GB 5009.31-2016 (GB5009.31-2016) & related versions
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GB 5009.31-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Determination of
p-hydroxybenzoic acid esters in foodstuffs
ISSUED ON. AUGUST 31, 2016
IMPLEMENTED ON. MARCH 1, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Instrument and Apparatus ... 6
5 Analysis Steps ... 6
6 Expression of Analysis Results ... 8
7 Precision ... 8
8 Others ... 8
Appendix A ... 9
6 Expression of Analysis Results ... 7
7 Precision ... 8
8 Others ... 8
Appendix A - Chromatogram of Parabens Standard Solution ... 9
Foreword
This Standard replaces GB/T 5009.31-2003 "Determination of p-hydroxybenzoic acid
esters in foods".
Compared with GB/T 5009.31-2003, main changes in this Standard are as follows.
- The Standard’s name was changed to "National Food Safety Standard -
Determination of p-hydroxybenzoic acid esters in foodstuffs";
- Expand the detection range of parabens and add the detection for methyl paraben
and butyl paraben;
- Revise the expression for the samples’ weighing method - soy sauce, vinegar and
juice - in analysis step;
- Revise the standard curve range of parabens;
- Gas chromatography adds analysis and measurement conditions for capillary
column and deletes analysis and measurement conditions for packed column;
- Add the limit of quantitation for the determination method of parabens in foods;
- Modify the calculation formula. Modify the calculation basis for calculation result -
from parabens to p-hydroxybenzoic acid.
National Food Safety Standard - Determination of
p-hydroxybenzoic acid esters in foodstuffs
1 Scope
This Standard specifies the gas chromatography method for the methyl paraben, ethyl
p-hydroxybenzoate, propyl paraben and butyl paraben in foods.
This Standard is applicable to the determination of methyl paraben, ethyl p-
hydroxybenzoate, propyl paraben and butyl paraben in soy sauce, vinegar, beverages
and jams.
2 Principle
After the acidification of the sample, use ethyl ether to extract the parabens,
concentrate it until it closes to dryness; use ethanol to re-dissolve it; use the gas
chromatography of hydrogen flame ionization detector to perform separated
determination; use retention time to conduct qualitative diagnosis; use external
standard method to conduct quantitative diagnosis.
3 Reagents and Materials
Unless otherwise stated, all the reagents used in this method shall be the analytical
purity. The water shall be the grade-II water specified in GB/T 6682.
3.1 Reagents
3.1.1 Anhydrous ether (C2H5OC2H5). Redistilled.
3.1.2 Anhydrous ethanol (C2H5OH). Guaranteed reagent.
3.1.3 Hydrochloric acid (HCl).
3.1.4 Sodium chloride (NaCl).
3.1.5 Anhydrous sodium sulfate (Na2SO4).
3.1.6 Sodium bicarbonate (NaHCO3).
3.2 Preparation of reagents
4 Instrument and Apparatus
4.1 Gas chromatograph. it is equipped with the hydrogen flame ionization detector
(FID).
4.2 Balance. the sensitivity weight is 0.1 mg and 1 mg.
4.3 Rotary evaporator.
4.4 Vortex mixer.
5 Analysis Steps
5.1 Preparation for the sample
5.1.1 Processing for the sample
5.1.1.1 Soy sauce, vinegar and beverages. general liquid sample can be sampled
directly after the shaking. Weigh and take 5g (accurate to 0.001g) of the sample into a
small beaker; transfer it into a 125mL separating funnel; use 10mL of saturated sodium
chloride solution to wash the small beakers in batch; combine the cleaning solutions
in the 125mL separating funnel; add 1mL of 1.1 hydrochloric acid to perform
acidification; shake it evenly; use 75mL, 50mL and 50mL of anhydrous ether to
respectively extract it for three times and 2min for each time; place it for a moment;
discard the water layer; combine the ether layer into the 250mL separating funnel; add
10mL of saturated sodium chloride solution to wash it for one time; respectively use 30
mL, 30 mL and 30 mL of sodium bicarbonate solution to wash it for three times; discard
the water layer. Use filter paper to absorb the water at funnel’s neck; through the
anhydrous sodium sulfate (about 20g), filter the organic layer into a concentrating flask;
concentrate it on the rotary evaporator until it closes to dryness; use nitrogen to remove
the residual solvent; accurately add 2.0 mL of anhydrous ethanol to dissolve the
residues for gas chromatography.
5.1.1.2 Jam. weigh and take 5g (accurate to 0.001g) of jam sample which has been
homogenized in advance in the 100mL test tube with stopper; add 1mL of 1.1
hydrochloric acid to perform acidification AND 10 mL of saturated sodium chloride
solution; perform 1min~2min vortex mixing to make uniform solution; then use 50 mL,
30 mL and 30 mL of anhydrous ether to extract it for three times and 2min for each
time; transfer it with the pipette into a 250mL separating funnel; add 10mL of saturated
sodium chloride solution to wash it for one time; then use 30mL, 30mL and 30mL of
sodium bicarbonate solution to wash it for three times; discard the water layer. Use
filter paper to absorb the water on the funnel’s neck; through the anhydrous sodium
sulfate (about 20g), filter the organic layer into a concentrating flask; concentrate it on
the rotary evaporator until it closes to dryness; use nitrogen to remove the residual
......
| Standard ID | GB 5009.31-2016 (GB5009.31-2016) | | Description (Translated English) | National Food Safety Standard -- Food stuffs -- Determination of p-hydroxybenzoic acid esters in food stuffs | | Sector / Industry | National Standard | | Classification of Chinese Standard | C53 | | Word Count Estimation | 7,759 | | Date of Issue | 2016-08-31 | | Date of Implementation | 2017-03-01 | | Older Standard (superseded by this standard) | GB/T 5009.31-2003 | | Regulation (derived from) | Announcement of the State Administration of Public Health and Family Planning 2016 No.11 |
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