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食品安全国家标准 食品中阿斯巴甜和阿力甜的测定
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GB 5009.263-2016
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标准编号: GB 5009.263-2016 (GB5009.263-2016)
中文名称: 食品安全国家标准 食品中阿斯巴甜和阿力甜的测定
英文名称: Determination of Aspartame and Alitame in Foods
行业: 国家标准
中标分类: X09
字数估计: 7,762
发布日期: 2016-12-23
实施日期: 2017-06-23
旧标准 (被替代): GB/T 22253-2008; GB/T 22254-2008
标准依据: National Health and Family Planning Commission Notice No.17 of 2016
GB 5009.263-2016: 食品安全国家标准 食品中阿斯巴甜和阿力甜的测定
GB 5009.263-2016 英文名称: Determination of Aspartame and Alitame in Foods
中华人民共和国国家标准
GB 5009.265-2016
1 范围
本标准规定了食品中多环芳烃(萘、苊、芴、菲、蒽、荧蒽、芘、苯并[a]蒽、 、苯并[b]荧蒽、苯并[k]荧
蒽、苯并[a]芘、茚并[1,2,3-c,d]芘、二苯并[a,h]蒽和苯并[g,h,i]苝的液相色谱测定方法和食品中
多环芳烃(萘、苊烯、苊、芴、菲、蒽、荧蒽、芘、苯并[a]蒽、 、苯并[b]荧蒽、苯并[k]荧蒽、苯并[a]芘、茚
并[1,2,3-c,d]芘、二苯并[a,h]蒽和苯并[g,h,i]苝的气相色谱-质谱测定方法。本标准适用于食品中多环芳烃含量的测定。
第一法 高效液相色谱法
5 分析步骤
5.1 试样制备
5.1.1 干样:取样品约500g,经粉碎机粉碎、混匀,分装于洁净盛样袋中,密封标识后于-18℃冷冻保存。
5.1.2 湿样:取样品约500g,将其可食部分先切碎,经均质器充分搅碎均匀,分装于洁净盛样袋中,密封标识后于-18℃冷冻保存。
5.2 试样提取
5.2.1 粮谷或水分少的食品称取2g~5g(精确至0.01g)试样于50mL具塞玻璃离心管A中,按以下步骤处理:
a) 加入10mL正己烷,涡旋振荡30s后,放入40℃水浴超声30min;以4500r/min离心5min,
吸取上清液于玻璃离心管B中;离心管A下层用10mL正己烷重复提取1次,提取液合并于
离心管B中,氮吹(温度控制在35℃以下)除去溶剂,吹至近干。
b) 在离心管B中,加入4mL乙腈,涡旋混合30s,再加入900mg硫酸镁、100mgPSA和100mg
C18填料,涡旋混合30s,以4500r/min离心3min,取上清液于10mL玻璃刻度离心管C中,
离心管B下层再用2mL乙腈重复提取1遍,合并提取液于离心管C中,氮吹蒸发溶剂至近
1mL,用乙腈定容至1mL,混匀后,过0.22μm有机相型微孔滤膜,制得试样待测液。
5.2.2 水产品、肉类和蔬菜等食品
称取2g~5g(精确至0.01g)试样于50mL具塞玻璃离心管A中,加1g~5g硅藻土,用玻棒搅
匀,以下按5.2.1中a)、b)步骤处理,制得试样待测液。
5.2.3 含油脂高的食品或动植物油脂
称取1g~4g(精确至0.01g)试样于50mL具塞玻璃离心管A中,按以下步骤处理:
a) 加入20mL乙腈和10mL乙腈饱和的正己烷,涡旋振荡30s后,放入40℃水浴超声30min;
摇匀后,以4500r/min冷冻(-4℃)离心5min,吸取下层乙腈层于100mL鸡心瓶中,离心
管A中溶液用20mL乙腈重复提取1次,提取液合并于鸡心瓶中,35℃减压旋转蒸发至近
干。加入5mL正己烷,涡旋振荡30s溶解。
b) 依次用5mL二氯甲烷和10mL正己烷活化弗罗里硅土固相萃取柱,将a)获得的5mL提取样
液全部移入弗罗里硅土固相萃取柱,再用5mL正己烷洗涤鸡心瓶并入柱中,用8mL正己烷-
二氯甲烷混合溶液洗脱,收集所有流出物于20mL玻璃离心管B中。氮吹(温度控制在35℃
以下)除去溶剂,吹至近干,加入0.5mL乙腈涡旋振荡10s,继续氮吹至除尽正己烷-二氯甲
烷,用乙腈定容至1mL,混匀后,过0.22μm有机相型微孔滤膜,制得试样待测液。
5.3 液相色谱参考条件
a) 色谱柱:PAHC18反相键合固定相色谱柱,柱长250mm,内径4.6mm,粒径5μm,或同等性能的色谱柱。
b) 检测器:荧光检测器。
c) 流动相:乙腈和水;梯度洗脱程序见表1,溶剂A为乙腈,溶剂B为水。
5.4 标准曲线的制作
将标准系列工作液分别注入液相色谱仪中,测得相应的峰面积,以标准工作液的质量浓度为横坐
标、以峰面积为纵坐标,绘制标准曲线。标准溶液的液相色谱图参见图A.1。
5.5 试样溶液的测定
将试样待测液注入液相色谱仪中,以保留时间定性,测得相应的峰面积,根据标准曲线得到试样待
测液中多环芳烃的质量浓度。如果试样待测液中被测物质的响应值超出仪器检测的线性范围,可适当稀释后测定。
5.6 空白试验空白试验除不加试样外,采用与试样完全相同的分析步骤。
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20%。
8 其他当试样取4g,定容体积为1mL时,本方法的检出限和定量限见表3。
9 原理
试样中的多环芳烃用有机溶剂提取,提取液浓缩至近干,用PSA(N-丙基乙二胺)和C18固相萃取填
料净化或用弗罗里硅土固相萃取柱净化,经浓缩定容后,用气相色谱-质谱联用仪进行测定,外标法定量。
12.3 空白试验
空白试验除不加试样外,采用与试验完全相同的分析步骤。
