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GB 23200.95-2016 English PDF

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GB 23200.95-2016: Food safety national standard -- Detection method of fenpropathrin residues in bee products
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PDF similar to GB 23200.95-2016


Standard similar to 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Older Standard (superseded by this standard) SN 0691-1997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


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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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