GB 5009.28-2016 PDF English
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Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
GB 5009.28-2016 | English | 85 |
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National food safety standard - Determination of Benzoic Acid, Sorbic Acid and Saccharin Sodium in Foods
| Valid |
GB/T 5009.28-2003 | English | 319 |
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3 days
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Determination of sacchar in sodium in foods
| Obsolete |
GB/T 5009.28-1996 | English | 239 |
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2 days
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Method for determination of saccharin sodium in foods
| Obsolete |
GB 5009.28-1985 | English | 199 |
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2 days
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Method for determination of saccharin sodium in foods
| Obsolete |
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GB 5009.28-2016: National food safety standard - Determination of Benzoic Acid, Sorbic Acid and Saccharin Sodium 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/GB5009.28-2016
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
Foreword
This Standard replaces GB/T 5009.29-2003 "Determination of sorbic acid and benzoic
acid in foods", GB/T 5009.28-2003 "Determination of saccharin sodium in foods", GB/T
23495-2009 "Determination of benzoic acid, sorbic acid and saccharin sodium in foods
– High performance liquid chromatography method”, GB 21703-2010 “National food
safety standard – Determination of benzoic acid and sorbic acid in milk and milk
products”, SN/T 2012-2007 “Determination of benzoic acid and sorbic acid in vinegar
for export and import-Liquid chromatography” AND SB/T 10389-2004 “Determination
of sorbic acid in meat and meat products”.
Compared with GB/T 5009.29-2003, main changes are as follows.
- The standard name was changed to "National Food Safety Standard –
Determination of benzoic acid, sorbic acid and saccharin sodium in foods";
- Add "multi-point calibration" method to prepare the standard curve;
- Modify the pre-processing method for sample;
- Delete contents of packed-column’s chromatography-column separation in
gas chromatography;
- Add contents of capillary’s chromatography-column separation in gas
chromatography.
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).
3.1.6 Methanol (CH3OH). chromatographic purity.
3.1.7 Ammonium acetate (CH3COONH4). chromatographic purity.
3.1.8 Formic acid (HCOOH). chromatographic purity.
3.2 Preparation for reagents
3.2.1 Ammonia solution (1+99). take 1mL of ammonia; add it into 99mL water; mix it
evenly.
3.2.2 Potassium ferrocyanide solution (92g/L). weigh and take 106g of potassium
ferrocyanide; add appropriate amount of water to dissolve it; use water to dilute it to
1000mL.
3.2.5 Formic acid-ammonium acetate solution (2mmol/L formic acid + 20 mmol/L
ammonium acetate). weigh and take 1.54 g of ammonium acetate; add appropriate
amount of water to dissolve it; add 75.2μL of formic acid; use water to dilute it to
1000mL. After it is filtered by 0.22μm aqueous microfiltration membrane, it shall be set
for standby application.
3.3 Standard products
3.3.1 Sodium benzoate (C6H5COONa, CAS No.. 532-32-1). The purity shall be ≥
99.0%; OR 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.
3.4 Preparation of standard solution
3.4.1 Benzoic acid, sorbic acid AND saccharin sodium (calculated as saccharine)
standard stock solution (1000mg/L).
3.4.2 Mixed standard intermediate solution (200mg/L) of benzoic acid, sorbic acid AND
saccharin sodium (calculated as saccharin). respectively and accurately pipette
10.0mL of the mixed standard stock solution of benzoic acid, sorbic acid AND
saccharin sodium into a 50mL volumetric flask; use water to set the constant volume.
At 4°C, store it. The preservation period shall be 3 months.
3.5 Materials
3.5.1 Aqueous microporous membrane. 0.22μm.
3.5.2 Plastic centrifuge tube. 50mL.
4 Instruments and Apparatus
4.1 High performance liquid chromatography. be equipped with UV detector.
4.5 Homogenizer.
4.6 Constant temperature water bath.
4.7 Ultrasonic generator.
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;
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;
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.
5.3 Reference conditions of instrument
5.3.1 Chromatographic column. C18 column; column length - 250mm; inner diameter
- 4.6mm; particle size - 5μm; OR the chromatographic column with equivalent
performance.
5.3.2 Mobile phase. methanol + ammonium acetate solution = 5 + 95.
5.3.3 Flow rate. 1 mL/min.
5.3.4 Detection wavelength. 230nm.
5.5 Determination of sample solution
Inject the sample solution into the liquid chromatograph; obtain the peak area;
according to the standard curve, obtain the mass concentration of benzoic acid, sorbic
acid AND saccharin sodium (calculated as saccharine) in test solution.
6 Expression of Analysis Results
Content of benzoic acid, sorbic acid AND saccharin sodium (calculated as saccharin)
in sample shall be calculated according to formula (1).
7 Precision
The absolute difference between the two independent determinations results which
are obtained under repeatability conditions shall not exceed 10% of the arithmetic
mean.
8 Others
When the sample volume is 2g AND the constant volume is 50 mL, the detection limit
of benzoic acid, sorbic acid and saccharin sodium (calculated as saccharine) shall all
be 0.005g/kg; the limit of quantitation shall all be 0.01g/kg.
9 Principle
After the sample is acidified by hydrochloric acid, use ethyl ether to extract the benzoic
acid and sorbic acid;
10 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.
10.1.1 Ether (C2H5OC2H5).
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.
10.3 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.
10.4 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.
10.5 Materials
Plastic centrifuge tube. 50mL.
11 Instruments and Apparatus
11.1 Gas chromatograph. Flame Ionization Detector (FID) with hydrogen.
11.5 Homogenizer.
11.6 Nitrogen blowing instrument.
...... Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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