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食品安全国家标准 食品中苯甲酸、山梨酸和糖精钠的测定
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GB 5009.28-2016
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标准编号: GB 5009.28-2016 (GB5009.28-2016)
中文名称: 食品安全国家标准 食品中苯甲酸、山梨酸和糖精钠的测定
英文名称: National Food Safety Standard -- Determination of Benzoic Acid, Sorbic Acid and Saccharin Sodium in Foods
行业: 国家标准
中标分类: X09
字数估计: 10,114
发布日期: 2016-12-23
实施日期: 2017-06-23
旧标准 (被替代): GB 21703-2010; GB/T 23495-2009; GB/T 5009.28-2003; GB/T 5009.29-2003; SB/T 10389-2004; SN/T 2012-2007
标准依据: National Health and Family Planning Commission Notice No.17 of 2016
GB 5009.28-2016: 食品安全国家标准 食品中苯甲酸、山梨酸和糖精钠的测定
GB 5009.28-2016 英文名称: National Food Safety Standard -- Determination of Benzoic Acid, Sorbic Acid and Saccharin Sodium in Foods
中华人民共和国国家标准
食品安全国家标准
1 范围
本标准规定了食品中苯甲酸、山梨酸和糖精钠测定的方法。
本标准第一法适用于食品中苯甲酸、山梨酸和糖精钠的测定;第二法适用于酱油、水果汁、果酱中苯甲酸、山梨酸的测定。
第一法 液相色谱法
5 分析步骤
5.1 试样制备
取多个预包装的饮料、液态奶等均匀样品直接混合;非均匀的液态、半固态样品用组织匀浆机匀浆;
固体样品用研磨机充分粉碎并搅拌均匀;奶酪、黄油、巧克力等采用50℃~60℃加热熔融,并趁热充分
搅拌均匀。取其中的200g装入玻璃容器中,密封,液体试样于4℃保存,其他试样于-18℃保存。
5.2 试样提取
5.2.1 一般性试样
准确称取约2g(精确到0.001g)试样于50mL具塞离心管中,加水约25mL,涡旋混匀,于50℃水
浴超声20min,冷却至室温后加亚铁氰化钾溶液2mL和乙酸锌溶液2mL,混匀,于8000r/min离心
5min,将水相转移至50mL容量瓶中,于残渣中加水20mL,涡旋混匀后超声5min,于8000r/min离
心5min,将水相转移到同一50mL容量瓶中,并用水定容至刻度,混匀。取适量上清液过0.22μm滤膜,待液相色谱测定。
注:碳酸饮料、果酒、果汁、蒸馏酒等测定时可以不加蛋白沉淀剂。
5.2.2 含胶基的果冻、糖果等试样
准确称取约2g(精确到0.001g)试样于50mL具塞离心管中,加水约25mL,涡旋混匀,于70℃水
浴加热溶解试样,于50℃水浴超声20min,之后的操作同5.2.1。
5.2.3 油脂、巧克力、奶油、油炸食品等高油脂试样
准确称取约2g(精确到0.001g)试样于50mL具塞离心管中,加正己烷10mL,于60℃水浴加热
约5min,并不时轻摇以溶解脂肪,然后加氨水溶液(1+99)25mL,乙醇1mL,涡旋混匀,于50℃水浴
超声20min,冷却至室温后,加亚铁氰化钾溶液2mL和乙酸锌溶液2mL,混匀,于8000r/min离心
5min,弃去有机相,水相转移至50mL容量瓶中,残渣同5.2.1再提取一次后测定。
5.3 仪器参考条件
5.3.1 色谱柱:C18柱,柱长250mm,内径4.6mm,粒径5μm,或等效色谱柱。
5.3.2 流动相:甲醇+乙酸铵溶液=5+95。
5.3.3 流速:1mL/min。
5.3.4 检测波长:230nm。
5.3.5 进样量:10μL。
注:当存在干扰峰或需要辅助定性时,可以采用加入甲酸的流动相来测定,如流动相:甲醇+甲酸-乙酸铵溶液=
8+92,参考色谱图见图A.2。
5.4 标准曲线的制作
将混合标准系列工作溶液分别注入液相色谱仪中,测定相应的峰面积,以混合标准系列工作溶液的
质量浓度为横坐标,以峰面积为纵坐标,绘制标准曲线。
5.5 试样溶液的测定
将试样溶液注入液相色谱仪中,得到峰面积,根据标准曲线得到待测液中苯甲酸、山梨酸和糖精钠
(以糖精计)的质量浓度。
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 其他按取样量2g,定容50mL时,苯甲酸、山梨酸和糖精钠(以糖精计)的检出限均为0.005g/kg,定量
限均为0.01g/kg。
第二法 气相色谱法
9 原理试样经盐酸酸化后,用乙醚提取苯甲酸、山梨酸,采用气相色谱-氢火焰离子化检测器进行分离测
定,外标法定量。
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规定的一级水。
10.1 试剂
10.1.1 乙醚(C2H5OC2H5)。
10.1.2 乙醇(C2H5OH)。
10.1.3 正己烷(C6H14)。
10.1.4 乙酸乙酯(CH3CO2C2H5):色谱纯。
10.1.5 盐酸(HCl)。
10.1.6 氯化钠(NaCl)。
10.1.7 无水硫酸钠(Na2SO4):500℃烘8h,于干燥器中冷却至室温后备用。
10.2 试剂配制
10.2.1 盐酸溶液(1+1):取50mL盐酸,边搅拌边慢慢加入到50mL水中,混匀。
10.2.2 氯化钠溶液(40g/L):称取40g氯化钠,用适量水溶解,加盐酸溶液2mL,加水定容到1L。