12.4 气相色谱-质谱参考条件
a) 色谱柱:DB-5MS,柱长30m,内径0.25mm,膜厚0.25μm,或同等性能的色谱柱。
b) 柱温度程序:初始温度90℃,以20℃/min升温至220℃,再以5℃/min升温至320℃,保持2min;
c) 进样口温度:250℃;
d) 色谱-质谱接口温度:280℃;
e) 离子源温度:230℃;
f) 载气:氦气,纯度≥99.999%,1.0mL/min;
g) 电离方式:EI;
h) 电离能量:70eV;
i) 质量扫描范围:50amu~450amu;
j) 测定方式:选择离子监测方式;
k) 进样方式:不分流进样,2.0min后开阀;
l) 进样量:1.0μL;
m) 溶剂延迟:3min。
12.5 标准曲线的制作
将标准系列工作液分别注入气相色谱-质谱仪中,测得相应的峰面积,以标准工作液的质量浓度为
横坐标、以峰面积为纵坐标,绘制标准曲线。
12.6 试样溶液的测定
将试样待测液注入气相色谱-质谱仪中,测得相应的峰面积,根据标准曲线得到试样待测液中多环
芳烃的质量浓度。如果试样待测液中被测物质的响应值超出仪器检测的线性范围,可适当稀释后测定。
12.7 定性
如果试样待测液中检出的色谱峰保留时间与标准工作溶液相一致,且选择离子的相对丰度与标准
工作溶液的相对丰度两者之差不大于允许相对偏差(相对丰度≥50%,允许±10%偏差;50% >相对丰
度 >20%,允许±15%偏差;10%< 相对丰度< 20%,允许±20%偏差;相对丰度≤10%,允许±50%偏
差),则可判断试样中存在对应的被测物。在上述色谱条件下,总离子流图参见图B.1。参考保留时间和特征离子见表4。
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20%。
15 其他
当试样取4g,定容体积为1mL时,本方法的检出限和定量限见表5。
GB 5009.263-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Standard of Food Safety -
Determination of Aspartame and Alitame in Foods
ISSUED ON. DECEMBER 23, 2016
IMPLEMENTED ON. JUNE 23, 2017
Issued by. National Health and Family Planning Commission of PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Apparatus ... 5
5 Analytical Procedures ... 5
6 Expression of Analytical Results ... 9
7 Precision ... 9
8 Others ... 9
Appendix A Chromatogram ... 11
National Standard of Food Safety -
Determination of Aspartame and Alitame in Foods
1 Scope
This Standard specifies the determination of aspartame and alitame in foods.
This Standard is applicable to the determination of aspartame and alitame in foods.
2 Principle
According to the characteristics that the aspartame and alitame are soluble in water,
while the methanol and ethanol are not soluble in the fat-soluble solvents, use aqueous
methanol solution to extract the samples of vegetables and their products, fruits and
their products, edible fungi and algae, cereals and their products, baked products,
puffed products and jellies under ultrasonic vibration conditions; use water to extract
the samples of concentrated juices, carbonated beverages, solid beverages, table
sauces and other candies except gum base candies; after the ethanol precipitates the
protein, use the aqueous ethanol solution to extract the samples of dairy products,
milk-containing beverages and frozen drinks; for gum base candies, use n-hexane to
dissolve gum base, then use water to extract; use water to extract the fat emulsified
products, cocoa products, chocolate and its products, nuts and seeds, aquatic
products, and egg products, then use n-hexane to remove the fat compositions.
