GB 5009.279-2016 PDF in English
GB 5009.279-2016 (GB5009.279-2016) PDF English
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Determination of xylitol, sorbitol, maltitol in foods -- High-performance liquid chromatography
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Standards related to (historical): GB 5009.279-2016
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GB 5009.279-2016: PDF in English GB 5009.279-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Determination of
Xylitol, Sorbitol, Maltitol and Erythritol in Foods
ISSUED ON: DECEMBER 23, 2016
IMPLEMENTED ON: JUNE 23, 2017
Issued by: National Health and Family Planning Commission of the PRC;
China Food and Drug Administration.
Table of Contents
Foreword ... 3
1 Application Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Instruments and Apparatuses ... 5
5 Analysis Steps ... 6
6 Description of the Analysis Result ... 8
7 Precision ... 9
8 Others ... 9
9 Principle ... 9
10 Reagents and Materials ... 9
11 Instruments and Apparatuses ... 10
12 Analysis Steps ... 11
13 Description of the Analysis Result ... 13
14 Precision ... 13
15 Others ... 13
Appendix A High Performance Liquid Chromatography - Differential Refractive Index
Detection Chromatogram of Sugar Alcohol Standard Solution ... 14
Appendix B High Performance Liquid Chromatography - Evaporative Light Scattering
Detection Chromatogram of Sugar Alcohol Standard Solution ... 15
National Food Safety Standard - Determination of Xylitol,
Sorbitol, Maltitol and Erythritol in Foods
1 Application Scope
This Standard specifies the method to use high performance liquid chromatography -
differential refractive index detection and evaporative light scattering detection for the
test of xylitol, sorbitol, maltitol and erythritol in chewing gum, biscuit, pastry, bread and
beverage.
This Standard applies to the determination of the content of xylitol, sorbitol, maltitol
and erythritol in chewing gum, biscuit, pastry, bread and beverage.
Method 1 -- High Performance Liquid Chromatography -
Differential Refractive Index Detection.
2 Principle
After the protein is precipitated, filter the sample; put the supernatant into to the high
performance liquid chromatography, use amino chromatographic column or cation
exchange chromatographic column to separate; use differential refractive index
detector to test; use external standard method to fix-volume.
3 Reagents and Materials
Unless otherwise specified, all the reagents in this method are analytical reagents, the
water is grade-1 water specified by GB/T 6682.
3.1 Reagents
3.1.1 Acetonitrile (CH3CH): chromatographic purity.
3.1.2 Trichloroacetic acid (CCl3COOH).
3.1.3 Anhydrous sodium carbonate (Na2CO3).
3.2 Preparation of reagents
4.6 Ultrasonic cleaning machine: with a working frequency of 40 kHz and the power of
500 W.
5 Analysis Steps
5.1 Sample preparation and pretreatment
5.1.1 Chewing gum
Take at least 20 g of the chewing gum sample; use a blade to cut into small pieces;
put into a closed container to mix. Accurately weigh 2 g of chopped sample; place the
sample in a 50 mL centrifuge tube; add 40 mL of water; mix and heat in a water bath
at 80°C for 20 min; mix and shake every 6 min; take out and centrifuge at 9 000 r/min
for 10 min. Take 8 mL of supernatant in a 10 mL volumetric flask; add water to fix-
volume; shake well; filter through a 0.22 μm filter membrane; test on the machine.
5.1.2 Beverage
For non-protein beverages, take at least 200 mL of sample; mix well; place in a closed
container. Take 10 mL of beverage in a 50 mL volumetric flask; add water to fix-volume
to 50 mL; shake well; filter through a 0.22 μm filter membrane; test on the machine.
For protein beverages, take at least 200 mL of sample; place in a closed container to
mix well. Weigh 5 g of sample; place in a 50 mL volumetric flask; add 35 mL of water;
shake well; then sonicate for 30 min; shake it every 6 min; take out and centrifuge at
9 000 r/min for 10 min.
Precipitate protein: add 5 mL of trichloroacetic acid solution (100 g/L) into the
supernatant; shake it; then place it at room temperature for 30 min; centrifuge at 9 500
r/min for 10 min. Take 8 mL of the supernatant in a 10 mL volumetric flask; add water
to fix-volume. After shaking, take 850 μL of filtrate; add 150 μL of sodium carbonate
solution (21.2 g/L); shake and neutralize; or take 10 mL of supernatant; add 20 mL of
acetonitrile; shake well and place it at room temperature for 30 min; centrifuge at 9
500 r/min for 10 min; fix-volume the supernatant to 50 mL; shake well; filter through
0.22 μm microporous membrane; test on the machine.
Note: For samples with sugar alcohol content lower than the detection-limit after being
precipitated and diluted by acetonitrile, trichloroacetic acid shall be used for
precipitation. For samples with low erythritol content (≤1%), acetonitrile shall be used
for precipitation. In other cases, both methods are available.