10.2.3 正己烷-乙酸乙酯混合溶液(1+1):取100mL正己烷和100mL乙酸乙酯,混匀。
10.3 标准品
10.3.1 苯甲酸(C6H5COOH,CAS号:65-85-0),纯度≥99.0%,或经国家认证并授予标准物质证书的标准物质。
10.3.2 山梨酸(C6H8O2,CAS号:110-44-1),纯度≥99.0%,或经国家认证并授予标准物质证书的标准物质。
10.4 标准溶液配制
10.4.1 苯甲酸、山梨酸标准储备溶液(1000mg/L):分别准确称取苯甲酸、山梨酸各0.1g(精确到
0.0001g),用甲醇溶解并分别定容至100mL。转移至密闭容器中,于-18℃贮存,保存期为6个月。
10.4.2 苯甲酸、山梨酸混合标准中间溶液(200mg/L):分别准确吸取苯甲酸、山梨酸标准储备溶液各
10.0mL于50mL容量瓶中,用乙酸乙酯定容。转移至密闭容器中,于-18℃贮存,保存期为3个月。
10.4.3 苯甲酸、山梨酸混合标准系列工作溶液:分别准确吸取苯甲酸、山梨酸混合标准中间溶液0mL、
0.05mL、0.25mL、0.50mL、1.00mL、2.50mL、5.00mL和10.0mL,用正己烷-乙酸乙酯混合溶剂(1+
1)定容至10mL,配制成质量浓度分别为0mg/L、1.00mg/L、5.00mg/L、10.0mg/L、20.0mg/L、
50.0mg/L、100mg/L和200mg/L的混合标准系列工作溶液。临用现配。
10.5 材料
塑料离心管:50mL。
11 仪器和设备
11.1 气相色谱仪:带氢火焰离子化检测器(FID)。
11.2 分析天平:感量为0.001g和0.0001g。
11.3 涡旋振荡器。
11.4 离心机:转速 >8000r/min。
11.6 氮吹仪。
12 分析步骤
12.1 试样制备
取多个预包装的样品,其中均匀样品直接混合,非均匀样品用组织匀浆机充分搅拌均匀,取其中的
200g装入洁净的玻璃容器中,密封,水溶液于4℃保存,其他试样于-18℃保存。
12.2 试样提取
准确称取约2.5g(精确至0.001g)试样于50mL离心管中,加0.5g氯化钠、0.5mL盐酸溶液(1+
1)和0.5mL乙醇,用15mL和10mL乙醚提取两次,每次振摇1min,于8000r/min离心3min。每
次均将上层乙醚提取液通过无水硫酸钠滤入25mL容量瓶中。加乙醚清洗无水硫酸钠层并收集至约
吹至干,加入2mL正己烷-乙酸乙酯(1+1)混合溶液溶解残渣,待气相色谱测定。
12.3 仪器参考条件
12.3.1 色谱柱:聚乙二醇毛细管气相色谱柱,内径320μm,长30m,膜厚度0.25μm,或等效色谱柱。
12.3.2 载气:氮气,流速3mL/min。
12.3.3 空气:400L/min。
12.3.4 氢气:40L/min。
12.3.5 进样口温度:250℃。
12.3.6 检测器温度:250℃。
12.3.7 柱温程序:初始温度80℃,保持2min,以15℃/min的速率升温至250℃,保持5min。
12.3.9 分流比:10∶1。
12.4 标准曲线的制作
将混合标准系列工作溶液分别注入气相色谱仪中,以质量浓度为横坐标,以峰面积为纵坐标,绘制标准曲线。
12.5 试样溶液的测定
将试样溶液注入气相色谱仪中,得到峰面积,根据标准曲线得到待测液中苯甲酸、山梨酸的质量浓度。
13 分析结果的表述
14 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%。
15 其他取样量2.5g,按试样前处理方法操作,最后定容到2mL时,苯甲酸、山梨酸的检出限均为0.005g/kg,定量限均为0.01g/kg。
GB 5009.28-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Determination of Benzoic
Acid, Sorbic Acid and Saccharin Sodium in Foods
ISSUED ON. DECEMBER 23, 2016
IMPLEMENTED ON. JUNE 23, 2017
Issued by. National Health and Family Planning Commission of the
People's Republic of China;
China Food and Drug Administration.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Instruments and Apparatus ... 6
5 Analysis Steps ... 7
6 Expression of Analysis Results ... 8
7 Precision ... 9
8 Others ... 9
9 Principle ... 9
10 Reagents and Materials ... 9
11 Instruments and Apparatus ... 11
12 Analysis Steps ... 11
13 Expression of Analysis Results ... 12
14 Precision ... 13
15 Others ... 13
Appendix A - Liquid Chromatogram of Benzoic Acid, Sorbic Acid and Saccharin
Sodium ... 14
Appendix B - Gas Chromatogram of Standard Solutions of 100mg/L Benzoic
Acid, Sorbic Acid and Saccharin Sodium ... 15
National Food Safety Standard - Determination of Benzoic
Acid, Sorbic Acid and Saccharin Sodium in Foods
