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GB 23200.42-2016: Food safety national standard -- Detection Method of Residual Fluoride in Grain
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Food safety national standard -- Detection Method of Residual Fluoride in Grain
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GB 23200.42-2016
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Basic data | Standard ID | GB 23200.42-2016 (GB23200.42-2016) | | Description (Translated English) | Food safety national standard -- Detection Method of Residual Fluoride in Grain | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 11,154 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 1017.9-2004 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No.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 23200.42-2016: Food safety national standard -- Detection Method of Residual Fluoride in Grain---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 - Detection Method of Residual Fluoride in Grain
National Standards of People's Republic of China
GB
Instead of SN/T 1017.9-2004
National standards for food safety
Detection Method of Residual Fluoride in Grain
National food safety standards-
Determination of haloxyfop residue in cereal
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 1017.9-2004 "Method for the determination of fluticillin residues in import and export grain".
This standard compared with SN/T 1017.9-2004, 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 grain" to "grain".
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 1017.9-2004.
National standards for food safety
Detection Method of Residual Fluoride in Grain
1 Scope
This standard specifies the sampling, sample preparation and gas chromatographic methods for the determination of flupirtine residues in grain.
This standard applies to the determination of vanillafen residues in rice, and other foods may be referred to the implementation.
2 normative reference documents
The following documents are indispensable for the application of this document. For dated references, only the date of the note applies
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 principle
Extraction of phosphoric acid and acetone fluoride in the sample of fluoride, the extract extracted with chloroform, and then through the liquid distribution purification. Then by five
Fluorobromotoluene was purified and purified by silica gel column. The method was quantitatively determined by gas chromatograph with electron capture detector.
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 Trichloromethane (CHCl3). Distillation.
4.1.2 anhydrous ether (C4H10O). re-distillation.
4.1.3 n-Hexane (C6H14). for pesticide residues analysis.
4.1.4 Acetone (C3H6O). re-distillation.
4.1.5 Dichloromethane (CH2Cl2). Distillation.
4.1.6 phosphoric acid (H3PO4).
4.1.7 Triethylamine (C6H15N).
4.1.8 Toluene (C7H8).
4.1.9 Hydrochloric acid (HCl).
4.1.10 anhydrous sodium sulfate (Na2SO4). anhydrous sodium sulfate at 650 ℃ for 4 hours, into the dryer standby.
4.2 solution preparation
4.2.1 Phosphate solution. 1 g of sodium hydroxide and 17 g of disodium hydrogen phosphate, dissolved in water and diluted to 500 mL.
4.2.2 Pentafluorobromotoluene (PFBBr) Derivative Reagent. 100 μL Pentafluorobromotoluene was dissolved in 4.9 mL of toluene.
4.3 standards
4.3.1 Fluprofen standard. content ≥ 99.5%.
4.4 standard solution preparation
4.4.1 Fenfloxacin standard solution. accurately weighed the appropriate amount of Fenfen Wo Ling standard, with methanol dubbed 0.1mg/mL of the stock solution, according to
Need to be diluted to the appropriate concentration of standard working fluid.
4.5 Materials
4.5.1 silica gel column. 3 mL, before use in the top of the column loaded 1c m high anhydrous sodium sulfate, and with two grams of methane-n-hexane (1585)
Solution 3 mL pre-leaching.
5 instruments and equipment
5.1 Gas Chromatograph with Electronic Capture Detector (ECD).
5.2 Quick Mixer.
5.3 Centrifuge. 4 000 r/min.
5.4 Multifunctional micro-chemical sample processor or other equivalent instruments.
5.5 with a plug centrifuge tube. 5 mL.
5.6 Centrifuge tube. 5 mL, 15 mL.
5.7 pointed mouth straw.
5.8 Trace Adjustable pipettes. 50 μL,.200 μL, 1 000 μL.
5.9 Microinjector. 10 μL.
5.10 Analysis of balance. 0.01 g and 0.0001 g
6 Preparation and storage of samples
6.1 Preparation of the sample
The samples were scaled to 1 kg by quarter, all ground and passed through a 40 mesh sieve, mixed, divided into two portions, packed in clean containers
Inside, sealed, marked mark. During sample and sample preparation, it is necessary to prevent contamination of the sample or the change in the content of the residue.
6.2 Sample storage
Keep the sample below 5 ° C in dark.
