GB 5009.263-2016 (GB5009.263-2016) & related versions
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Determination of Aspartame and Alitame in Foods
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GB 5009.263-2016
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GB 5009.263-2016: PDF in English
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
containing the fruit pulp, it is necessary to use a food processor for homogenization.
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.
5.1.4 Vegetables and their products, fruits and their products, edible fungi and
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
20min through ultrasonic vibration; stand for 1min; centrifuge for 5min at 4000r/min;
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
4.6mm, particle size of 5µm.
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
working solution as the abscissa, while the peak area (peak height) as the ordinate;
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.
......
| Standard ID | GB 5009.263-2016 (GB5009.263-2016) | | Description (Translated English) | Determination of Aspartame and Alitame in Foods | | Sector / Industry | National Standard | | Classification of Chinese Standard | X09 | | Word Count Estimation | 7,787 | | Date of Issue | 2016-12-23 | | Date of Implementation | 2017-06-23 | | Older Standard (superseded by this standard) | GB/T 22253-2008; GB/T 22254-2008 | | Regulation (derived from) | National Health and Family Planning Commission Notice No.17 of 2016 |
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