GB/T 22507-2008 PDF English
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Animal and vegetable fats and oils -- Determination of the content of trans fatty acid isomers of vegetable fats and oils -- Gas chromatographic method
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GB/T 22507-2008: PDF in English (GBT 22507-2008) 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
ICS 67.040
X04
National Standards of People's Republic of China
GB/T 22507-2008/ISO 15304.2002
Animal and vegetable fats vegetable oils trans fatty acid isomers
Determination by gas chromatography
(ISO 15304.2002, IDT)
Posted 2008-11-04
2009-01-20 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
This standard is identical with ISO 15304.2002 "Animal and vegetable fats vegetable oils Determination of trans fatty acid isomers by GC
Law "(in English).
For ease of use, the standard ISO 15304.2002 includes the following editorial changes.
--- "This International Standard" be replaced by "this standard";
"." --- With a decimal point instead of a comma as the decimal point, "";
--- Delete international standards foreword, preface adds this standard;
--- Delete ISO 15304.2002 in the informative overview of elements (including the cover, inside front cover, preface);
--- According to ISO 15304.2002 Technical Corrigendum 1, Figure B. 2 marked correct;
--- With GB/T 17376 "fatty acid methyl esters prepared animal fat" instead of ISO 5509.2000.
The Standard Appendix A, Appendix B, Appendix C, Appendix D and Appendix E are informative appendices.
The standard proposed by the National Food Authority.
This standard by the National Standardization Technical Committee OILS.
This standard was drafted. Academy of State Grain Administration, Jiangnan University School of food.
The main drafters of this standard. Rui Zhang, Xue Yalin, Wang Xingguo, PROJECTILES.
GB/T 22507-2008/ISO 15304.2002
Animal and vegetable fats vegetable oils trans fatty acid isomers
Determination by gas chromatography
1 Scope
This standard specifies the vegetable oil trans fatty acid isomers of determination by capillary column gas chromatography.
This standard uses a single capillary column gas chromatography (GC) method for the determination of generating (high temperature) refining or hydrogenated vegetable oils trans-iso
Structure content of the body.
The same standard in the same sample analysis can also be given in the report of other fatty acids (for example. total fatty acid composition, saturated fatty acids, single
Unsaturated fatty acids and polyunsaturated fatty acids of the total).
Note 1. The trans isomer content may be obtained by the standard method of obtaining other trans isomer content is not the same.
Note 2 .( temperature) refining (deacidification and deodorization) produced only monounsaturated fatty acids and polyunsaturated fatty acids geometric isomers, such as the double bond position remains unchanged;
Hydrogenation process produces both positional isomers and geometric isomers produced.
Note 3. Some special produced by hydrogenation of cis, trans isomers may also peaks will affect the accuracy of the results. Typically, this part of the partially hydrogenated oils heterogeneous
Body may be negligible.
2 Normative references
The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research
Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.
GB/T 15687 animal and plant oils prepared sample (GB/T 15687-2008, ISO 661.2003, IDT)
GB/T 17376 Animal and vegetable fats fatty acid methyl esters prepared (GB/T 17376-2008, ISO 5509.2000, IDT)
3 Terms and Definitions
The following terms and definitions apply to this standard.
3.1
3.2
The sum of all trans double bonds of fatty acid methyl esters, expressed as a mass fraction of total fatty acid methyl esters.
Note. The content of trans fatty acid isomers, expressed as a percentage.
Principle 4
Based on the fatty acid carbon chain length, (not) the different degree of saturation, geometry and position of double bonds in the polar stationary phase by capillary gas chromatography
Spectral separation column fatty acid methyl ester sample.
5 Reagents and materials
Unless otherwise specified, use only analytical reagent.
GB/T 22507-2008/ISO 15304.2002
5.1 The carrier gas
Use a dry, remove gas chromatography grade oxygen carrier gas, preferably helium, hydrogen or nitrogen.
Warning --- only when using capillary column analysis, optional hydrogen as a carrier gas, make analysis faster than doubled (relative to helium
Ratio), but there is a risk. Hydrogen should be used with safety devices, safety devices, combined with the instrument together is the basic requirement.
5.2 has certified reference material (CRM)
BCR162 (soybean/corn hybrid) can be obtained from the European Commission (EC) Standards Board.