1 Scope
This Standard specifies the determination method for benzoic acid, sorbic acid AND
sodium saccharin in foods.
The first method of this Standard is applicable to the determination of benzoic acid,
sorbic acid AND saccharin sodium in foods; the second method is applicable to the
determination of benzoic acid and sorbic acid in soy sauce, fruit juice AND jam.
First method – Liquid chromatography
2 Principle
Use water to extract the sample; use n-hexane to degrease high-fat sample; use
protein precipitation agent to precipitate the protein of high-protein sample; adopt liquid
chromatography to perform separation; use UV detector to perform detection; use
external standard method to determine the quantity.
3 Reagents and Materials
Unless otherwise stated, the used reagents in this method shall all be analytical purity;
the water shall be the Grade-1 water which is specified in GB/T 6682.
3.1 Reagents
3.1.1 Ammonia (NH3·H2O).
3.1.2 Potassium ferrocyanide [K4Fe(CN)6·3H2O].
3.1.3 Zinc acetate [Zn(CH3COO)2·2H2O].
3.1.4 Anhydrous ethanol (CH3CH2OH).
3.1.5 N-hexane (C6H14).
3.1.6 Methanol (CH3OH). chromatographic purity.
5 Analysis Steps
5.1 Preparation of sample
Take a plurality of prepackaged homogeneous samples, such as beverages and liquid
milk, etc.; mix them directly; use tissue homogenizer to homogenize the non-
homogeneous-liquid and semi-solid samples; use grinder to fully comminute and stir
the solid sample evenly; perform heating and melting - 50°C ~ 60°C - for cheese, butter
AND chocolate, etc.; when it is hot, stir it evenly. Take 200g of it into a glass container
and seal it. The liquid sample shall be stored at 4°C; the rest sample shall be stored at
-18°C.
5.2 Sample’s extraction
5.2.1 General Samples
Accurately weigh and take about 2g (accurate to 0.001g) of sample in a 50mL
stoppered centrifuge tube; add about 25mL of water; vortex-mix it; in 50°C water bath,
sonicate it for 20min; cool it to room temperature; then, add 2mL of potassium
8000r/min for 5min; transfer the aqueous phase into a 50mL volumetric flask; add
20mL of water in the residue; vortex-mix it; then sonicate it for 5min; centrifuge it at
8000r/min for 5min; transfer the aqueous phase into the same 50mL volumetric flask;
use water to dilute it to the scale; mix it evenly. Take appropriate amount of supernatant
to pass the 0.22μm filter; wait for the determination of liquid chromatography.
Note. When carbonated drinks, fruit wines, fruit juices and distilled spirits, etc. are determined, protein
precipitants may not be added.
