GB 5009.257-2016 PDF English
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| GB 5009.257-2016 | English | 85 |
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National food safety standard - Determination of Trans-fatty Acids in Foodstuffs
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GB 5009.257-2016: National food safety standard - Determination of Trans-fatty Acids in Foodstuffs---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/GB5009.257-2016
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Determination of
Trans-fatty Acids 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 Instruments and Equipment... 5
5 Analytical Procedures... 6
6 Expression of Analytical Result... 9
7 Precision... 11
8 Others... 11
Appendix A Information of Standard Substance... 12
Appendix B Chromatogram of Standard Substance... 14
Appendix C Calculation of FID Response Factor and FID Calibration Factor 16
Appendix D FID Response Factor and FID Calibration Factor... 17
Foreword
This Standard serves as a replacement of GB/T 22110-2008 Determination of Trans-
fatty Acids in Foods - Gas Chromatographic Method; GB/T 22507-2008 Animal and
Vegetable Fats and Oils - Determination of the Content of Trans-fatty Acid Isomers of
Vegetable Fats and Oils - Gas Chromatographic Method; SN/T 1945-2007
Determination of Trans-fatty Acids in Foods - Capillary Gas Chromatography.
In comparison with the standards being replaced by this Standard, there are certain
main changes as follows.
---The title of this Standard is modified into “National Food Safety Standard -
Determination of Trans-fatty Acids in Foodstuffs”;
---The scope of application is extended to animal fats and oils, and foods
containing animal fats and oils;
---The analyte is extended to 15 kinds of fatty acid, for example, C16.1t ~ C22.1t.
National Food Safety Standard - Determination of
Trans-fatty Acids in Foodstuffs
1 Scope
This Standard specifies the gas chromatographic method for the determination of
trans-fatty acids and isomer in foods.
This Standard is applicable to the determination of trans-fatty acids in animal and
vegetable fats and oils, hydrogenated vegetable oil, refined vegetable oil and frying oil,
as well as foods that contain animal and vegetable fats and oils, hydrogenated
vegetable oil, refined vegetable oil and frying oil.
This Standard is not applicable to the determination of food samples, in which, free
fatty acid (FFA) content in fats and oils is more than 2%.
2 Principle
Animal and vegetable fats and oils samples, or fats in food samples extracted through
acid hydrolysis method, under alkaline condition, go through transesterification with
methanol; generate fatty acid methyl ester. Furthermore, on strong polarity stationary
phase capillary chromatographic column, separate it. Use gas chromatograph, which
is equipped with hydrogen flame ionization detector, for determination. Use area
normalization method to quantify it.
3 Reagents and Materials
Unless it is otherwise stipulated, all reagents used in this method shall be analytically
pure. Water shall be Grade-2 water stipulated in GB/T 6682.
3.1 Reagents
3.2 Preparation of Reagents
Potassium hydroxide - methanol solution (2 mol/L). weigh-take 13.2 g of potassium
hydroxide; dissolve it in 80 mL of methanol. Cool it down to room temperature. Use
methanol to reach a constant volume of 100 mL.
3.3 Standard Substance
Fatty acid methyl ester standard substance. please refer to Table A.1 for the type of
fatty acid methyl ester standard substance. Purity shall be > 99%.
3.4 Preparation of Standard Solutions
3.4.1 Fatty acid methyl ester standard stock solution. respectively and accurately
weigh-take 100 mg (accurate to 0.1 mg) of trans-fatty acid methyl ester standard
substances; place them in 25 mL beaker. Respectively use isooctane to dissolve them,
then, transfer them into 10 mL volumetric flask. Accurately reach the volume of 10 mL.
The concentration of the standard stock solutions is 10 mg/mL.
4 Instruments and Equipment
4.1 Gas chromatograph. equipped with hydrogen flame ionization detector.
4.2 Constant-temperature water bath kettle.
4.3 Vortex oscillator.
4.7 Round-bottomed flask. 200 mL. Before usage, place it in 100 °C oven to reach a constant weight.
4.8 Rotary evaporator.
4.9 Balance. division value. 0.1 g, 0.1 mg.
5 Analytical Procedures
5.1 Sample Preparation
5.1.1 Solid sample
Take 500 g of representative test sample. Use a grinder to grind and mix it up. Evenly
divide it into two parts. Respectively load them into clean containers. Seal them up;
5.1.2 Semi-solid lipid sample
Take 500 g of representative sample. Place it in a beaker. At 60 °C ~ 70 °C water bath,
melt it. Thoroughly mix it up. After cooling it down, evenly divide it into two parts.