NOTE. In addition to the EC CRM, but also to use well-known vendors such as calibration standards Supelco, Larodan, Nuchek and Sigma companies. different
Hydrogenated oils should choose different standards (for example. lauric oil, lauric oils and palm oil-free).
6 Instruments
Common laboratory instruments, and the following special equipment.
6.1 Gas chromatograph. equipped with capillary injection system (preferably with shunt, shunt ratio of about 1.100) and flame ionization detector
(FID).
6.2 Capillary column. having a strong polar stationary phase (for example, CPTM-Sil88, SP-2340, BPX-70 or similar polar cyanopropyl stationary phase,
Such as the SP-2380 and SP-2560, they also have different geometric isomers similar resolving power).
Note. In order to increase the separation effect, it is recommended to use the SP-2560 or 100m CPTM-Sil88 column, hydrogen as a carrier gas.
Column specifications are as follows.
--- CPTM-Sil88, (50m ~ 100m) × 0.25mm inner diameter, 0.20μm;
--- SP-2360, (50m ~ 100m) × 0.25mm inner diameter, 0.2μm;
--- SP-2340,60m × 0.25mm inner diameter, 0.2μm;
--- BPX-70,50m × 0.22mm inner diameter, 0.25μm.
Best conditions used are listed in 10.2.1, see Appendix A.
7 for sampling
This standard does not provide for sampling method is recommended for sampling execution GB/T 5524 "Animal and vegetable fats for sampling." [1].
Laboratory received the samples should be representative, it has not been damaged in transit and during storage or change.
8 Sample Preparation
Sample preparation according to GB/T 15687 execution.
Before removing the test portion from the sample, the sample mixed well. Solid sample is completely melted to ensure adequate mixing.
Preparation 9 Methyl
In accordance with GB/T 17376 A sample of the methyl esterification of triglycerides.
May also be used AOCSCe2-66 [2] or IUPAC2.301 [3] Method.
Determination of trans isomers, such as extra virgin olive oil, according to GB/T 17376 trans esterification procedures, the sample should be avoided
heating.
10 analysis steps
10.1 General
At the same analytical sample (or series of samples), blank samples (n-heptane) and a reference sample (CRM) (5.2).
10.2 GC conditions
10.2.1 Selection Table 1 Recommended set temperature and column, set the gas chromatograph. Table 1 to adjust the carrier gas linear velocity, the split ratio of about
100. A typical chromatogram under chromatographic conditions given in Table 1 obtained see Appendix B.
GB/T 22507-2008/ISO 15304.2002
Table 1 hydrogenated vegetable oil refining and trans-isomers of qualitative and quantitative GC recommended conditions of use
Parameters recommended best operating conditions
Stationary phase SP-2340 CPTM-Sil88 BPX-70
Temperature/℃ 192 175 198
Pre-column pressure/kPa 125 130 155
Linear velocity carrier gas (helium)/(cm/s) 15 19 17
Column parameter recommendations 100m optimum conditions
Stationary phase SP-2560 CPTM-Sil88 CPTM-Sil88
Temperature/℃
120 to 240
(4 ℃/min)
Pre-column pressure/kPa 220 170 160
Linear velocity carrier gas (hydrogen)/(cm/s) 30 30 30
10.2.2 inlet temperature and the detector temperature was 250 ℃.
10.3 Performance check
0.5μL ~ 1μL draw a sample of the methyl ester (concentration of approximately 7mg/mL heptane), injected into a gas chromatograph for analysis. The similar kind
Product test results Appendix B typical chromatograms comparison. As examples of spectra and chromatograms obtained are not identical, they need to enter the oven temperature
Fine adjustment. 1 ℃ each time the magnitude of increase or decrease in the temperature of the oven, until a good separation effect. By fine-tuning can eliminate batch chromatography
Differences column and instrument temperature control, generally indicates the temperature range of fine-tuning of the positive and negative within a few degrees.
Peak (Control Appendix B).
Such as gas chromatography system is set up correctly, refining (high temperature) in oil, such as. soybean oil, a small amount of spectrum should naturally occurring C18.1
NOTE. hydrogenated marine oil more difficult to produce a wider range of trans isomers, qualitative and quantitative.
