GB 5009.306-2025 PDF English
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| GB 5009.306-2025 | English | 125 |
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National food safety standard - Determination of diphenyl ether in foods
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GB 5009.306-2025: National food safety standard - Determination of diphenyl ether in foods---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GB5009.306-2025
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Determination of Diphenyl
Ether in Foods
Issued on: MARCH 16, 2025
Implemented on: SEPTEMBER 16, 2025
Issued by. National Technical Commission of the People’s Republic of China;
State Administration for Market Regulation.
Table of Contents
1 Scope... 3
2 Principle... 3
3 Reagents and Materials... 3
4 Instruments and Equipment... 4
5 Analysis Procedures... 4
6 Expression of Analysis Results... 6
7 Precision... 7
8 Others... 7
9 Principle... 8
10 Reagents and Materials... 8
11 Instruments and Equipment... 8
12 Analysis Procedures... 9
13 Expression of Analysis Results... 11
14 Precision... 11
15 Others... 11
Appendix A Gas Chromatogram of Diphenyl Ether Standard Solution... 12
Appendix B Selected Ion Flow Chromatogram and Ion Mass Spectrum of Diphenyl
Ether Standard Solution... 13
National Food Safety Standard - Determination of Diphenyl
Ether in Foods
1 Scope
This Standard specifies the determination method of diphenyl ether in foods by gas
chromatography and gas chromatography-mass spectrometry.
This Standard is applicable to the determination of diphenyl ether in fruits, fruit products, fruit
and vegetable juices, and soft candies.
Method-I Gas Chromatography
2 Principle
Diphenyl ether in the specimen is extracted with n-hexane; leached by salting out; and the
extract liquor is purified by N-propylethylenediamine (PSA) solid phase adsorbent and
graphitized carbon black (GCB) solid phase adsorbent; detected by gas chromatograph
equipped with hydrogen flame ionization detector; and quantified by external standard method.
3 Reagents and Materials
Unless otherwise specified, all the reagents used in this method are analytically pure; and water
is Grade-1 water specified in GB/T 6682.
3.1 Reagents
3.1.1 n-hexane (C6H14). Chromatographically pure.
3.1.2 Sodium chloride (NaCl).
3.1.3 Anhydrous magnesium sulfate (MgSO4).
3.1.4 Sodium citrate (C6H5Na3O7).
3.1.5 Disodium hydrogen citrate (C6H6Na2O7).
3.2 Standard sample
Diphenyl ether (Phenyl ether, C12H10O, CAS No.. 101-84-8). Standard substance purity ≥ 99%;
or standard sample certified by the state and awarded with a standard substance certificate.
3.3 Preparation of standard solutions
3.3.1 Diphenyl ether standard stock solution (1,000 mg/L). Accurately weigh 10 mg (accurate
to 0.1 mg) of diphenyl ether standard sample; dissolve it in n-hexane and make constant volume
to 10 mL; store at 4 ℃ in the dark; the validity period is 3 months; or directly purchase a
standard solution that meets the traceability requirements.
3.3.2 Diphenyl ether standard intermediate solution (10.0 mg/L). Accurately pipette 0.25 mL
of diphenyl ether standard stock solution into a 25 mL volumetric flask; and make constant
volume with n-hexane. Store at 4 ℃ away from light; with a validity period of 1 week.
3.3.3 Standard working solution. Accurately pipette 0.50 mL, 1.00 mL, 2.00 mL, 5.00 mL and
10.00 mL of diphenyl ether standard intermediate solution; make constant volume to 10 mL
with n-hexane; and prepare standard working solutions with mass concentrations of 0.5 μg/mL,
1.0 μg/mL, 2.0 μg/mL, 5.0 μg/mL and 10.0 μg/mL, respectively. Prepare immediately before
use.
3.4 Materials
3.4.1 N-propylethylenediamine (PSA) solid phase adsorbent. Particle size 40 μm~60 μm.
3.4.2 Graphitized carbon black (GCB) solid phase adsorbent. Particle size 120 μm~400 μm.
4 Instruments and Equipment
4.1 Gas chromatograph. Equipped with hydrogen flame ionization detector (FID).
4.2 Analytical balance. Sensitivity is 0.001 g and 0.000 1 g, respectively.
4.3 Centrifuge. speed ≥ 5,000 r/min.
4.4 Vortex mixer.
5 Analysis Procedures
5.1 Preparation of specimen
Fruit samples refer to GB 2763 Appendix A Food Categories and Test Parts for sampling. Fruit
products take the edible part, and soft candy takes the whole; and fully mash them with a masher.
Fruit and vegetable juice samples are directly sampled after being fully mixed. The sampling
volume shall be no less than 500 g. The prepared specimens shall be placed in a clean container;
sealed; labeled with sample information; and tested as soon as possible.
5.2 Extraction
5.2.1 Fruits and fruit and vegetable juices. Weigh 5 g of the specimen (accurate to 0.001 g) in
a 50 mL centrifuge tube; add 10 mL of n-hexane; and vortex and oscillate for 1 min.