Respectively load them into clean containers. Seal them up;
5.2 Analytical Procedure
5.2.1 Animal and vegetable fats and oils
Weigh-take 60 mg of fats and oils; place it in a 10 mL test tube with a stopper. Add 2
mL of isooctane to thoroughly dissolve it. Add 0.2 mL of potassium hydroxide-methanol
solution. Conduct vortex mixing for 1 min. Place it till the mixed liquid in the test tube
becomes pellucid.
5.2.2 Foods containing fats and oils (except from animal and vegetable fats and oils)
5.2.2.1 Determination of fats in foods
Solid and semi-solid lipid sample. weigh-take 2.0 g (accurate to 0.01 g; the weighing
amount of different foods may be properly adjusted, so as to guarantee that fat mass
in foods is not less than 0.125 g) of homogeneous sample. Place it in a 50 mL test
tube. Add 8 mL of water to thoroughly mix it up. Then, add 10 mL of hydrochloric acid
to evenly mix it up. Liquid sample. weigh-take 10.00 g of homogeneous sample, then,
place it in a 50 mL test tube. Add 10 mL of hydrochloric acid to evenly mix it up. Place
the above-mentioned test tube into 60 °C ~ 70 °C water bath. In every 5 min ~ 10 min,
oscillate it once. Last for around 40 min ~ 50 min, till the sample is completely
hydrolyzed. Take out the test tube. Add 10 mL of ethanol to thoroughly mix it up, then,
cool it down to room temperature.
5.3 Reference Conditions of Instruments
5.3.1 Capillary gas chromatographic column. SP-2560 polydicyanopropyl siloxane;
column length. 100 m 0.25 mm. Membrane thickness. 0.2 μm, or others with
equivalent performance.
5.3.2 Detector. hydrogen flame ionization detector.
5.3.3 Carrier gas. high-purity helium 99.999%.
5.3.4 Flow rate of carrier gas. 1.3 mL/min.
5.3.9 Split ratio. 30.1.
5.4 Quantitative Determination
Respectively inject the standard working solution and the sample test solution into the
gas phase chromatograph. In accordance with the chromatographic peak response
area of the standard solution, adopt normalization method for quantitative
determination.
5.6 Blank Test
In blank test, except from the adding of test sample, other test procedures, reagents
and dosage that are completely identical to the sample analysis shall be adopted.
6 Expression of Analytical Result
The content of trans-fatty acids is reported in trans-fats (%, mass fraction). The content
of trans-fats is calculated in the form of trans-fatty acid methyl ester’s percentage
content.
6.1 Calculation of Mass Fraction of Fats in Foods
The mass fraction of fats in foods shall be calculated in accordance with Formula (1).
6.4 Calculation of Trans-fatty Acids Content in Foods
Mass fraction of trans-fatty acids content in foods shall be calculated in accordance
with Formula (4).
7 Precision
The absolute difference between two independent determination results obtained
under repeatability condition shall not exceed 15% of the arithmetic mean value.
8 Others
The detection limit of this method is 0.012% (counted by fats); the quantitation limit of
this method is 0.024% (counted by fats).
Appendix A
Information of Standard Substance
Table A.1 provides a chemical information sheet of fatty acid methyl ester.
Table A.1 -- Chemical Information Sheet of Fatty Acid Methyl Ester
Appendix B
Chromatogram of Standard Substance
B.1 Gas phase chromatogram of trans-fatty acid methyl ester mixed standard
solution
B.2 Gas phase chromatogram of 37 fatty-acid methyl ester mixed standard
solution
Appendix C
Calculation of FID Response Factor and FID Calibration Factor
C.1 Calculation of FID response factor
Appendix D
FID Response Factor and FID Calibration Factor
Table D.1 provides FID response factor and FID calibration factor.
Table D.1 -- FID Response Factor and FID Calibration Factor
(reference)
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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