(Linolenic acid) between the peak C18.3 Ba Ba Ba. For this type of analysis, if sufficient separation, refining (high temperature) oil, there should C18.1
Peak body.
Isomer peak between precise degree of separation (see Appendix B).
10.4 peak identification
Refining (high temperature) fats, trans isomer limited number, produce only geometric isomers, the double bond position remains unchanged. These special exclusive
In partially hydrogenated oils, and other isomers with a chain length (ECL) concept contain trans double bonds identified. In order to use this system on the peaks
Accurate identification, should be in the cis and trans fatty acid with a valid standard isomer 1) calibration, measured ECL value (see Appendix C).
1) You can buy [such as Nu-CheckPrepInc from many suppliers of chemical reagents. (United States); Sigma (USA); Larodan (Sweden)].
In each analysis, a sample of the first blank (n-heptane). When you run the blank, there should be no peak is detected. Ten samples per test
After testing a blank.
GB/T 22507-2008/ISO 15304.2002
Each batch of analysis (for example, a number of methylated each), at least analyzing a reference sample (5.2), to check the performance of methyl and gas analytical
can. Every ten samples measured backward needle has a methyl ester of the reference sample.
11 Calculation results
11.1 General
The relative content of each component and the ratio of the area of all peaks in the calibration calculated by measuring the area of the corresponding component peaks calibration. Calibration
FID response to the compensation value for each component. Use BCR standard (see 5.2) measured the individual components of the calibration factor.
11.2 Calculation FID response factor
The components FID calculated by the formula (1) Response Factor.
Fx = Mx (like x-1) AC
(1)
Where.
FID Fx --- composition x response factor;
Relative molar mass MX --- composition x;
Like x --- carbon atoms esterified fatty acid composition x;
AC --- relative atomic mass of carbon atoms (AC = 12.01).
The formula gives a theoretical response factor.
11.3 Calculation FID calibration factor
By the formula (2) calibration factors calculated for each component FID.
(2)
Where.
FID Fx --- composition x response factor;
FID Fr --- C16.0 response factor (Fr = 1.407).
This factor is a relative value. For example, C10.0 calibration response factor of 1.10. See Appendix D listed FID factor.
11.4 to calculate the relative mass fraction
(3) calculated by the relative content of each component type.
(3)
Where.
Relative mass fraction of component x x --- peak area percentage method of calculation;
--- AX composition x corresponding peak area;
The sum of all the peaks AT --- calibration area, removing the solvent peak.
11.5 calculate the content of trans fatty acid isomers
11.5.1 Refining (high temperature) oil
Results are accurate to 0.01% (mass fraction).
11.5.2 partially hydrogenated oils
Partially hydrogenated fat content of trans fatty acid isomers, expressed as relative to all the fatty acid methyl ester, all trans fatty acids containing double bonds
GB/T 22507-2008/ISO 15304.2002
Methyl ester fraction relative to the total mass.
Results are accurate to 0.1% (mass fraction).
12 Precision
12.1 Joint Experiment
The report of the joint experimental precision of the method in Appendix E. When the concentration exceeds the concentration range has been given, these joint experiments measured
Test data may not apply.
Note. The individual level of partially hydrogenated oils contain trans fatty acids beyond the level range from joint experiments.
12.2 Repeatability
In the same laboratory by the same operator using the same equipment, the same testing methods in a short time on the same object to be measured phase
12.3 Reproducibility
In different laboratories by different operators using different equipment, according to the same test method for the same object to be measured independently of each other
Under test conditions, the absolute difference between the two measurement result exceeds the value given in Table 2 R case not exceed 5%.
sample
Trans fatty acid isomers
Average content /% (mass fraction)
% (Mass fraction)
R /
% (Mass fraction)
Sunflower oil 0.34 0.08 0.21
Soybean Oil 0.78 0.13 0.31
Rapeseed Oil 1.09 0.13 0.40
13 Test Report
Test Report Description.
--- Completely identify all of the information required for the sample;
--- Methods for sampling;
--- About this test method criteria used;
--- All not specified in this standard or regarded as optional in the details of the operation and use of this method may affect the results of the measurements
event;
--- Obtain test results;
--- If the test reproducibility, the results are listed.
