|
US$179.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email.
GB 23200.27-2016: Food safety national standard -- Determination of 4,6-dinitro-o-cresol Residue in Fruits by Gas Chromatography -- Mass Spectrometry
Status: Valid
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GB 23200.27-2016 | English | 179 |
Add to Cart
|
3 days [Need to translate]
|
Food safety national standard -- Determination of 4,6-dinitro-o-cresol Residue in Fruits by Gas Chromatography -- Mass Spectrometry
| Valid |
GB 23200.27-2016
|
PDF similar to GB 23200.27-2016
Basic data | Standard ID | GB 23200.27-2016 (GB23200.27-2016) | | Description (Translated English) | Food safety national standard -- Determination of 4,6-dinitro-o-cresol Residue in Fruits by Gas Chromatography -- Mass Spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 9,910 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 1734-2006 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of 2016 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration | GB 23200.27-2016: Food safety national standard -- Determination of 4,6-dinitro-o-cresol Residue in Fruits by Gas Chromatography -- Mass Spectrometry
---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.
Food safety national standard - Determination of 4,6 - dinitro - o - cresol Residue in Fruits by Gas Chromatography - Mass Spectrometry
National Standards of People's Republic of China
GB
Instead of SN/T 1734-2006
National standards for food safety
Determination of 4,6 - dinitro - o - cresol Residue in Fruits
Gas chromatography - mass spectrometry
National food safety standards-
Determination of 4, 6-dinitro-cresol residue in fruits
Gas chromatography - mass spectrometry
2016-12-18 Release.2017-06-18 Implementation
National Health and Family Planning Commission of the People 's Republic of China
Issued by the Ministry of Agriculture of the People 's Republic of China
State Administration of Food and Drug Administration
Foreword
This standard replaces SN/T 1734-2006 "Test Method for Residue of 4,6-Dinitro-o-cresol in Import and Export Fruits Gas Chromatography-Mass Spectrometry
law".
Compared with SN/T 1734-2006, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the name of the "import and export fruit" to "fruit".
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 1734-2006.
National standards for food safety
Determination of 4,6 - dinitro - o - cresol Residue in Fruits by Gas Chromatography - Mass Spectrometry
1 Scope
This standard specifies the method for the determination of 4,6-dinitro-o-cresol residues in fruit by gas chromatography-mass spectrometry.
This standard applies to the apple, pear 4,6 6-dinitro-o-cresol residue test, other food can refer to the implementation.
2 normative reference documents
The following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this article
Pieces. For undated references, the latest edition (including all modifications) applies to this document.
GB 2763 National Standard for Food Safety - Maximum Residue Limit of Pesticides in Foodstuffs
GB/T 6682 Analytical laboratory water specifications and test methods.
3 principle
Fruit sample 4,6-dinitro-o-cresol residue extracted with dichloromethane, blowing nitrogen to dry after acetonitrile dissolved, with N- (p-butyl dimethyl
(MTBSTFA), which was determined by gas chromatography-mass spectrometry and quantified by external standard method.
4 reagents and materials
Unless otherwise specified, all reagents are of analytical grade and water is in accordance with the primary water specified in GB/T 6682.
4.1 Reagents
4.1.1 dichloromethane (CH2Cl2). excellent grade pure.
4.1.2 acetonitrile (CH3CN). pure chromatography.
4.1.3 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, placed in the dryer in the spare.
4.1.4 Derivative reagent N- (tert-butyldimethylsilyl) -N-methyltrifluoroethylphthalide (MTBSTFA). 99% purity.
4.2 standards
4.2.1 4,6-dinitro-o-cresol standard (C7H6N2O5, CAS No .. 534-52-1). purity 99%.
4.3 standard solution preparation
4.3.1 4,6-dinitro-o-cresol standard stock solution. accurately weighed 10 mg 6,6-dinitro-o-cresol standard, dissolved in acetonitrile and prepared
Into the concentration of 100 rng/L of the standard stock solution, can be stored in the refrigerator 0 ℃ ~ 4 ℃ for 3 months.
4.3.2 4,6-dinitro-o-cresol standard working solution. according to the need for acetonitrile will be 4,6-dinitro-o-cresol standard stock solution diluted to the appropriate concentration
Degree of standard working fluid, can be stored in the refrigerator 0 ℃ ~ 4 ℃ for 1 month.
5 instruments and equipment
5.1 Gas Chromatography - Mass Spectrometer, with electron bombardment source.
5.2 Analysis of balance. 0.0001 g and 0.01 g.
5.3 Crusher.
5.4 Centrifuge..2000 r/min.
5.5 Scroll Mixer.
5.6 blowing nitrogen enrichment instrument.
5.7 incubator.
5.8 Polypropylene centrifuge tube. 15 mL, with plug.
6 Preparation and storage of samples
6.1 Preparation of the sample
Replace the sample of about 500 g, the sampling site according to GB 2763 Appendix A implementation, (not available washing) chopped, with a crusher will sample
The product is processed into a slurry, mixed, packed into a clean container, sealed and marked.
6.2 Sample storage
Samples stored at -5 ° C in the dark. During sample preparation, the sample should be protected from contamination or changes in the residue content.