5.2.2 Fruit products, soft candy. Weigh 5 g of the specimen (accurate to 0.001 g) into a 50 mL
centrifuge tube; add 10 mL of warm water at about 50°C; dissolve by ultrasonic for 30 min;
accurately add 10 mL of n-hexane; and vortex for 1 min.
5.3 Salting out
Respectively weigh 1 g of sodium chloride, 4 g of anhydrous magnesium sulfate, 1 g of sodium
citrate, and 0.5 g of disodium hydrogen citrate in a n-hexane-water mixed solution; vortex and
mix for 1 min; stand and cool to room temperature. Centrifuge at 5,000 r/min for 5 min; and
wait for purification.
NOTE. Commercial salt packs with the same adsorbent can also be used directly.
5.4 Purification
Transfer 5 mL of the upper-layer n-hexane extract to a centrifuge tube containing 885 mg of
anhydrous magnesium sulfate, 150 mg of N-propylethylenediamine (PSA) solid phase
adsorbent, and 15 mg of graphitized carbon black (GCB) solid phase adsorbent; vortex and mix
for 1 min; centrifuge at 5,000 r/min for 5 min; and take about 1 mL of the upper-layer clear
liquid for determination.
NOTE. Commercial salt packs with the same adsorbent can also be used directly.
5.5 Instrument reference conditions
5.5.1 Gas chromatography reference conditions
The gas chromatography reference conditions are as follows.
a) Chromatographic column. 5% phenyl-methyl polysiloxane non-polar column [30 m×0.32
mm (inner diameter), 0.25 μm (film thickness)], or equivalent;
b) Chromatographic column temperature. Maintain 80 ℃ for 1 min; increase to 150 ℃ at a
heating rate of 10 ℃/min, maintain for 10 min; increase to 280 ℃ at a heating rate of
30 ℃/min, maintain for 1 min;
c) Inlet temperature. 285 ℃;
d) Carrier gas flow rate. 1.0 mL/min;
e) Combustion gas. hydrogen, flow rate of about 30 mL/min;
f) Combustion-supporting gas. air, flow rate of about 300 mL/min;
Method-II Gas Chromatography-Mass Spectrometry
9 Principle
Diphenyl ether in the specimen is extracted with n-hexane; leached by salting out; and the
extract is purified by N-propylethylenediamine (PSA) solid phase adsorbent and graphitized
carbon black (GCB) solid phase adsorbent; detected by gas chromatography-mass spectrometry;
and quantified by external standard method.
10 Reagents and Materials
Unless otherwise specified, all the reagents used in this method are analytically pure; and water
is Grade-1 water specified in GB/T 6682.
10.1 Reagents
The same as 3.1.
10.2 Standard sample
The same as 3.2.
10.3 Preparation of standard solutions
10.3.1 The same as 3.3.1.
10.3.2 The same as 3.3.2.
10.3.3 Standard working solution. Accurately pipette 0.025 mL, 0.050 mL, 0.100 mL, 0.200
mL and 0.500 mL of diphenyl ether standard intermediate solution; make constant volume to
10 mL with n-hexane; and prepare standard working solutions with mass concentrations of
0.025 μg/mL, 0.050 μg/mL, 0.100 μg/mL, 0.200 μg/mL and 0.500 μg/mL, respectively. Prepare
immediately before use.
10.4 Materials
The same as 3.4.
11 Instruments and Equipment
11.1 Gas chromatograph-mass spectrometer. Equipped with electron impact source (EI).
11.2 Analytical balance. The sensitivity is 0.001 g and 0.000 1 g, respectively.
11.3 Centrifuge. speed ≥5,000 r/min.
11.4 Vortex mixer.
11.5 Pipettor. 5 mL, 1 mL, 200 μL.
12 Analysis Procedures
12.1 Preparation of specimen
The same as 5.1.
12.2 Extraction
The same as 5.2.
12.3 Salting out
The same as 5.3.
12.4 Purification
The same as 5.4.
12.5 Instrument reference conditions
12.5.1 Gas chromatography-mass spectrometry reference conditions
The gas chromatography-mass spectrometry reference conditions are as follows.
a) Chromatographic column. 5% diphenyl-methyl polysiloxane non-polar column [30
m×0.25 mm (inner diameter) 0.25 μm (film thickness)], or equivalent;
b) Chromatographic column temperature. Maintain 80 ℃ for 1 min; increase to 150 ℃ at a
heating rate of 10 ℃/min, maintain for 10 min; increase to 280 ℃ at a heating rate of
30 ℃/min, maintain for 1 min;
c) Inlet temperature. 285 ℃;
d) Chromatography-mass spectrometry interface temperature. 280 ℃;
e) Ion source temperature. 250 ℃;
f) Carrier gas. Helium, Purity ≥ 99.999%, flow rate 1.0 mL/min;
g) Injection volume. 1 μL;
h) Injection method. Splitless injection, valve opening after 1.0 min;
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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