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GB 23200.43-2016: Food safety national standard -- Determination of residual chloroquine phosphate in grain and oilseeds -- Gas chromatographic method
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Food safety national standard -- Determination of residual chloroquine phosphate in grain and oilseeds -- Gas chromatographic method
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GB 23200.43-2016
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Basic data | Standard ID | GB 23200.43-2016 (GB23200.43-2016) | | Description (Translated English) | Food safety national standard -- Determination of residual chloroquine phosphate in grain and oilseeds -- Gas chromatographic method | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 10,118 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 1017.5-2002 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No.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 23200.43-2016: Food safety national standard -- Determination of residual chloroquine phosphate in grain and oilseeds -- Gas chromatographic method
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Food safety national standard - Determination of residual chloroquine phosphate in grain and oilseeds - Gas chromatographic method
National Standards of People's Republic of China
GB
Instead of SN/T 1017.5-2002
National standards for food safety
Determination of Quercetin Residues in Grains and Oilseeds
Gas chromatography
National food safety standards-
Determination of quinclorac residue in cereals and oil seeds
Gas chromatography
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 1017.5-2002 "Test method for the presence of quinclorac residues in grain and oilseeds".
Compared with SN/T 1017.5-2002, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the name "export grain and oilseed" in the standard name is replaced by "grain and oilseed";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 1017.5-2002.
National standards for food safety
Determination of quercetin acid residues in grain and oilseeds - Gas chromatographic method
1 Scope
This standard specifies the method for the determination of quinclorac residues in grain and oilseeds by gas chromatography.
This standard applies to brown rice, soybeans, corn, wheat, the determination of residual chlorine quinolines, 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
file. 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
The sample was extracted with acetone, evaporated to dryness and dissolved in water. The methylene chloride was extracted with methylene chloride and purified by methyl ester
Purification, gas chromatography, external standard method quantitative.
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 Acetone (C3H6O). Chromatographic pure.
4.1.2 Sodium bicarbonate (NaHCO3). Chromatographic purity.
4.1.3 Sodium hydroxide (NaOH).
4.1.4 dichloromethane (CH2Cl2). chromatographic purity.
4.1.5 Sulfuric acid (H2SO4).
4.1.6 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, set the dryer in the spare.
4.1.7 petroleum ether.
4.1.8 ether (C4H10O). re-distillation.
4.1.9 Potassium hydroxide (KOH).
4.2 solution preparation
4.2.1 sulfuric acid solution. 3 mol/L.
4.2.2 Sodium hydroxide solution. 1 mol/L.
4.2.3 Potassium hydroxide solution. 10 mol/L.
4.2.4 Diazomethane. Set 4 mL of ether and 2 mL of potassium hydroxide solution in the reaction tube, add 5 mL of ether dissolved 2 g N-methyl
-N-nitroso-4-toluenesulfonic acid amine solution, blowing nitrogen for 5 min, collecting the ether solution in the reaction tube.
4.3 standards
4.3.1 Quinclorac acid standard. purity ≥ 99%.
4.4 standard solution preparation
4.4.1 Quinclorac acid standard stock solution. accurately weighed the right amount of quinolinic acid standard, with a small amount of acetone dissolved, and petroleum ether
Prepared as standard stock solution of 1 000 μg/mL, stored at 0 ℃ ~ 4 ℃.
4.4.2 Quinclorac Acid Standard working solution. According to the work need to use petroleum ether diluted to the appropriate concentration of standard working solution.
4.5 Materials
4.5.1 Magnesium silicate solid phase extraction column. 6 mL/1 g, or equivalent.
5 instruments and equipment
5.1 Gas chromatograph, with electron capture detector.
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 Oscillator.
5.4 Rotary Evaporator.
5.5 separatory funnel.
5.6 Solid phase extraction unit with vacuum pump.
6 Preparation and storage of samples
6.1 Preparation of the sample
Take a representative sample 500 g, the sampling site according to GB 2763 Appendix A implementation, crushed with a pulverizer. Mix, are divided into two as a test
Type, into a clean sample container, sealed and marked.
6.2 Sample storage
The sample was stored at -5 ° C.
During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue.
7 Analysis steps
7.1 Extraction
Weigh 20 g (accurate to 0.01 g) sample in 250 mL stoppered conical flask, add 100 mL of acetone and shake for 30 min.
The filtrate was filtered into a 250 mL heart flask and the residue was washed twice with 50 mL of acetone. The washings were filtered and combined in the above-
40 ℃ water bath evaporated to near dry, add 10 mL of water and 5 g sodium bicarbonate. After dissolving, add about 2 mL of sodium hydroxide solution, adjust the pH
The value is 9 ± 0.2. Mixed thoroughly and moved into a separatory funnel, washed twice with 20 mL of water, and the solution was combined in a separatory funnel.
