GB 5009.280-2020 English PDF

GB 5009.280-2020: National food safety standard - Determination of 4-Hexylesorinol Residues in Foods
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GB 5009.280-2020
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Determination of 4-Hexylesorinol Residues in Foods
ISSUED ON: SEPTEMBER 11, 2020
IMPLEMENTED ON: MARCH 11, 2021
Issued by: National Health Commission of the People’s Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Apparatus ... 5
5 Analytical Procedures ... 6
6 Calculation and Expression of Results... 7
7 Precision ... 8
8 Others ... 8
Appendix A 4-Hexylresorcinol Standard Solution and Spiked Chromatogram . 9
National Food Safety Standard -
Determination of 4-Hexylesorinol Residues in Foods
1 Scope
This Standard specifies the method for the determination of 4-hexylresorcinol residues
in shrimp and crabs.
This Standard is applicable to the determination of 4-hexylresorcinol residues in shrimp
and crabs.
2 Principle
The sample was extracted by ethyl acetate, removed fat by acetonitrile saturated n-
hexane, separated by high performance liquid chromatography, detected by
fluorescence detector, and quantified by external standard method.
3 Reagents and Materials
Unless otherwise specified, the reagents used in this method are analytically pure; and
the water is the Class-I water specified in GB/T 6682.
3.1 Reagents
3.1.1 Acetonitrile (C2H3N): chromatographically pure.
3.1.2 Methanol (CH3OH): chromatographically pure.
3.1.3 Ethyl acetate (C4H8O2): chromatographically pure.
3.1.4 n-hexane (C6H14): chromatographically pure.
3.1.5 Anhydrous sodium sulfate (Na2SO4): Place anhydrous sodium sulfate in a muffle
furnace at 400°C for 4h; then place it in a desiccator for later-use.
3.2 Preparation of reagents
3.2.1 Acetonitrile saturated n-hexane solution: Add a certain amount of acetonitrile to
n-hexane; shake and mix; after the mixture is clearly separated into layers, the upper
4.8 Homogenizer.
4.9 Concentrate bottle.
4.10 Organic phase microporous filter membrane: 0.45μm.
5 Analytical Procedures
5.1 Preparation of the specimen
Take about 500g of the edible part of the representative sample; pulverize and mix by
a tissue grinder, and then put it into a clean container as a specimen; seal it and make
a mark. The specimen is stored at -18°C.
5.2 Extraction of the specimen
Take 2g (accurate to 0.01g) of the sample in a 50mL centrifuge tube; add 20mL of ethyl
acetate and 3g of anhydrous sodium sulfate; homogenize for 30s; then centrifuge at
4000r/min for 3min; and transfer all the supernatant to a 100mL concentrate bottle.
Add 20mL ethyl acetate to the residue again; homogenize for 30s; then centrifuge at
4000r/min for 3min; combine the supernatant with the supernatant obtained for the first
time in the same concentrate bottle; and evaporate to near dryness in a 35°C water
bath.
5.3 Purification of the specimen
Accurately add 2mL of methanol-acetonitrile-water mixed solution to the residue for
reconstitution; sonicate for 10s; vortex for 30s. After the residue is dissolved, add 2mL
of acetonitrile saturated n-hexane solution; vortex for 30s; transfer to a 15mL centrifuge
tube and centrifuge at 4000r/min for 3min. After discarding the n-hexane layer, add 2
mL of acetonitrile saturated n-hexane solution to the centrifuge tube again; vortex for
30s; centrifuge at 4000r/min for 3min; discard the upper n-hexane layer; take the lower
layer and filter through a 0.45μm organic microporous filter; the filtrate is reserved for
using on the machine.
5.4 Blank test
Except that no sample is added, the determination procedures are carried out in
accordance with 5.2 and 5.3.
5.5 Determination
5.5.1 Reference condition of the instrument
a) Chromatographic column: C18 column, 250mm×4.6mm (i.d.), particle size 5μm;
1000 - Unit conversion factor;
m - The weighing amount of the specimen, in g.
The calculation result retains 3 significant digits.
7 Precision
The absolute difference between two independent determination results obtained
under repeatability conditions shall not exceed 10% of the arithmetic mean.
8 Others
When the weight of shrimp and crab is 2.00g, the limit of detection 0.0200mg/kg, and
the quantification limit is 0.0500mg/kg.