GB/T 22507-2008/ISO 15304.2002
Appendix A
(Informative)
Optimal conditions
Optimal conditions Figure A. 1 to A. 3.
Peak identification.
Figure A. 1 BPX-70 column optimum conditions, 198 ℃ (isothermal), sample BO35
GB/T 22507-2008/ISO 15304.2002
Peak identification.
Peak identification.
Figure A. 3 SP-2340 column optimum conditions, 192 ℃ (isothermal), sample BO35
GB/T 22507-2008/ISO 15304.2002
Appendix B
(Informative)
Representative examples of FIG chromatogram obtained under the recommended conditions
Methyl chromatography shown in Figure B. 1 to B. 5.
NOTE. 50m × 0.25mm × 0.20μm, CP
Fatty acid isomers reserved area.
Figure B. 1 chromatogram of partially hydrogenated soybean oil methyl ester sample
GB/T 22507-2008/ISO 15304.2002
Isomer reserved area.
Figure B. 2 partially hydrogenated soybean oil sample chromatogram of methyl
GB/T 22507-2008/ISO 15304.2002
Reserved area.
Figure B. 3 the chromatogram partially hydrogenated soybean oil methyl ester sample
GB/T 22507-2008/ISO 15304.2002
NOTE. 50m × 0.25mm × 0.20μm, CP
section.
Figure B. 4 chromatograms physical refining of rapeseed oil methyl ester sample
GB/T 22507-2008/ISO 15304.2002
Figure B. 5 high-temperature refining chromatograms of rapeseed oil methyl ester sample
GB/T 22507-2008/ISO 15304.2002
Appendix C
(Informative)
And other chain length (ECL) value
And other chain length (ECL) are given in Table C. 1.
Table C. 1 and other chain length (ECL) value
C18 isomer
Stationary phase and temperature
SP-2340
192 ℃
CPTM-Sil88
175 ℃
BPX-70
198 ℃
C18.1
C18.2
Ba Ba 9 12 19.62 19.63 19.14
12 15 Ba Ba - 19.92 -
C18.3
6 9 Ba Ba Ba 12 - 20.28 -
12 Ba Ba Ba 9 15 20.68 20.67 19.93
Note 1. in three polar stationary phase and recommend the best conditions, UnileverResearchVlaardinggen [Vlaardingen (Netherlands southwestern port city of)]
Found mainly fatty acid isomers.
Note 2. The literature data, see reference [5] and [6].
GB/T 22507-2008/ISO 15304.2002
Appendix D
(Informative)
FID FID response factors and calibration factor
FID FID response factors and calibration factors are shown in Table D. 1.
Table D. 1 FID FID response factors and calibration factor
Fatty acid methyl ester (x) in
Fatty acid carbon atoms
4-0 4 2.126 1.51 102.13
6-0 6 1.807 1.28 130.19
8.0 8 1.647 1.17 158.24
9.0 9 1.594 1.13 172.27
10.0 186.30 10 1.551 1.10
11.0 200.32 11 1.516 1.08
12.0 214.35 12 1.487 1.06
13.0 228.37 13 1.463 1.04
14.0 242.40 14 1.442 1.02
15.0 256.42 15 1.423 1.01
16.0 270.46 16 1.407 1.00 (reference)
17.0 284.49 17 1.393 0.99
18.0 298.52 18 1.381 0.98
19.0 312.52 19 1.370 0.97
20.0 326.57 20 1.360 0.97
21.0 340.57 21 1.350 0.96
22.0 354.62 22 1.342 0.95
23.0 368.62 23 1.334 0.95
24.0 382.68 24 1.328 0.94
aMx relative molecular mass composition x;
Fatty acid methyl ester-like component x to x carbon atoms;
Fx for the FID component x factor;
GB/T 22507-2008/ISO 15304.2002
Appendix E
(Informative)
Joint laboratory test results
1995 in accordance with ISO 5725-1 [7], ISO 5725-2 [8] and MEN6303 [9] conducted a joint laboratory to test the precision of the method.
60 laboratories participated in the test. 38 laboratory results to be accepted. Test 6 blind sample. sunflower oil, soybean oil and rapeseed oil
Each of the two (see Table E.1). Test report has been published (see reference [10]).
