GB 5009.148-2014 English PDF

GB 5009.148-2014: National Food Safety Standard -- Determination of Free Gossypol in Vegetable Food
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GB 5009.148-2014
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard - Determination of free
gossypol in vegetable good
ISSUED ON: FEBRUARY 04, 2015
IMPLEMENTED ON: MAY 01, 2015
Issued by: National Health and Family Planning Commission of PRC
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Principle ... 4 
3 Reagents and materials ... 4 
4 Instrument and equipment ... 5 
5 Analytical procedures ... 5 
6 Expression of analysis results ... 6 
7 Precision ... 7 
8 Others ... 7 
Appendix A Standard solution of gossypol and sample spiked chromatogram 8 
National food safety standard - Determination of free
gossypol in vegetable good
1 Scope
This standard specifies the method for determination of free gossypol in
vegetable oil or other liquid foods using cottonseed cake as raw material.
This standard applies to the determination of free gossypol in vegetable oil or
other liquid foods using cottonseed cake as raw material.
2 Principle
The free gossypol in vegetable oil was extracted by absolute ethanol and
detected by high performance liquid chromatography. The retention time of the
chromatographic peak is qualitatively determined, and it is quantified by
external standard method.
The free gossypol in the water-soluble liquid sample using cottonseed cake as
the raw material is extracted by the use of anhydrous ether, concentrated to
dryness, then dissolved in ethanol, detected by high performance liquid
chromatography. The retention time of the chromatographic peak is qualitatively
determined, and it is quantified by external standard method.
3 Reagents and materials
Note: Unless otherwise specified, the reagents used in this method are all analytically
pure; the water is the level 1 water as specified in GB/T 6682.
3.1 Reagents
3.1.1 Phosphoric acid (H3PO4).
3.1.2 Anhydrous ethanol (CH3CH2OH).
3.1.3 Acetone (C3H6O).
3.1.4 Nitrogen (N2).
3.1.5 Methanol (CH3OH).
upper layer of ether. Use nitrogen to blow it dry. Use 1.0 mL of absolute ethanol
to make its volume reach to the mark. Make it pass through a 0.45 μm filter
membrane, which is the sample solution.
5.2 Chromatographic determination
5.2.1 Reference chromatographic conditions
Chromatographic column: C18 column, 250 mm × 4.6 mm, 5 μm, or a column
with equivalent performance.
Mobile phase: Methanol: phosphoric acid solution = 85: 15.
Flow rate: 1.0 mL/min.
Column temperature: 40 °C ± 1 °C.
Measurement wavelength: 235 nm.
Sample injection volume: 10 μL.
5.2.2 Drawing standard curve
Inject the standard working solution of gossypol into the high performance liquid
chromatograph and record the peak height or peak area. Draw a standard curve
with the peak height or peak area as the ordinate and the concentration of the
standard working solution of gossypol as the abscissa (see Figure A.1 in
Appendix A for the liquid chromatogram of the standard solution).
5.2.3 Specimen measurement
Inject the specimen solution into the high performance chromatograph. Record
the peak height or peak area. Calculate the concentration of gossypol in the
test solution based on the standard curve (see Figure A.2 in Appendix A for the
sample spiked liquid chromatogram).
6 Expression of analysis results
The free gossypol content in specimen 5.1.1 is calculated according to formula
(1):
Where:
X - The content of gossypol in the specimen, in milligrams per kilogram
GB 5009.148-2014
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard - Determination of free
gossypol in vegetable good
ISSUED ON: FEBRUARY 04, 2015
IMPLEMENTED ON: MAY 01, 2015
Issued by: National Health and Family Planning Commission of PRC
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Principle ... 4 
3 Reagents and materials ... 4 
4 Instrument and equipment ... 5 
5 Analytical procedures ... 5 
6 Expression of analysis results ... 6 
7 Precision ... 7 
8 Others ... 7 
Appendix A Standard solution of gossypol and sample spiked chromatogram 8 
National food safety standard - Determination of free
gossypol in vegetable good
1 Scope
This standard specifies the method for determination of free gossypol in
vegetable oil or other liquid foods using cottonseed cake as raw material.
This standard applies to the determination of free gossypol in vegetable oil or
other liquid foods using cottonseed cake as raw material.
2 Principle
The free gossypol in vegetable oil was extracted by absolute ethanol and
detected by high performance liquid chromatography. The retention time of the
chromatographic peak is qualitatively determined, and it is quantified by
external standard method.
The free gossypol in the water-soluble liquid sample using cottonseed cake as
the raw material is extracted by the use of anhydrous ether, concentrated to
dryness, then dissolved in ethanol, detected by high performance liquid
chromatography. The retention time of the chromatographic peak is qualitatively
determined, and it is quantified by external standard method.
3 Reagents and materials
Note: Unless otherwise specified, the reagents used in this method are all analytically
pure; the water is the level 1 water as specified in GB/T 6682.
3.1 Reagents
3.1.1 Phosphoric acid (H3PO4).
3.1.2 Anhydrous ethanol (CH3CH2OH).
3.1.3 Acetone (C3H6O).
3.1.4 Nitrogen (N2).
3.1.5 Methanol (CH3OH).
upper layer of ether. Use nitrogen to blow it dry. Use 1.0 mL of absolute ethanol
to make its volume reach to the mark. Make it pass through a 0.45 μm filter
membrane, which is the sample solution.
5.2 Chromatographic determination
5.2.1 Reference chromatographic conditions
Chromatographic column: C18 column, 250 mm × 4.6 mm, 5 μm, or a column
with equivalent performance.
Mobile phase: Methanol: phosphoric acid solution = 85: 15.
Flow rate: 1.0 mL/min.
Column temperature: 40 °C ± 1 °C.
Measurement wavelength: 235 nm.
Sample injection volume: 10 μL.
5.2.2 Drawing standard curve
Inject the standard working solution of gossypol into the high performance liquid
chromatograph and record the peak height or peak area. Draw a standard curve
with the peak height or peak area as the ordinate and the concentration of the
standard working solution of gossypol as the abscissa (see Figure A.1 in
Appendix A for the liquid chromatogram of the standard solution).
5.2.3 Specimen measurement
Inject the specimen solution into the high performance chromatograph. Record
the peak height or peak area. Calculate the concentration of gossypol in the
test solution based on the standard curve (see Figure A.2 in Appendix A for the
sample spiked liquid chromatogram).
6 Expression of analysis results
The free gossypol content in specimen 5.1.1 is calculated according to formula
(1):
Where:
X - The content of gossypol in the specimen, in milligrams per kilogram