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GB 23200.25-2016: Food safety national standard -- Determination of Herbicide Residue in Fruits
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Food safety national standard -- Determination of Herbicide Residue in Fruits
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GB 23200.25-2016
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Basic data | Standard ID | GB 23200.25-2016 (GB23200.25-2016) | | Description (Translated English) | Food safety national standard -- Determination of Herbicide Residue in Fruits | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 10,116 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 1115-2002 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.25-2016: Food safety national standard -- Determination of Herbicide Residue in Fruits---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 Herbicide Residue in Fruits
National standards for food safety
Determination of Herbicide Residue in Fruits
National food safety standards-
Determination of oxadiazon residue in fruits
GB
National Standards of People's Republic of China
Instead of SN/T 1115-2002
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 1115-2002 "Method for the determination of oxadiazone residues in fruit and vegetable".
This standard and SN/T 1115-2002, 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 1115-2002.
National standards for food safety
Determination of Herbicide Residue in Fruits
1 Scope
This standard specifies the sampling, sample preparation and gas chromatography-mass spectrometry and confirmation of the test of oxytetracycline residues in fruit
law.
This standard applies to citrus, apple maltitol residues in the test, other food can refer to the implementation.
2 normative reference documents
The following documents are indispensable for the application of this document. Note the date of the reference file, only the date of the date
Apply to this document. 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 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.
3.1 Reagents
3.1.1 Benzene (C6H6). heavy distillation.
3.1.2 n-hexane (C6H14). re-distillation.
3.1.3 Sodium chloride (NaCl).
3.1.4 anhydrous sodium sulfate (Na2SO4). after 650 ℃ burning 4h, placed in the dryer in the spare.
3.2 solution preparation
3.2.1 benzene - n-hexane solution (1 1). take 100 mL of benzene, add 100 mL of n-hexane, shake back.
3.2.2 benzene - n-hexane solution (2 1). take.200 mL of benzene, add 100 mL of n-hexane, shake back.
3.3 standards
3.3.1 maloxione standard. purity ≥ 99%.
3.4 standard solution preparation
3.4.1 maloxione stock solution. accurately weighed appropriate amount of maloxone standard, with a small amount of n-hexane dissolved, and n-hexane preparation
Into a concentration of 1000 μg/mL standard stock solution. The standard stock solution is diluted to the appropriate concentration with n-hexane as needed
Quasi working fluid.
3.5 material
3.5.1 Activated carbon cartridge. SUPELCLEAN ENVI-CARB cartridge, 125 mg, 3 mL or equivalent.
4 instruments and equipment
4.1 Gas chromatograph with mass selective detector.
4.2 Analysis of balance. 0.01 g and 0.0001 g
4.3 solid phase extraction device with vacuum pump.
4.4 Centrifuge. 3000r/min.
4.5 Scroll Mixer.
4.6 centrifuge tube. 15mL.
4.7 scale tube. 15mL.
4.8 Micro-syringe. 10 μL.
5 Preparation and storage of samples
5.1 Preparation of the sample
Will be taken to take the original sample shrink 1kg, sampling site according to GB 2763 Appendix A, the organization of crusher mashed, are
Divided into two, into a clean container, as a sample. Sealed and marked with mark.
5.2 Sample storage
The sample was stored at -18 ° C or lower.
Note. During sampling and sample preparation, it is necessary to prevent contamination of the sample or change in the content of the residue.
6 Analysis steps
The oxytetracycline residue in the sample was extracted with benzene-n-hexane and then purified by activated charcoal column.
Determination and confirmation of the gas chromatograph of the detector, and the external standard method.
6.1 Extraction
Accurately weigh 2.0 g homogeneous sample (accurate to 0.001g) in a 15 mL centrifuge tube, add 1 g of sodium chloride, mix
And mixed with 2 mL of the benzene-n-hexane mixed solution on the mixer for 3 min at 2 500 r/min
After centrifugation for 2 min, the supernatant was transferred to another 15 mL graduated tube and the residue was washed with 2 mL of benzene-n-hexane
The solution was extracted twice, the combined extracts were added, and 1.0 g of anhydrous sodium sulfate was added to dryness.