5.2.2 Samples of gum-base jelly and candy, etc.
Accurately weigh and take about 2g (accurate to 0.001g) of sample in a 50mL
heat and dissolve the sample; in 50°C water bath, sonicate it for 20min. Subsequent
operations shall be the same as those in 5.2.1.
5.2.3 High-fat sample such as fat, chocolate, butter and fried food, etc.
Accurately weigh and take about 2g (accurate to 0.001g) of sample in a 50mL
stoppered centrifuge tube; add 10mL of n-hexane; in 60°C water bath, heat it for 5min;
gently and occasionally shake it to dissolve fat; then add 25mL of ammonia solution
(1+99) AND 1mL of ethanol; vortex-mix them; in 50°C water bath, sonicate it for 20min;
cool it to room temperature; add 2mL of potassium ferrocyanide solution AND 2mL of
zinc acetate solution; mix them evenly; at 8000r/min 5min, centrifuge it for 5min;
10.1.2 Ethanol (C2H5OH).
10.1.3 N-hexane (C6H14).
10.1.4 Ethyl acetate (CH3CO2C2H5). chromatographic purity.
10.1.5 Hydrochloric acid (HCl).
10.1.6 Sodium chloride (NaCl).
10.1.7 Anhydrous sodium sulfate (Na2SO4). at 500°C, dry for 8 hours; in desiccator,
after it is cooled to room temperature, it shall be set for standby application.
10.2 Preparation of reagent
10.2.1 Hydrochloric acid solution (1+1). take 50mL of hydrochloric acid; at the time of
10.2.2 Sodium chloride solution (40g/L). weigh 40g of sodium chloride; use proper
amount of water to dissolve with; add 2mL of hydrochloric acid solution; add water to
set the constant volume to 1L.
10.2.3 N-hexane-ethyl acetate mixed solution (1+1). take 100 mL of n-hexane AND
100 mL of ethyl acetate; mix them evenly.
10.3 Standard products
10.3.1 Benzoic acid (C6H5COOH, CAS No.. 65-85-0). the purity shall be ≥ 99.0%; OR
the standard substance which is certified by the country AND granted for standard
substance certificate.
standard substance which is certified by the country AND granted for standard
substance certificate.
10.4 Preparation of standard solution
10.4.1 Benzoic acid AND sorbic acid standard stock solution (1000mg/L). respectively
and accurately weigh and take 0.1g of benzoic acid AND sorbic acid (accurate to
0.0001g); use methanol to dissolve them AND dilute them to 100 mL respectively;
Transfer them into a sealed container; at -18°C, store it. The preservation period shall
be 6 months.
10.4.2 Mixed standard intermediate-solution (200mg/L) of benzoic acid AND sorbic
standard stock solution into a 50mL volumetric flask; use ethyl acetate to dilute to
constant volume. Transfer it into a sealed container; at -18°C, store it. The preservation
anhydrous sodium sulfate. Add ethyl ether to wash the anhydrous-sodium-sulfate layer;
collect it to the scale of about 25mL; finally, use diethyl ether to set the constant volume;
mix it evenly. Accurately pipette 5mL of ethyl ether in a 5mL stoppered test tube; at
35°C, use nitrogen to blow it until dryness; add 2mL of n-hexane-ethyl acetate (1+1)
mixed solution to dissolve the residue; wait for the determination of gas
chromatography.
12.3 Reference conditions of instruments
column; inner diameter - 320μm; length - 30 m; membrane’s thickness - 0.25μm; OR
the chromatographic column with equivalent performance.
12.3.2 Carrier gas. nitrogen; flow rate - 3mL/min.
12.3.3 Air. 400L/min.
12.3.4 Hydrogen. 40L/min.
12.3.5 Inlet temperature. 250°C.
12.3.6 Detector temperature. 250°C.
12.3.7 Column temperature program. the initial temperature is 80 °C; hold for 2min; at
a rate of 15°C/min, it shall be heated to 250°C; hold for 5min.
12.3.9 Split ratio. 10.1.
12.4 Preparation for standard curves
Respectively inject the mixed-standard-series working solution into the liquid
chromatograph; treat the mass concentration as abscissa AND treat the peak area as
ordinate; draw the standard curve.
12.5 Determination of sample solution
Inject the sample solution into the liquid chromatograph; obtain the peak area;
according to the standard curve, obtain the mass concentration of benzoic acid and
sorbic acid in test solution.
Content of benzoic acid and sorbic acid in sample shall be calculated according to
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