为微克每毫升(μg/mL);
V ---样品溶液定容体积,单位为(mL);
1000---换算系数;
m ---最终样液代表的试样质量,单位为克(g);
F ---标准品的纯度折算系数。
计算结果保留两位有效数字。
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15%。
8 其他
他样品取样量为2.0g时,藏花素为12.5mg/kg,藏花酸为2.5mg/kg。
方法定量限(LOQ):酱油样品当称样量为1.0g时,藏花素为250mg/kg,藏花酸为50.0mg/kg,其
他样品取样量为2.0g时,藏花素为62.5mg/kg,藏花酸为12.5mg/kg。
附 录 A
藏花素和藏花酸的标准色谱图
藏花素和藏花酸标准色谱图见图A.1。
图A.1 藏花素和藏花酸的标准色谱图(藏花素浓度50μg/mL,藏花酸浓度10μg/mL)

GB 5009.149-2016
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Determination of Gardenia Yellow in Foods
食品安全国家标准
食品中栀子黄的测定
ISSUED ON: DECEMBER 23, 2016
IMPLEMENTED ON: JUNE 23, 2017
Issued by: National Health and Family Planning Commission of the PRC;
State Food and Drug Administration.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and materials ... 4
4 Instruments and apparatuses ... 5
5 Analysis steps ... 5
6 Description of the analysis result ... 7
7 Precision ... 8
8 Others ... 8
Appendix A Standard chromatogram of crocin and crocetin ... 9
National Food Safety Standard -
Determination of Gardenia Yellow in Foods
1 Scope
This Standard specifies the determination method of crocin and crocetin, the
representative components of gardenia yellow in food.
This Standard applies to the determination of crocin and crocetin in ice cream, candied
fruit, pickle, dried almond, chocolate, pastries, cooked meat, soy sauce, fruit juice,
mixed wine, jelly and potato chip.
2 Principle
The sample which is ultrasonically extracted by methanol, shall be separated by C18
reversed-phase chromatography / visible light detector to determine crocin and
crocetin, major color-developing components of gardenia yellow, at 440 nm. It is
characterized by retention time and quantified by external standard method.
3 Reagents and materials
Unless otherwise specified, all the reagents in this method are analytical reagents, the
water is grade-1 water which is specified by GB/T 6682.
3.1 Reagents
3.1.1 Methanol (CH3OH): chromatographic pure.
3.1.2 Acetonitrile (CH3CH): chromatographic pure.
3.1.3 Glacial acetic acid (CH3COOH).
3.1.4 Ammonium acetate (CH3COONH4).
3.2 Preparation of reagents
3.2.1 Acetic acid-ammonium acetate solution (pH=4): accurately weigh 0.77 g of
ammonium acetate in a 1 L volumetric flask; add 900 mL of water to dissolve; use
glacial acetic acid to adjust pH=4.0; add water to fix volume to 1 L; mix well. Use it
after it is filtered through a 0.45 μm microporous membrane.
5.1.1 Liquid sample
Shake well and pack the samples such as beverage, alcohol and soy sauce; seal and
store at room temperature or in a refrigerator.
5.1.2 Semi-solid sample
For samples such as jelly, take the edible portion to homogenate; stir evenly; package;
seal; refrigerate or freeze to store.
5.1.3 Solid sample
For samples of low-water content, such as biscuit, cake, cooked meat products and
cocoa products, use the high-speed pulverizer to pulverize; package; seal and store
at room temperature out of the sun.
5.2 Sample processing
5.2.1 Liquid sample
Weigh 2 g (accurate to 0.01 g) of uniform sample (carbon dioxide in the sample, if any,
shall be removed by ultrasound firstly) in a beaker; use an appropriate amount of
methanol to dissolve it; transfer it to a 25 mL volumetric flask; add methanol to fix
volume; shake well. Pipette 1 mL of the solution; filter it through a 0.45 μm organic
filter for testing.
5.2.2 Semi-solid and solid samples
Weigh 2 g (accurate to 0.01 g) of uniform sample in a 50 mL centrifuge tube; accurately
measure 25 mL of methanol solution into it; use ultrasound for 20 min and vortex for 2
min; centrifuge at 4 000 r/min for 10 min; absorb 1 mL of supernatant to filter through
a 0.45 μm organic filter membrane, which is for later test.
Weigh 1 g (accurate to 0.01 g) of uniform sample in a beaker; use an appropriate
amount of methanol to dissolve it; transfer it to a 50 mL volumetric flask; add methanol
to fix volume; shake well. Pipette 1 mL of the solution; filter it through a 0.45 μm organic
filter for testing.
Note: 5.2 shall be performed in an environment without strong light exposure.
5.3 Apparatus reference conditions
Apparatus reference conditions are listed as below:
a) Chromatographic column: C18 column with a column length of 250 mm, an inner
diameter of 4.6 mm, a particle size of 5 μm, or columns of equivalent performance;
ρ -- the concentration of crocin or crocetin in the sample solution that is obtained from
the standard curve, in micrograms per milliliter (μg/mL);
V -- the volumetric volume of the sample solution, in milliliters (mL);
1 000 -- conversion coefficient;
m -- the sample mass of the final sample, in grams (g);
F -- the purity conversion factor of the standard.
The calculation result shall keep two significant figures.
7 Precision
The absolute difference of two independent test results under repeatability cannot
8 Others
Method detection-limit (LOD): for soy sauce sample, when the sampling amount is 1.0
g, the crocin is 50 mg/kg, and the crocetin is 10.0 mg/kg; for other samples, when the
sampling amount is 2.0 g, the crocin is 12.5 mg/kg, the crocetin is 2.5 mg/kg.
Method quantitation-limit (LOQ): for soy sauce sample, when the sampling amount is
1.0 g, the crocin is 250 mg/kg, and the crocetin is 50.0 mg/kg; for other samples, when
the sampling amount is 2.0 g, the crocin is 62.5 mg/kg, the crocetin is 12.5 mg/kg.
   
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