GB 5009.262-2016 PDF English
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB 5009.262-2016 | English | 70 |
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Method for analysis of hygienic standard of edible oils
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GB 5009.262-2016: Method for analysis of hygienic standard of edible oils---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/GB5009.262-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard –
Determination of Solvent Residual in Food
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 Application Scope... 4
2 Terms and Definitions... 4
3 Principle... 4
4 Reagents and Materials... 4
5 Apparatus... 5
6 Analytical Procedure... 6
7 Expression of Analytical Results... 7
8 Accuracy... 8
9 Others... 8
Annex A Gas Chromatogram of No. 6 Solvent... 9
Foreword
This Standard replaces “4.8 Determination of solvent residual” of GB/T 5009.37-2003,
Method for Analysis of Hygienic Standard of Edible Oils, and “6 Determination of
solvent residual” of GB/T 5009.117-2003, Method for Analysis of Hygienic Standard of
Edible Soybean Meal.
Compared with GB/T 5009.37-2003 and GB/T 5009.117-2003, the major changes of
this Standard are as follows.
-- it changes the standard name into “National Food Safety Standard –
Determination of Solvent Residual in Food”;
-- it modifies the method for analysis of solvent residual;
-- it modifies the method for plotting standard curves;
-- it modifies the calculation formula of results.
National Food Safety Standard –
Determination of Solvent Residual in Food
1 Application Scope
This Standard specifies the method for determination of solvent residual in edible
vegetable oils and edible soybean meal.
This Standard applies to the determination of solvent residual in edible vegetable oils
and edible soybean meal.
2 Terms and Definitions
For the purposes of this document, the following terms and definitions apply.
2.1 Matrix vegetable oil
Refined vegetable oil obtained through the refining processes including colour and
odour removal, or vegetable oil produced by ultrasonic degassing at room temperature,
of the same species as that of specimen to be tested. The solvent residual in matrix
vegetable oil shall be lower than the detection limit.
3 Principle
The solvent residual existing in specimen will diffuse to gas phase in a closed container;
after a certain time, the dynamic equilibrium between the concentrations of gas phase
and liquid phase can be achieved; the content of solvent residual in the upper gas
phase is measured by headspace gas chromatography, i.e.
4 Reagents and Materials
Unless specified otherwise, all reagents used for this method are analytically pure and
the water is of grade 1 water specified in GB/T 6682.
4.1 Reagents
4.2 Preparation of reagent
n-heptane standard working solution. add 1 mL of n-heptane accurately in a 10-mL
volumetric flask immediately; add quickly N,N-dimethylacetamide; add dropwise to the
scale.
4.3 Standard product
Solvent residual standard product. “no. 6 solvent” solution of concentration 10 mg/mL;
the solvent is N,N-dimethylacetamide. Or other standard products for the
determination of solvent residual, which have been certified by the state or granted
standard product certificates.
4.4 Preparation of standard solution
4.4.1 For vegetable oils, weigh 6 shares of 5.0 g (accurate to 0.01 g) of matrix
vegetable oil to place into a 20-mL headspace specimen bottle.
4.4.2 For meals, weigh 6 shares of 3.0 g (accurate to 0.01 g) of matrix meal to place
into a 20-mL headspace specimen bottle; add 400 μL of water to each headspace
specimen bottle; finally use microsyringe to add quickly 0 μL, 3 μL, 9 μL, 15 μL, 30 μL
and 150 μL of no. 6 solvent standard product; after sealing, obtain the matrix meal
standard solutions of concentrations 0 mg/kg, 10 mg/kg, 30 mg/kg, 50 mg/kg, 100
mg/kg and 500 mg/kg.
5 Apparatus
5.1 Gas chromatograph. equipped with flame ionization detector.
5.2 Headspace bottle. 20 mL, equipped with aluminium cover and sealing washer of
butyl rubber or silicon resin containing no residual of hydrocarbon solutions.
5.5 Ultrasonic oscillator.
5.6 Air blowing oven.
5.7 Thermostatic oscillator.
6 Analytical Procedure
6.1 Specimen preparation
6.1.1 Preparation of vegetable oil specimen. weigh 5 g (accurate to 0.01 g) of
vegetable oil specimen to place into a 20-mL headspace specimen bottle; add quickly
5 μL of n-heptane standard working solution to vegetable oil specimen as internal
standard; use hand to shake up before sealing. Keep headspace specimen bottle
upright for analysis. During the preparation, vegetable oil specimen shall not touch
sealing washer; if vegetable oil specimen touches sealing washer, the specimen shall
be prepared once again.
6.2 Instrument reference conditions
6.2.1 Headspace specimen injector reference conditions
The reference conditions for headspace specimen injector are as follows.
6.2.2 Gas chromatography reference conditions
The reference conditions for gas chromatography are as follows.
6.3 Plotting of standard curves
6.3.1 For vegetable oils, the internal standard method is used in this method for
quantitation.
6.4 Specimen determination
After analyzing the prepared vegetable oil or meal specimen, measure its peak area
and calculate the solvent residual in specimen in accordance with relevant standard
curves.
7 Expression of Analytical Results
The content of solvent residual in specimen is calculated in accordance with Formula
(1).
8 Accuracy
The absolute difference between the results of two independent measurements under
repeatable conditions shall not exceed 10% of the arithmetic mean value.
9 Others
The detection limits and quantitation limits of this method are as follows.
Annex A
Gas Chromatogram of No. 6 Solvent
See Figure A.1 for the gas chromatogram of no. 6 solvent.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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