7 Analysis steps
7.1 Extraction
Weigh 1 g (accurate to 0.01 g) of the prepared homogeneous sample in a 15 mL centrifuge tube, add 3 g of anhydrous sodium sulfate and 5 mL of dichloromethane,
Mix thoroughly for 3 min on a vortex mixer and centrifuge at 2 000 r/min for 5 min. Transfer the dichloromethane to another 15 mL centrifuge tube,
With 5 mL of methylene chloride repeated extraction time, combined extract, 50 ℃ nitrogen blowing concentrated to near dry.
7.2 Derivatization
After drying in nitrogen, add 0.4 mL of acetonitrile to the centrifuge tube and add 100 μL of MTBSTFA, sealed at 80 ° C
Derived 1 h. Standard working fluid also added 100 μL MTBSTFA, sealed, under the above conditions for derivatization. After derivatization
0.22 μm microporous membrane was determined by gas chromatography-mass spectrometry.
7.3 Determination
7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions
A) Column. HP-5MS quartz capillary column. 30 m × 0.25 mm (inner diameter) × 0.25 μm film thickness, or equivalent.
B) Column temperature. 100 ° C (1 min) 30 ° C/min 180 ° C (1 min) 50 ° C/min 205 ° C 10 ° C/min 260 ° C (20 min).
C) Inlet temperature. 210 ° C.
D) Transmission line temperature. 250 ° C.
E) Carrier gas. helium, purity 99.999%, flow rate 1.0 mL/min.
F) Injection volume. 1 μL.
G) Injection method. no split injection, 1 min, open the diverter valve, split ratio of 20. 1.
H) ionization mode. EI.
I) Ionization energy. 70 eV.
J) Measurement method. Select the ion monitoring mode (SIM).
K) monitoring of ions. m/z 255,209,239,179, quantitative ion m/z 255.
L) solvent delay. 5 min.
7.3.2 Determination and confirmation of chromatography
According to the content of 4,6-dinitro-o-cresol in the sample, the standard working solution with similar concentration of sample peak area was selected. Derivatized
The response values of the 4,6-dinitro-o-cresol derivative in the standard working solution and the sample should be within the linear range of the instrument. Derivative
After the standard working solution and sample volume to participate in the measurement. The retention time of the 4,6-dinitro-o-cresol derivative under the above chromatographic conditions
About 9.31 min. Under the same experimental conditions, the chromatographic retention time of the test substance in the sample was the same as that of the standard working solution and after subtracting the background
Of the selected ions in the sample mass chromatogram, the abundance of the selected ions is compared to the abundance ratio of the corresponding ions of the standard,
Within the allowable range (see Table 1) allows you to determine the corresponding sample in the sample. Standard SIM chromatograms and full scan spectra
See Appendix A, Figure A.1, Figure A.2.
Table 1 Maximum allowable error for relative ion abundance using gas chromatography-mass spectrometry
7.4 blank experiment
In addition to the sample, according to the above determination steps.
8 results are calculated and expressed
The content of 4,6-dinitro-o-cresol in the sample was calculated according to the following formula (1)
MΑs
VCsA
.. (1)
Where.
The content of 4,6-dinitro-o-cresol in the X-sample, in milligrams per kilogram, mg/kg;
The peak area of 4,6 - dinitro - o - cresol derivative in A -
AS - standard working solution 4,6 - dinitro - o - cresol derivative peak area;
Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10%
Allowable relative deviation ± 20% ± 25% ± 30% ± 50%
C - Concentration of 4,6 - dinitro - o - cresol in standard working solution in milligrams per liter, mg/L;
M - the final sample quality of the sample, in grams, g;
V - the final volume of the sample solution, in milliliters, mL.
Note. The result of the calculation shall be deducted from the blank value. The result of the measurement shall be expressed as the arithmetic mean of the parallel measurement, and two valid digits shall be retained.
9 precision
9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix B requirements.
9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix C requirements.
10% limit and recovery rate
10.1 Quantitation limits
The quantitation limit of this method 4, 6-dinitro-o-cresol is 0.01 mg/kg.
10.2 Recovery rate
The recoveries of 4, 6 - dinitro - o - cresol were between 74.0% and 105.0% at the concentration of 0.01 mg/kg.
The recoveries of 4, 6 - dinitro - o - cresol were between 72.0% and 101.0% at the concentration of 0.05 mg/kg.
The recoveries of 4, 6 - dinitro - o - cresol were between 81.1% and 105.0% at the concentration of 0.10 mg/kg.
Appendix A
(Informative)
4, 6-dinitro-o-cresol standard-MTBSTFA derivative gas chromatography-mass spectrometry
Figure A.2 SIM spectra of 4, 6-dinitro-o-cresol-MTBSTFA derivatives
Figure A.1 SIM chromatogram of 0.5 mg/L 4,6-dinitro-o-cresol-MTBSTFA derivative
Appendix B
(Normative appendix)
Laboratory repeatability requirements
Table B.1 Laboratory repeatability requirements
Measured component content
Mg/kg
Precision
0.001 36
> 0.01
> 1 14
Appendix C
(Normative appendix)
Inter-laboratory reproducibility requirements
Table C.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
Precision
0.001 54
> 0.01
> 1 19
|