7 Analysis steps
7.1 Extraction and purification
Weigh 0.5g homogeneous sample (accurate to 0.001g) in 15mL small test tube, add 2mL phosphoric acid and 1ml acetone, in the mixer quickly mixed
2 min, centrifuge 5 min (3000 r/min), with a tip of the straw to the phosphate - acetone extract into another tube, and then repeat the extraction of a
Times the residue. Combined with phosphoric acid - acetone extract, add anhydrous sodium sulfate to saturation, with 3 × 2 mL of chloroform extraction, standing stratification, with
The flask was transferred to another tube by adding a 2 mL of aqueous phosphate solution and rapidly mixed in a mixer for 2 min.
Centrifuge 5min (3000 r/min), separate the water phase, and then 2 × 2mL phosphate solution extracted chloroform twice, the water phase, with 1
. 1 hydrochloric acid water phase PH value of less than 2.0, adding excess anhydrous sodium sulfate to saturation, and then with 3 × 2 mL of anhydrous ether extraction of water,
After the solution was allowed to stand, the anhydrous ether solution was transferred to a plug centrifuge tube by means of a pointed pipette in a multi-function micro-chemical sample processor or other
Equivalent to 50 ℃ on the instrument through the nitrogen dry.
7.2 Derived
To a plug centrifuge tube containing the residue (7.1), add 100 μL of pentafluorobromotoluene derivative and 2 μl of triethylamine,
In a multi-functional micro-chemical sample processor or other equivalent instrument at 90 ℃ for 1 hour, 50 ℃ with nitrogen blowing to near dry, add 1mL
Dichloromethane-n-hexane (15 85) solution to dissolve the residue. Take the appropriate amount of standard working fluid in the multifunctional micro chemical sample processor or its
He was equivalent to 50 ℃ on the instrument through the nitrogen dry, according to the same step child derived.
7.3 silica gel column purification
The derivative of 7.2 was transferred to a silica gel column using 3 x 1 m L of dichloromethane-n-hexane (15 85), washed with 3 mL =
Hexane (15.50) solution, discard the eluent and elute with 4 mL of methylene chloride and blown at 50 ° C
Near dry, add 1.0 m L n-hexane volume, gas chromatographic analysis.
7.4 determination
7.4.1 Chromatographic reference conditions
A) Column. HP-5 column, size. 30m × 0.32mm (inner diameter) × 0.25μm, or equivalent;
B) Column temperature. 100 ° C (1 min.) 30 ° C/min. 150 ° C (1 min.) 3 ° C/min.
C) Inlet temperature. 250 ° C;
D) Detector temperature. 280 ° C;
E) Carrier gas. nitrogen. purity ≥99.999%, flow rate 3 mL/min, tail gas 30mL/min. ;
F) Injection method. no split injection;
J) Injection volume. 1 μL.
7.4.2 Chromatographic determination
According to the content of fenfluramine in the sample solution, the standard working solution with similar peak height is selected. Standard working solution and sample solution derived from fluorine
The response value of pyridoxine should be within the linear range of the instrument. On the standard working solution and sample solution volume of the plug-in measurement, in the above chromatogram
Conditions, the derivative of fluprofen after the retention time of about 28 min.
7.5 blank test
In addition to the standard sample, according to the above measurement steps.
8 results are calculated and expressed
Use the chromatographic data processor or the formula (2) to calculate the residual value of fluprofen in the sample.
X =
Mh
Vch
(2)
In the formula. X - the content of fluphenazine in the sample, in milligrams per kilogram (mg/kg);
H - peak height of fluprofen in the sample solution in millimeters (mm);
Hs - peak height of fluprofen in standard working solution in millimeters (mm);
C - the concentration of fluphenazine in the standard working solution in micrograms per milliliter (μg/mL);
M - the amount of sample to be weighed in grams (g);
V - The final volume of the sample solution in microliters (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)
Together with the requirements of Appendix B.
9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage)
Together with the requirements of Appendix C.
10% limit and recovery rate
10.1 Quantitation limits
The limit of quantification of fluprofen was 0.02 mg/kg.
10.2 Recovery rate
When the concentration was 0.02 mg/kg ~ 1.0 mg/kg, the recovery was between 79% and 101%.
Appendix A
(Informative)
Fluoropitrazine standard derivatives Gas chromatograms
Min 0 5 10 15 20 25 30 35
Hz
ECD1 B, (HAX1129 \\ HAX11291.D)
.9
Lo
Fo
Td
Figure A.1 Gas chromatogram of standard derivatives of fluproparine
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
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