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GB 21926-2016: Determination of 2-dodecylcyclobutanone in irradiated foods containing fat -- GC/MS method
Status: Valid GB 21926: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GB 21926-2016 | English | 119 |
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Determination of 2-dodecylcyclobutanone in irradiated foods containing fat -- GC/MS method
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GB 21926-2016
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| GB/T 21926-2008 | English | 319 |
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Determination of 2-Dodecylcyclobutanone in Irradiated foods Containing Fat -- GC/MS Method
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GB/T 21926-2008
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PDF similar to GB 21926-2016
Basic data | Standard ID | GB 21926-2016 (GB21926-2016) | | Description (Translated English) | Determination of 2-dodecylcyclobutanone in irradiated foods containing fat -- GC/MS method | | Sector / Industry | National Standard | | Classification of Chinese Standard | X10 | | Word Count Estimation | 6,60 | | Date of Issue | 2016-12-23 | | Date of Implementation | 2017-06-23 | | Regulation (derived from) | National Health and Family Planning Commission Notice No.17 of 2016 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration | GB 21926-2016: Determination of 2-dodecylcyclobutanone in irradiated foods containing fat -- GC/MS method
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of 2 - dodecylcyclobutanone in irradiated foods containing fat - GC/MS method
National Standards of People's Republic of China
National Food Safety Standard
Identification of lipid-containing irradiated food
2-dodecyl cyclobutanone GC -
Mass spectrometry
Published 2016-12-23
2017-06-23 implementation
National Health and Family Planning Commission People's Republic of China
China Food and Drug Administration issued
Foreword
Instead of the standard GB/T 21926-2008 "irradiated food containing fat 2-dodecyl-azetidinone by Gas Chromatography/Mass Spectrometry."
As compared with the present standard GB/T 21926-2008, the main changes are as follows.
--- standard name changed to "Food Safety Standard irradiated food containing lipid-2-dodecyl cyclobutanone identified by gas chromatography -
Mass Spectrometry ";
--- Improved silica gel column chromatography.
National Food Safety Standard
Identification of lipid-containing irradiated food
2-dodecyl cyclobutanone GC -
Mass spectrometry
1 Scope
This standard specifies the use of 2-dodecyl-azetidinone lipid-containing food irradiation identified by gas chromatography - mass spectrometry.
This standard applies to the identification of irradiated food fat content greater than 1%.
Principle 2
After extraction using n-hexane fat sample cyclobutanone and 2-dodecyl out together, purification by silica gel column chromatography, concentrated gas
Chromatography - mass spectrometer 2-dodecyl cyclobutanone, external standard.
3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are analytically pure water three water GB/T 6682 provisions.
3.1 Reagent
3.1.1 hexane (C6H14).
3.1.2 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4h, cool in a desiccator, stored for use.
3.1.3 ether (C4H10O).
3.1.4 nitrogen (N2). purity ≥99.999%.
3.1.5 helium (He). purity ≥99.999%.
3.2 Material
Silicone. 250μm ~ 500μm, column chromatography. Before use, the activated silica gel placed in an oven at 100 deg.] C 12h, cool in a desiccator. in
Stoppered Erlenmeyer flask was added 4% (mass ratio) of water deactivation of the conical flask shaken until uniformly dispersed silica. The deactivated silica gel in a desiccator
Ping Heng 12h, available within a week.
3.3 Standard
2-dodecyl cyclobutanone standard (C16H30O). purity ≥99%.
3.4 Standard Preparation
3.4.1 2-dodecyl azetidinone standard stock solution
Accurately weighed amount of 2-dodecyl cyclobutanone standard (accurate to 0.1 mg), was dissolved with n-hexane, formulated at a concentration of 100μg/mL of
Standard stock solution, -20 ℃ storage, 3 months effective.
3.4.2 2-dodecyl azetidinone standard working solution
Standard stock solution was diluted with hexane (100μg/mL), were formulated as 0.10μg/mL, 0.25μg/mL, 0.50μg/mL, 1.00
Standard working solution levels μg/mL, 2.50μg/mL, 5.00μg/mL of, -20 ℃ storage 1 month effective, but appear abnormal peaks
You should consider re-formulated.
4 instruments and equipment
4.1 GC-MS. with a less polar (e.g., DB-5) and suitable properties or specifications of the capillary column, column length. 30m, inner diameter. 0.25mm, film
Thickness. 0.25μm.
4.2 Soxhlet extractor.
4.3 Nitrogen blowing instrument.
4.4 electric mixer.
4.5 Ovens.
4.6 temperature water bath.
4.7 rotary evaporator.
4.8 Electronic balance. a sense of the amount of 0.1mg.
4.9 Glass chromatography columns. column length.200mm ~ 300mm, inner diameter. 20mm.
b) inlet temperature. 250 ℃;
c) Interface temperature. 280 ℃;
d) Ion source. EI source, 70eV;
e) Measurement mode. SIM (the SIM); ion monitoring (m/z). 55,98,112, quantitative ion (m/z). 98;
f) Carrier gas. Helium, flow rate 1.0mL/min;
g) Injection volume. 1.0μL;
h) Injection mode. splitless.
6 expression analysis results
Standard working solution and the volume of the sample solution and the like is inserted into the sample measured parameters, external standard. In the chromatographic conditions, 2-dodecyl cyclobutanone
Selected ion chromatogram of the standard sample shown in Figure A.1.2- dodecyl cyclobutanone retention time of approximately 17.1 min, mass spectrum is shown in Figure A.2.
2-dodecyl cyclobutanone peaks detected if the sample liquid retention time retain the 2-dodecyl cyclobutanone standard peaks
Same time (relative deviation ≤2s), which spectrum is consistent with the 2-dodecyl cyclobutanone standard spectrum, after deducting the background monitor select
Measuring ions m/z55,98 and 112 both occur, and the relative abundance of m/z55,112 and the base peak m/z98 and the ratio of standard 2-dodecyl cyclobutanone
Registration deviation relative abundance ratio not exceeding 20%, can be detected in the sample confirmed 2-dodecyl cyclobutanone, indicated the sample had received irradiated
deal with.
Appendix A
2-dodecyl cyclobutanone standard chromatogram and mass spectrum
A.1 2- azetidinone-dodecyl selected ion chromatogram of the standard
2-dodecyl azetidinone standards selected ion chromatogram shown in Figure A.1.
FIG A.1 2- azetidinone-dodecyl selected ion chromatogram of the standard
A.2 2- azetidinone-dodecyl standard full scan mass spectrum
2-dodecyl azetidinone standard full-scan mass spectra shown in Figure A.2.
FIG A.2 2- azetidinone-dodecyl standard full scan mass spectrum
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