Add 100 mL of methylene chloride to the above-mentioned separatory funnel, shake for 5 min, allow to separate the layers, discard the lower organic phase, and then use 2 x 50 mL
Dichloromethane repeatedly washed the water phase twice. About 5 mL of sulfuric acid solution was added to the aqueous phase to give a pH of 2 ± 0.2. Add 100 mL of dichloromethane
And the mixture was allowed to stand for 5 min. The lower organic phase was separated from the Erlenmeyer flask and the aqueous phase was repeatedly extracted with 2 x 50 mL of dichloromethane
Twice, combined with organic phase. Dehydrated by anhydrous sodium sulfate, placed in a heart-shaped bottle, in 40 ℃ water bath spin concentrated to near dry, adding 2
ML of acetone to dissolve the residue.
7.2 Derivatization
5 mL of diazomethane solution was added to the above acetone solution and sealed. The reaction was carried out in a water bath at 60 ° C for 10 min. The solvent was evaporated,
Petroleum ether dissolved.
7.3 purification
The magnesium silicate solid phase extraction column was installed on the solid phase extraction device, first with 6 mL of petroleum ether pre-leaching, discarded. The solution (7.2) was poured into
To the solid phase extraction column, after all the outflow, and then 10 mL of petroleum ether in two separate solid phase extraction column, discarded. With 10 mL of acetone - stone
Oil ether (9 1) to maintain the flow rate of 1.5 mL/min, collecting all the effluent, 45 ℃ nitrogen flow to near dry. Dissolved with petroleum ether
And moved into a volumetric flask to a volume of 1.0 mL, measured by a gas chromatograph.
7.4 Derivatives of reference materials
Accurate removal of the appropriate concentration of quinacquine acid standard working solution in a heart-shaped bottle, in 40 ℃ water bath rotation concentrated to near dry, plus
Into 2 mL of acetone to dissolve the residue, the following according to 7.2 operation.
7.5 Determination
7.5.1 Gas Chromatographic Reference Conditions
A) Column. BP10 quartz capillary column, 30 m 0.25 mm (id), film thickness 0.25 m, or equivalent.
B) Column temperature. 240 ° C
C) Inlet temperature. 280 ° C.
D) Detector temperature. 290 ° C.
E) Carrier gas. nitrogen, purity greater than or equal to 99.995%, 10 mL/min.
F) Injection volume. 1 μL.
G) Tail gas. nitrogen, purity greater than or equal to 99.995%, 50 mL/min.
7.5.2 Chromatographic determination
According to the content of pesticide in the sample solution, the standard working solution with similar concentration is selected. Standard working solution and methyl in the sample solution to be tested
The response value of the pesticide should be within the linear range of the instrument detection. The standard working solution and sample solution were measured by volume injection. In the above
Under the conditions of chromatography, the retention time of methyl quinclorac is about 3 min. The chromatogram of the standard is shown in Appendix A, Appendix A.1.
7.6 blank experiment
In addition to the sample, according to the above determination steps.
8 results are calculated and expressed
Use the chromatographic data processor or calculate the amount of quinclorac pesticide in the sample according to the following formula (1).
Mh
Vch
S
.. (1)
Where.
X - Residual content of quinclorac in the sample, in milligrams per kilogram, mg/kg;
H - chromatographic peak of palmatic acid methyl ester in sample solution, mm;
Hs - the standard working solution of dichloroquinolate methyl ester peak height, mm;
C - concentration of quinclorac in standard working solution, g/mL;
V - the final volume of the standard volume, mL;
M - the amount of sample represented by the final sample, 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.
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 C 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 D requirements.
10% limit and recovery rate
10.1 Quantitation limits
The quantification limit of the method for quinclorac is 0.05 mg/kg.
10.2 Recovery rate
When the levels were 0.05 mg/kg, 0.5 mg/kg, 1.0 mg/kg, the recovery rates of the addition of quinclorac are shown in Appendix B.
Appendix A
(Informative)
Chromoquinoline methyl ester standard chromatogram
Table A.1 Gas chromatograms of methyl quinolinic acid methyl ester standards
Appendix B
(Informative)
Sample concentration and recovery of the experimental data
Table B.1 Experimental data on the concentration and recovery of the sample
sample name
Add concentration (mg/kg)
0.05 0.50 1.00
Brown rice 89.2% 87.9% 82.9%
Corn 92.7% 91.3% 92.2%
Wheat 88.2% 92.7% 88.2%
Soybean 82.6% 83.1% 80.9%
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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