NOTE. Individual levels of trans fatty acids in hydrogenated oils partially beyond the level ranges from laboratory tests.
Table E. 1 Joint Laboratory test results
project
sample
Sunflower oil soybean oil rapeseed
Excluding number of laboratories after the outlier laboratory 383 837
Excluding the results of outlier results acceptable number 144 147 143
Trans-isomer fatty acid content of the average /% (mass fraction) 0.34 0.78 1.09
Repeatability relative standard deviation /% 8.64 5.85 4.34
Reproducibility standard deviation SR /% (mass fraction) 0.077 0.109 0.143
Reproducibility relative standard deviation/22.64 14.07 13.14%
Reproducibility limit R (R = 2.8SR) /% (mass fraction) 0.21 0.31 0.40
In 1999, UnileverResearchVlaardingen multi-laboratory study associations organize different types of edible oils trans
Determination of fatty acid isomers of international joint laboratory testing. 62 laboratories from 29 different countries participated in the interlaboratory testing;
57 laboratories returned results. According to ISO 5725-2, the calculation method using the same level of repeatability limit and reproducibility limit. Research on six samples.
Sunflower oil, rapeseed oil and olive oil each two (see Table E.2 ~ Table E.4).
Table E. 2-sunflower oil laboratory test results
project
Sunflower seed oil
transC18.1 transC18.2 transC18.3
Total trans fatty acids
isomer
Excluding number of laboratories after the outlier laboratory 39,513,050
Excluding the results of outlier results acceptable number 468612360600
Trans-isomer fatty acid content of the average /% (mass fraction) 0.029 0.154 0.033 0.205
Repeatability relative standard deviation/21.65 7.49 5.8 18.48%
Reproducibility standard deviation SR /% (mass fraction) 0.014 0.030 0.013 0.048
Reproducibility relative standard deviation /% 46.80 19.25 38.96 23.17
Reproducibility limit R (R = 2.8SR) /% (mass fraction) 0.038 0.083 0.036 0.133
GB/T 22507-2008/ISO 15304.2002
Table E. 3-rapeseed laboratory test results
project
Rapeseed oil
transC18.1 transC18.2 transC18.3
Total trans fatty acids
isomer
Excluding number of laboratories after the outlier laboratory 33,484,747
Excluding the results of outlier results acceptable number 396576564564
Trans-isomer fatty acid content of the average /% (mass fraction) 0.032 0.074 0.406 0.521
Repeatability relative standard deviation/15.63 15.93 3.69 5.21%
Reproducibility standard deviation SR /% (mass fraction) 0.009 0.020 0.058 0.081
Reproducibility relative standard deviation /% 29.02 27.03 14.16 15.63
Reproducibility limit R (R = 2.8SR) /% (mass fraction) 0.026 0.056 0.161 0.228
Table E. Olive oil 4 laboratory test results
project
olive oil
transC18.1 transC18.2 transC18.3
Total trans fatty acids
isomer
Excluding number of laboratories after the outlier laboratory 31,362,240
Excluding the results of outlier results acceptable number 372432264480
Trans-isomer fatty acid content of the average /% (mass fraction) 0.023 0.021 0.016 0.055
Repeatability relative standard deviation /% 23.29 34.01 29.02 22.08
Reproducibility standard deviation SR /% (mass fraction) 0.009 0.011 0.009 0.030
Reproducibility relative standard deviation /% 40.37 51.02 53.57 54.55
Reproducibility limit R (R = 2.8SR) /% (mass fraction) 0.026 0.030 0.024 0.084
GB/T 22507-2008/ISO 15304.2002
references
[1] GB/T 5524 Animal and vegetable fats for sampling (GB/T 5524-2008, ISO 5555.2001, IDT)
[4] DUCHATEAUG. S. M. J. E, vanOOSTENH. J. andVASCONCELLOSM. A. Analysis
[5] SCHOLFIELDC. R. Gaschromatographicequivalentchainlengthsoffattyacidmethyles-
[6] RATNAYAKEW. M. N. andPELLETIERG. Positionalandgeometricalisomersoflinole-
[10] BRUGGENP. C. van, DUCHATEAUG. S. M. J. E. , MOOREN, M. M. W. andOOST-
GB/T 22507-2008/ISO 15304.2002
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