GB 5009.280-2020
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Determination of 4-Hexylesorinol Residues in Foods
ISSUED ON: SEPTEMBER 11, 2020
IMPLEMENTED ON: MARCH 11, 2021
Issued by: National Health Commission of the People’s Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Apparatus ... 5
5 Analytical Procedures ... 6
6 Calculation and Expression of Results... 7
7 Precision ... 8
8 Others ... 8
Appendix A 4-Hexylresorcinol Standard Solution and Spiked Chromatogram . 9
National Food Safety Standard -
Determination of 4-Hexylesorinol Residues in Foods
1 Scope
This Standard specifies the method for the determination of 4-hexylresorcinol residues
in shrimp and crabs.
This Standard is applicable to the determination of 4-hexylresorcinol residues in shrimp
and crabs.
2 Principle
The sample was extracted by ethyl acetate, removed fat by acetonitrile saturated n-
hexane, separated by high performance liquid chromatography, detected by
fluorescence detector, and quantified by external standard method.
3 Reagents and Materials
Unless otherwise specified, the reagents used in this method are analytically pure; and
the water is the Class-I water specified in GB/T 6682.
3.1 Reagents
3.1.1 Acetonitrile (C2H3N): chromatographically pure.
3.1.2 Methanol (CH3OH): chromatographically pure.
3.1.3 Ethyl acetate (C4H8O2): chromatographically pure.
3.1.4 n-hexane (C6H14): chromatographically pure.
3.1.5 Anhydrous sodium sulfate (Na2SO4): Place anhydrous sodium sulfate in a muffle
furnace at 400°C for 4h; then place it in a desiccator for later-use.
3.2 Preparation of reagents
3.2.1 Acetonitrile saturated n-hexane solution: Add a certain amount of acetonitrile to
n-hexane; shake and mix; after the mixture is clearly separated into layers, the upper
4.8 Homogenizer.
4.9 Concentrate bottle.
4.10 Organic phase microporous filter membrane: 0.45μm.
5 Analytical Procedures
5.1 Preparation of the specimen
Take about 500g of the edible part of the representative sample; pulverize and mix by
a tissue grinder, and then put it into a clean container as a specimen; seal it and make
a mark. The specimen is stored at -18°C.
5.2 Extraction of the specimen
Take 2g (accurate to 0.01g) of the sample in a 50mL centrifuge tube; add 20mL of ethyl
acetate and 3g of anhydrous sodium sulfate; homogenize for 30s; then centrifuge at
4000r/min for 3min; and transfer all the supernatant to a 100mL concentrate bottle.
Add 20mL ethyl acetate to the residue again; homogenize for 30s; then centrifuge at
4000r/min for 3min; combine the supernatant with the supernatant obtained for the first
time in the same concentrate bottle; and evaporate to near dryness in a 35°C water
bath.
5.3 Purification of the specimen
Accurately add 2mL of methanol-acetonitrile-water mixed solution to the residue for
reconstitution; sonicate for 10s; vortex for 30s. After the residue is dissolved, add 2mL
of acetonitrile saturated n-hexane solution; vortex for 30s; transfer to a 15mL centrifuge
tube and centrifuge at 4000r/min for 3min. After discarding the n-hexane layer, add 2
mL of acetonitrile saturated n-hexane solution to the centrifuge tube again; vortex for
30s; centrifuge at 4000r/min for 3min; discard the upper n-hexane layer; take the lower
layer and filter through a 0.45μm organic microporous filter; the filtrate is reserved for
using on the machine.
5.4 Blank test
Except that no sample is added, the determination procedures are carried out in
accordance with 5.2 and 5.3.
5.5 Determination
5.5.1 Reference condition of the instrument
a) Chromatographic column: C18 column, 250mm×4.6mm (i.d.), particle size 5μm;
1000 - Unit conversion factor;
m - The weighing amount of the specimen, in g.
The calculation result retains 3 significant digits.
7 Precision
The absolute difference between two independent determination results obtained
under repeatability conditions shall not exceed 10% of the arithmetic mean.
8 Others
When the weight of shrimp and crab is 2.00g, the limit of detection 0.0200mg/kg, and
the quantification limit is 0.0500mg/kg.