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GB 5009.28-2016

Chinese Standard: 'GB 5009.28-2016'
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GB 5009.28-2016English95 Add to Cart 0--10 minutes. Auto immediate delivery. National Food Safety Standard -- Determination of Benzoic Acid, Sorbic Acid and Saccharin Sodium in Foods Valid GB 5009.28-2016
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Detail Information of GB 5009.28-2016; GB5009.28-2016
Description (Translated English): Determination of sorbic acid and benzoic acid in foods
Sector / Industry: National Standard
Classification of Chinese Standard: X09
Date of Issue: 2016-12-23
Date of Implementation: 2017-06-23
Older Standard (superseded by this standard): GB 21703-2010; GB/T 23495-2009; GB/T 5009.28-2003; GB/T 5009.29-2003; SB/T 10389-2004; SN/T 2012-2007
Regulation (derived from): National Health and Family Planning Commission Notice No.17 of 2016

GB 5009.28-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Determination of Benzoic
Acid, Sorbic Acid and Saccharin Sodium in Foods
ISSUED ON. DECEMBER 23, 2016
IMPLEMENTED ON. JUNE 23, 2017
Issued by. National Health and Family Planning Commission of the
People's Republic of China;
China Food and Drug Administration.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Instruments and Apparatus ... 6
5 Analysis Steps ... 7
6 Expression of Analysis Results ... 8
7 Precision ... 9
8 Others ... 9
9 Principle ... 9
10 Reagents and Materials ... 9
11 Instruments and Apparatus ... 11
12 Analysis Steps ... 11
13 Expression of Analysis Results ... 12
14 Precision ... 13
15 Others ... 13
Appendix A - Liquid Chromatogram of Benzoic Acid, Sorbic Acid and Saccharin
Sodium ... 14
Appendix B - Gas Chromatogram of Standard Solutions of 100mg/L Benzoic
Acid, Sorbic Acid and Saccharin Sodium ... 15
National Food Safety Standard - Determination of Benzoic
Acid, Sorbic Acid and Saccharin Sodium in Foods
1 Scope
This Standard specifies the determination method for benzoic acid, sorbic acid AND
sodium saccharin in foods.
The first method of this Standard is applicable to the determination of benzoic acid,
sorbic acid AND saccharin sodium in foods; the second method is applicable to the
determination of benzoic acid and sorbic acid in soy sauce, fruit juice AND jam.
First method – Liquid chromatography
2 Principle
Use water to extract the sample; use n-hexane to degrease high-fat sample; use
protein precipitation agent to precipitate the protein of high-protein sample; adopt liquid
chromatography to perform separation; use UV detector to perform detection; use
external standard method to determine the quantity.
3 Reagents and Materials
Unless otherwise stated, the used reagents in this method shall all be analytical purity;
the water shall be the Grade-1 water which is specified in GB/T 6682.
3.1 Reagents
3.1.1 Ammonia (NH3·H2O).
3.1.2 Potassium ferrocyanide [K4Fe(CN)6·3H2O].
3.1.3 Zinc acetate [Zn(CH3COO)2·2H2O].
3.1.4 Anhydrous ethanol (CH3CH2OH).
3.1.5 N-hexane (C6H14).
3.1.6 Methanol (CH3OH). chromatographic purity.
5 Analysis Steps
5.1 Preparation of sample
Take a plurality of prepackaged homogeneous samples, such as beverages and liquid
milk, etc.; mix them directly; use tissue homogenizer to homogenize the non-
homogeneous-liquid and semi-solid samples; use grinder to fully comminute and stir
the solid sample evenly; perform heating and melting - 50°C ~ 60°C - for cheese, butter
AND chocolate, etc.; when it is hot, stir it evenly. Take 200g of it into a glass container
and seal it. The liquid sample shall be stored at 4°C; the rest sample shall be stored at
-18°C.
5.2 Sample’s extraction
5.2.1 General Samples
Accurately weigh and take about 2g (accurate to 0.001g) of sample in a 50mL
stoppered centrifuge tube; add about 25mL of water; vortex-mix it; in 50°C water bath,
sonicate it for 20min; cool it to room temperature; then, add 2mL of potassium
ferrocyanide solution AND 2mL of zinc acetate solution; mix them; centrifuge it at
8000r/min for 5min; transfer the aqueous phase into a 50mL volumetric flask; add
20mL of water in the residue; vortex-mix it; then sonicate it for 5min; centrifuge it at
8000r/min for 5min; transfer the aqueous phase into the same 50mL volumetric flask;