5.1.3 Biscuit, pastry, bread
Take at least 200 g of sample; use a grinder to grind; put it into a closed container to
mix. Weigh 1 g ~ 5 g of pulverized sample; place it in a 50 mL centrifuge tube; add 40
mL of water; shake it; then sonicate for 30 min; shake it every 6 min; take out and
10.3 Standard
10.3.1 Xylitol (C5H12O5, CAS No.: 87-99-0), with a purity ≥ 99%, or a standard
substance certified by the state and awarded with a standard substance certificate.
10.3.2 Sorbitol (C6H14O6, CAS No.: 50-70-4), with a purity ≥ 99%, or a standard
substance certified by the state and awarded with a standard substance certificate.
10.3.3 Maltitol (C12H24O11, CAS No.: 585-88-6), with a purity ≥ 99%, or a standard
substance certified by the state and awarded with a standard substance certificate.
10.3.4 Erythritol (C4H10O4, CAS No.: 149-32-6), with a purity ≥ 99%, or a standard
substance certified by the state and awarded with a standard substance certificate.
10.4 Preparation of standard solution
10.4.1 Standard stock solution: respectively and accurately weigh 25 mg of xylitol, 25
mg of sorbitol, 25 mg of maltitol and 35 mg of erythritol, (accurate to 0.1 mg); add
water to fix-volume to 10 mL; every milliliter of solution is equivalent to 3.5 mg of
erythritol, 2.5 mg of xylitol, 2.5 mg of sorbitol and 2.5 mg of maltitol; it can be stored
for 1 month at 4°C if sealed well.
10.4.2 Standard working solution: respectively and accurately transfer 40 μL, 60 μL,
80 μL, 100 μL, 120 μL and 140 μL of various sugar alcohol standard stock solutions;
add water to fix-volume to 1 mL; prepare erythritol into mixed series standard working
solution with the concentration of 0.14mg/mL, 0.21 mg/mL, 0.28 mg/mL, 0.35 mg/mL,
0.42 mg/mL and 0.49 mg/mL; and prepare xylitol, sorbitol and maltitol into mixed series
standard working solutions with the concentration of 0.10 mg/mL, 0.15 mg/mL, 0.20
mg/mL, 0.25 mg/mL, 0.30 mg/mL and 0.35 mg/mL respectively.
11 Instruments and Apparatuses
11.1 High performance liquid chromatography: with evaporative light scattering
detector.
11.2 Chromatographic column: amino column with a column length of 250 mm, an
inner diameter of 4.6 mm and a particle size of 5 μm, or equivalent columns.
11.3 Food grinder.
11.4 Analytical balance: with the sensitivity of 0.1 mg and 0.01 g.
11.5 High speed centrifuge: speed ≥ 9 500 r/min.
11.6 Ultrasonic cleaning machine: with the working frequency of 40 kHz, the power of
500 W.
Precipitate protein: add 5 mL of trichloroacetic acid solution into the supernatant;
shake it; then place it at room temperature for 30 min; centrifuge at 9 500 r/min for 10
min. Take 8 mL of the supernatant in a 10 mL volumetric flask; add water to fix-volume.
After shaking, take 850 μL of filtrate; add 150 μL of sodium carbonate solution; shake
and neutralize; or take 10 mL of supernatant; add 20 mL of acetonitrile; shake well and
place it at room temperature for 30 min; centrifuge at 9 500 r/min for 10 min; fix-volume
the supernatant to 50 mL; shake well. After filtering through a 0.22 μm filter, test it on
the machine after dilution.
Note: For samples with sugar alcohol content lower than the detection-limit after being
precipitated and diluted by acetonitrile, trichloroacetic acid shall be used for
precipitation. For samples with low erythritol content (≤1%), acetonitrile shall be used
for precipitation. In other cases, both methods are available.
12.2 Apparatus reference conditions
Apparatus reference conditions are listed as below:
a) Chromatographic column: amino column with a column length of 250 mm, an
inner diameter of 4.6 mm and a particle size of 5 μm, or equivalent columns;
b) Column temperature: 30°C;
c) Mobile phase: acetonitrile: water = 80:20;
d) Flow velocity: 1.0 mL/min;
e) Injection volume: 10 μL;
f) Drift tube temperature: 83.5°C;
g) Atomizing gas flow velocity: 2.1 L/min.
12.3 Preparation of the standard curve
Respectively inject 10 μL of standard series working solution into the high performance
liquid chromatograph; measure the response value (peak area) of the standard
solution under the described chromatographic conditions; use the logarithm to base
10 of the concentration of the standard working solution as the vertical ordinate, the
logarithm to base 10 of the response value (peak area) as the abscissa, draw the
standard curve.
12.4 Test of sample solution
Inject 10 μL of the sample solution into the high performance liquid chromatograph;
measure the response value (peak area) of the sample under the described
chromatographic conditions; determine the sugar alcohol in the sample through the
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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