Separate the extracting solutions on the liquid chromatography C18 reversed-phase
column; detect at a wavelength of 200nm; qualitative by retention time of the
chromatography peak; and quantitative by the external standard method.
3 Reagents and Materials
Unless otherwise specified, all used reagents shall be analytically pure; while the water
shall be Class-I water for laboratory as specified in GB/T 6682.
3.1 Reagents
3.1.1 Methanol (CH3OH). chromatographically pure.
3.1.2 Ethanol (CH3CH2OH). guarantee reagent.
20min; transfer the extracting solution into 25mL volumetric flask; add 10mL of water
again into the beaker, use ultrasonic vibrator to extract for 10min; transfer the
extracting solution into the same 25mL volumetric flask for later-use. Use water to
make constant volume against the above liquid in the volumetric; mix evenly; centrifuge
for 5minat 4000r/min; filter the supernatant through 0.45µm aqueous filter membrane
for the chromatographic analysis.
5.1.2 Dairy products, dairy drinks and frozen drinks
For the liquid-dairy products containing the slid fruit pulp, it is necessary to use a food
processor for homogenization; for the solid dairy products such as cheese, it is
necessary to use a food processor for homogenization according to the mass ratio of
1.4 between specimen and water.
Take about 5g (accurate to 0.001g) of homogenate specimen of liquid-dairy products,
milk-containing beverages, frozen drinks, solid dairy products into 50mL centrifuge
tube; add 10mL of ethanol; cover the lid; for the milk-containing beverage and frozen
drinks specimens, firstly, gently invert the centrifuge tube 5 times (not shaking); for
dairy products, firstly perform vortex mixing against the centrifuge tube for 10s, then
stand for 1min, centrifuge 5min at 4000r/min; filter the supernatant into a 25mL
volumetric flask; use 8mL of ethanol-water (2+1) to wash the precipitation; after
centrifuging, the supernatant is transferred into the same 25mL volumetric flask; use
the ethanol-water (2+1) to make constant volume; filter through a 0.45µm organic filter
membrane for the chromatographic analysis.
5.1.3 Jelly
For the suckable and transparent jellies, stir well with a glass rod; for the jellies
Take about 5g (accurate to 0.001g) of uniformly-prepared jelly specimen into a 50mL
colorimetric tube; add 25mL of 80% methanol aqueous solution; heat on the 70°C
water bath for 10min; take out the colorimetric tube; transfer the extracting solution into
a 50mL volumetric flask as it is hot; then use 15mL of 80% methanol aqueous solution
to wash the colorimetric tube for twice; each time shake it for about 10s; transfer into
the same 50mL volumetric flask; cool off to the room temperature; use 80% methanol
aqueous solution to make constant volume to the scale; mix evenly; centrifuge for 5min
at 4000r/min; filter the supernatant through a 0.45µm organic filter membrane for
chromatographic analysis.
algae
The specimen of fruits and their products shall first be removed if they have fruit core.
For the dry and hard specimen, use a food processor to homogenize the specimen
scale; after shaking evenly; filter through a 0.45µm aqueous filter membrane for the
chromatographic analysis.
Fat emulsified products, cocoa products, chocolate and its products, nuts and seeds,
aquatic products, egg products. use a food processor to homogenize according to the
mass ratio 1.4 between the specimen and water; take about 5g (accurate to 0.001g)
of homogenate specimen into a 25mL centrifuge tube; add 10mL of water to extract for
transfer the supernatant into a 100mL separator funnel; add 8mL of water into the
centrifuge tube to extract for 10min through ultrasonic vibration; after standing and
centrifuging, transfer the supernatant into the separator funnel; add 15mL of n-hexane
into the separator funnel; shake for 30s; stand and layer for 5min; place the lower
aqueous phase into a 25mL volumetric flask; use water to make constant volume to
the scale; after shaking evenly, filter through a 0.45µm aqueous filter membrane for
the chromatographic analysis.
5.2 Apparatus reference conditions
a) Chromatographic column. C18, column length of 250mm, inner diameter of
b) Column temperature. 30°C.
c) Mobile phase. methanol-water (40+60) or acetonitrile-water (20+80).
d) Flow rate. 0.8mL/min.
e) Sample-injection volume. 20µL.
f) Detector. diode array detector or UV detector.
g) Detection wavelength.200nm.
5.3 Drawing of standard curve
Measure the corresponding peak area (peak height) of the standard series of working
fluid under the above chromatographic conditions; take the concentration of standard
then draw the standard curve. The standard chromatograms are shown in Appendix A.
5.4 Measurement of specimen solution
Under the same liquid chromatographic conditions, inject the specimen solution into
the liquid chromatograph; qualitative with retention time; quantitative with comparison
between the specimen peak height or peak area and the standard one.
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