use water to dilute it to the scale; mix it evenly. Take appropriate amount of supernatant
to pass the 0.22μm filter; wait for the determination of liquid chromatography.
Note. When carbonated drinks, fruit wines, fruit juices and distilled spirits, etc. are determined, protein
precipitants may not be added.
5.2.2 Samples of gum-base jelly and candy, etc.
Accurately weigh and take about 2g (accurate to 0.001g) of sample in a 50mL
stoppered centrifuge tube; add about 25mL of water; vortex-mix it; in 70°C water bath,
heat and dissolve the sample; in 50°C water bath, sonicate it for 20min. Subsequent
operations shall be the same as those in 5.2.1.
5.2.3 High-fat sample such as fat, chocolate, butter and fried food, etc.
Accurately weigh and take about 2g (accurate to 0.001g) of sample in a 50mL
stoppered centrifuge tube; add 10mL of n-hexane; in 60°C water bath, heat it for 5min;
gently and occasionally shake it to dissolve fat; then add 25mL of ammonia solution
(1+99) AND 1mL of ethanol; vortex-mix them; in 50°C water bath, sonicate it for 20min;
cool it to room temperature; add 2mL of potassium ferrocyanide solution AND 2mL of
zinc acetate solution; mix them evenly; at 8000r/min 5min, centrifuge it for 5min;
discard the organic phase; transfer the aqueous phase into a 50 mL volumetric flask;
10.1.2 Ethanol (C2H5OH).
10.1.3 N-hexane (C6H14).
10.1.4 Ethyl acetate (CH3CO2C2H5). chromatographic purity.
10.1.5 Hydrochloric acid (HCl).
10.1.6 Sodium chloride (NaCl).
10.1.7 Anhydrous sodium sulfate (Na2SO4). at 500°C, dry for 8 hours; in desiccator,
after it is cooled to room temperature, it shall be set for standby application.
10.2 Preparation of reagent
10.2.1 Hydrochloric acid solution (1+1). take 50mL of hydrochloric acid; at the time of
stirring it, slowly add it into 50mL water; mix it evenly.
10.2.2 Sodium chloride solution (40g/L). weigh 40g of sodium chloride; use proper
amount of water to dissolve with; add 2mL of hydrochloric acid solution; add water to
set the constant volume to 1L.
10.2.3 N-hexane-ethyl acetate mixed solution (1+1). take 100 mL of n-hexane AND
100 mL of ethyl acetate; mix them evenly.
10.3 Standard products
10.3.1 Benzoic acid (C6H5COOH, CAS No.. 65-85-0). the purity shall be ≥ 99.0%; OR
the standard substance which is certified by the country AND granted for standard
substance certificate.
10.3.2 Sorbic acid (C6H8O2, CAS No.. 110-44-1). the purity shall be ≥ 99.0%; OR the
standard substance which is certified by the country AND granted for standard
substance certificate.
10.4 Preparation of standard solution
10.4.1 Benzoic acid AND sorbic acid standard stock solution (1000mg/L). respectively
and accurately weigh and take 0.1g of benzoic acid AND sorbic acid (accurate to
0.0001g); use methanol to dissolve them AND dilute them to 100 mL respectively;
Transfer them into a sealed container; at -18°C, store it. The preservation period shall
be 6 months.
10.4.2 Mixed standard intermediate-solution (200mg/L) of benzoic acid AND sorbic
acid. respectively and accurately pipette 10.0mL of benzoic acid and sorbic acid
standard stock solution into a 50mL volumetric flask; use ethyl acetate to dilute to
constant volume. Transfer it into a sealed container; at -18°C, store it. The preservation
anhydrous sodium sulfate. Add ethyl ether to wash the anhydrous-sodium-sulfate layer;
collect it to the scale of about 25mL; finally, use diethyl ether to set the constant volume;
mix it evenly. Accurately pipette 5mL of ethyl ether in a 5mL stoppered test tube; at
35°C, use nitrogen to blow it until dryness; add 2mL of n-hexane-ethyl acetate (1+1)
mixed solution to dissolve the residue; wait for the determination of gas
chromatography.
12.3 Reference conditions of instruments
12.3.1 Chromatographic column. polyethylene-glycol capillary gas chromatography
column; inner diameter - 320μm; length - 30 m; membrane’s thickness - 0.25μm; OR
the chromatographic column with equivalent performance.
12.3.2 Carrier gas. nitrogen; flow rate - 3mL/min.
12.3.3 Air. 400L/min.
12.3.4 Hydrogen. 40L/min.
12.3.5 Inlet temperature. 25......
Related standard:   GB 5009.22-2016  GB 5009.24-2016
   
 
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