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Food safety national standard -- Detection method of fenpropathrin residues in bee products
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GB 23200.95-2016
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Basic data | Standard ID | GB 23200.95-2016 (GB23200.95-2016) | | Description (Translated English) | Food safety national standard -- Detection method of fenpropathrin residues in bee products | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 9,927 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN 0691-1997 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.95-2016: Food safety national standard -- Detection method of fenpropathrin residues in bee products ---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 fenpropathrin residues in bee products
ICS
National Standards of People's Republic of China
GB
Instead of SN 0691-1997
National standards for food safety
Detection method of fenpropathrin residues in bee products
Nationalfood safety standards-
Determination of tau-fluvalinate residue in bees'products
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 0691-1997 "Method for the determination of fenpropathrin residues in export bee products".
This standard compared with SN 0691-1997, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the standard name "export bee products" to "bee products";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN 0691-1997.
National standards for food safety
Detection method of fenpropathrin residues in bee products
1 Scope
This standard specifies the sampling, sample preparation and gas chromatographic method for the determination of fenpropathrin residues in export bee products.
This standard applies to the export of honey in the residual determination of fenpropathrin residues, 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
After the sample was alkalized, it was extracted with n-hexane-acetone, and the extract was purified by liquid-liquid partitioning with acetonitrile and n-hexane.
Into the acetonitrile layer. Acetonitrile extract and then evaporated to dry, with n-hexane dissolved residue, solution for gas chromatography determination, 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 Acetone (C3H6O). Distillation.
4.1.2 Sodium hydroxide (NaOH) aqueous solution. 2 m ol/L.
4.1.3 N-Hexane (C6H14). Distillation.
4.1.4 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, stored in a sealed container for use.
4.2 solution preparation
4.2.1 N-Hexane. Saturated with acetonitrile.
4.2.2 acetonitrile. saturated with n-hexane.
4.3 standards
Fenvalerate standards. purity ≥ 97%.
4.4 standard solution preparation
Accurately weigh the appropriate amount of fenpropathrin standards, with n-hexane dubbed the concentration of 20 μg/mL standard stock solution, and then need to use
N-Hexane is formulated into a standard working solution at an appropriate concentration. Store in 4 ℃ refrigerator.
5 instruments and equipment
5.1 Gas chromatograph with electronic capture detector.
5.2 Analysis of balance. 0.01g and 0.0001g.
5.3 Rotary Evaporator.
5.4 Oscillator.
6 Sample preparation and storage
6.1 Preparation of the sample
The samples will be thoroughly stirred, divided into two, into the sample bottle as a sample, sealed, marked mark. Such as retrieving samples in a knot
When the crystal is precipitated, the vial is capped and placed in a water bath which does not exceed 40 ° C. To be all melted after crystallization, open cover, stir well,
Are divided into two, sealed, and marked with the mark.
In the case of a cup of honey, all the cups of honey will be retrieved, poured together, fully stir well, and take out about 1 kg to represent the sample. And then 1 kg on behalf of the equipment
After the samples were mixed, they were divided into two portions and placed in a sample bottle as a sample. Sealed, marked.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
6.2 Sample storage
Store the sample at room temperature.
Note. During sampling and sample preparation, it is necessary to prevent contamination of the sample or change in the content of the residue.
7 Analysis steps
7.1 Extraction
Weigh about 20 g of sample (accurate to 0.1 g), add 20 mL of sodium hydroxide solution (2 mol/L) to a 125 mL stoppered flask,
Oscillation causes the sample to dissolve. Pour into a 100 mL separatory funnel, add 20 mL of n-hexane and 10 mL of acetone, shake for 5 min, standing stratified. will
The n-hexane layer was filtered into.200 mL of pear-shaped bottles and 20 mL of n-hexane and 10 mL of acetone were added to the residual night and shaken for 5 min.
Operation once. The n-hexane layer was combined with the pear-shaped flask and evaporated to 40 ° C and evaporated to dryness.
7.2 Purification
The pear-shaped bottle was rinsed with 30 mL of acetonitrile saturated n-hexane and 30 mL of n-hexane saturated acetonitrile and the residue was dissolved. The solution was transferred to 100 mL of the solution
Funnel, intense oscillation 5 min, static stratification. Separate the acetonitrile layer into a.200 mL separatory funnel. Add 2 x 30 mL to n-hexane
Hexane-saturated acetonitrile, repeat the above procedure. Consolidate the acetonitrile layer in the appendix to the separatory funnel. Add 50 mL of acetone to the separatory funnel
And n-hexane, intense oscillation 5 min, standing stratification. The acetonitrile layer was taken in a.200 mL pear-shaped flask and evaporated at 40 ° C or below
To just dry. The residue was dissolved in 5.0 mL of n-hexane and the solution was subjected to gas chromatography.
7.3 Determination
7.3.1 Chromatographic reference conditions
A) Column. quartz capillary column, SE-54, 25 m x 0.53 mm (inner diameter), 1.0 μm (film thickness), or equivalent;
B) Carrier gas. nitrogen (purity ≥99.99%), 5.7 mL/min;
C) Auxiliary gas. nitrogen, 60 mL/min;
D) Column temperature. 220 ° C;
E) Inlet temperature. 250 ° C;
F) detector temperature. 300 ° C;
G) Injection volume. 1 μL 220 ° C;
H) Injection method. no shunt, 0.75 min after the valve.
7.3.2 Chromatographic determination
According to the sample solution was measured in the case of fenvalerate, selected peak height similar to the standard working solution. Standard working solution and fluoramine in sample solution
The cypermethrin response value 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-mentioned chromatographic bar
, The retention time of fenpropathrin was about 6.6 min, and the standard chromatogram was shown in Figure A1 in Appendix A.
7.4 blank test
In addition to the sample, according to the above steps.
8 results are calculated and expressed
Use the chromatographic data processor or (1) to calculate the residual content of fenpropathrin in the sample.
(1)
Where. X - the content of fenpropathrin residues in the sample;
H - peak height of fenpropathrin in the sample solution, mm;
Hs - standard work solution in the peak of fenpropathrin, mm;
C - concentration of fenpropathrin in standard working solution, μg/mL;
V - the final volume of the sample solution, mL;
M - the amount of sample represented by the final sample, g.
Note. The result of the calculation is deducted from the blank value. The result of the measurement is expressed by the arithmetic mean of the parallel measurement, and the two valid digits are retained.
9 precision
9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the
Record 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 the
Record C requirements.
10% limit and recovery rate
10.1 Quantitation limits
The quantification limit of this method is 0.02 mg/kg.
10.2 Recovery rate
The experimental data of the concentration of fenpropathrin in honey and its recovery rate.
At 0.02 mg/kg, the recovery was 93.1%.
At 0.10 mg/kg, the recovery rate was 98.3%.
At 1.0 mg/kg, the recovery was 90.8%.
Appendix A
(Suggested appendix)
Standard chromatogram
Figure A1 Gas chromatogram of fluorosaline standard
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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