6.2 purification
The active carbon pellet was loaded with solid phase extraction on a vacuum filtration device, and the column was pre-leached with 1 ml 3 benzene to keep the flow rate
0.5 mL/min. Remove the eluent. The sample extract was added to a column and washed with a 1.5 mL? 3 benzene-n-hexane mixed solution
The tubes were transferred to the pellet and the whole eluate was collected at 45 ° C. The air stream is blown to near and dissolved with n-hexane
The residue was set at 0.50 mL for CC/MSD analysis.
6.3 Determination
6.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions
A) Column. quartz capillary column HP-5,25 m0.2 mm (inner diameter), film thickness 0.33 μm, or equivalent;
B) column temperature. 100 ℃ for 1min, to 5 ℃/min rose to.200 ℃, and then 10 ℃/min, rose to
280 ℃, keep 5min;
C) Inlet temperature. 280 ° C;
D) chromatographic-mass spectrometer interface temperature. 250 ° C;
E) Carrier gas. nitrogen, purity ≥99,995%, 0.6 mL/min;
F) Injection volume. 1 μL;
G) Injection method. no split injection, 1min after the opening valve;
H) ionization mode. EI;
I) ionization energy. 70 ev;
J) Measurement method. Select the ion detection mode (SIM);
K) detection of ions (m/z). 177, 258, 344;
L) solvent delay. 20 min.
6.3.2 Chromatographic determination
According to the content of oxadiazone in the sample solution, the standard working solution with similar peak area is selected, the standard working solution and the sample solution are evil
The response value of the ketone should be within the linear range of the instrument detection, and the volume of the working fluid and the sample solution should be measured.
Under the above chromatographic conditions, the retention time of oxadiazone was about 25.95 min, and the standard SIM chromatogram and full scan mass spectrum were observed.
Appendix A, Figures A.1, A.2.
6.3.3 Confirmation of mass spectrometry
The standard solution and sample solution are determined according to the conditions specified in 6.3.2, if the sample solution with the standard solution of the same retention
Time peak appears, then its mass spectrometry confirmed. Under the above conditions of gas chromatography-mass spectrometry, the retention time of oxadiazone is about
For 25.95 min, monitoring of ionic strength ratio (m/z) 258. 177. 344- (65 ± 10). 100. (16 ± 2).
6.4 blank experiment
In addition to the sample, according to the above determination steps.
7 Results calculation and presentation
The content of oxadiazone in the formula is calculated using a chromatographic data processor or by the following formula (1)
VA
(1)
Where. X-sample content of oxadiazone in milligrams per kilogram (mg/kg);
The peak area of oxadiazone in A sample solution;
Cs - the concentration of oxadiazone in standard working fluid, in micrograms per milliliter (μg/mL);
As - standard working area of the peak area of oxadiazone;
V-sample liquid final volume, in milliliters (mL);
M - the amount of sample represented by the final sample, in grams (g);
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.
8 precision
8.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage)
Rate), shall comply with the requirements of Appendix C.
8.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage)
Rate), shall comply with the requirements of Appendix D.
9 Quantitation limit and recovery rate
9.1 Limit of limits
The quantification limit of this method was 0.010 mg/kg.
9.2 Recovery
When the levels were 0.01 mg/kg, 0.05 mg/kg, 0.5 mg/kg, the addition of oxadiazone in different substrates
Rate see Appendix B.
Appendix A
(Informative)
Maltose Standard Chromatography and Mass Spectrometry
Figure A A.1 hamstromycin standard SIM chromatogram
Figure A A.2 Vancomycin Standard SCAN Mass Spectrometry
Appendix B
(Informative)
The recovery of maloxione in different matrices
Table B.1 Recovery rates of oxadiazones in different matrices
unit.%
Name of pesticide
Sample matrix
Citrus apple
Oxadiazone 95.0-98.4 96.7-98.3
Appendix C
(Normative appendix)
Laboratory repeatability requirements
Table C.1 Laboratory repeatability requirements
Measured component content
Mg/kg
Precision
0.001 36
> 0.01
> 1 14
Appendix D
(Normative appendix)
Inter-laboratory reproducibility requirements
Table D.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
Precision
0.001 54
> 0.01
> 1 19
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