GB 23200.100-2016 English PDF

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GB 23200.100-2016: Food safety national standard -- Determination of permethrin residues in royal jelly -- Gas chromatography
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 23200.100-2016	219	Add to Cart	3 days	Food safety national standard -- Determination of permethrin residues in royal jelly -- Gas chromatography	Valid

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Basic data

Standard ID: GB 23200.100-2016 (GB23200.100-2016)
Description (Translated English): Food safety national standard -- Determination of permethrin residues in royal jelly -- Gas chromatography
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 11,183
Date of Issue: 2016-12-18
Date of Implementation: 2017-06-18
Older Standard (superseded by this standard): SN/T 2575-2010
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 23200.100-2016: Food safety national standard -- Determination of permethrin residues in royal jelly -- Gas chromatography

---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 permethrin residues in royal jelly by gas chromatography National Standards of People's Republic of China GB Replace SN/T 2575-2010 National standards for food safety Determination of Pyrethroid Pesticide Residues in Royal Jelly Gas chromatography National food safety standards- Determination of multiple pyrethroid pesticides residues in royal-jelly 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 2575-2010 "Import and export royal jelly in a variety of pyrele pesticide residues detection method." Compared with SN/T 2575-2010, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - standard name "import and export royal jelly" to "royal jelly"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 2575-2010. National standards for food safety Determination of permethrin residues in royal jelly by gas chromatography

1 Scope

This standard specifies the royal jelly in the bifenthrin, fenpropathrin, cyhalothrin, permethrin, cypermethrin, cypermethrin, Determination of Pesticide Residues of Fenpropathrin, Fenvalerate and Deltamethrin by Gas Chromatography. This standard applies to royal jelly in the buprofeix, fenpropathrin, cyhalothrin, permethrin, cypermethrin, cypermethrin, Fenvalerate, fenvalerate, deltamethrin pesticide residues determination, 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

The pyrethroid pesticide residues in the sample were extracted with a mixture of n-hexane acetone (1 1, V/V) and purified by a Florisil solid phase extraction column Purification, gas chromatography - electron capture tester, 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 ether (C4H10O). pure chromatography. 4.1.2 n-hexane (C6H14). pure chromatography. 4.1.3 Acetone (C3H6O). Chromatographic pure. 4.1.4 Sodium chloride (NaCl). 4.1.5 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve. 4.2 standards 4.2.1 Bifenthrin, fenpropathrin, cyhalothrin, permethrin, cypermethrin, cypermethrin, fenpropathrin, fenvalerate, Deltamethrin standard substance. purity ≥99%, see Appendix A. 4.3 standard solution preparation 4.3.1 Bifenthrin, fenpropathrin, cyhalothrin, permethrin, cypermethrin, cypermethrin, fenpropathrin, Pyrethrin, deltamethrin standard solution. accurately weighed the appropriate amount of standard material, with n-hexane dubbed the concentration of 100 g/mL standard stock solution. According to the need to use n-hexane diluted to the appropriate concentration of mixed standard working solution. Store in 4 ℃ refrigerator. 4.4 Materials 4.4.1 Florisil Solid Phase Extraction Column. (6 mL, 1 g) or equivalent. Use a 10 mm high anhydrous sodium sulphate layer in the front column 5 mL n-hexane elution activated solid phase extraction column.

5 instruments and equipment

5.1 Gas Chromatograph. Electron Capture Tester (ECD). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Vortex Mixer. 5.4 Centrifuge. speed greater than 5 000 r/min. 5.5 nitrogen blowing instrument. 5.6 Rotary evaporator.

6 Preparation and storage of samples

Take about 500g of the sample, the sampling site according to GB 2763 Appendix A implementation, will be forced to stir evenly, into the clean container Seal, and mark the mark. Save below -18 ° C. During the operation of the sample preparation, the contamination of the sample or the change in the content of the residue should be prevented.

7 Analysis steps

7.1 Extraction Weigh 2 g sample (accurate to 0.01 g) in 50 mL centrifuge tube, add 10 mL water vortex mixed 1 min, standing 5 min. Add 20 ML n-hexane acetone (1 1, volume ratio) mixed solvent, vortex mixed for 1 min, centrifuged at 4000 r/min for 3 min, the upper organic phase Transferred into the concentrated bottle. Add 10 mL of n-hexane acetone (1 1, volume ratio v/v) mixed solvent, repeated extraction time, Combined with the upper organic phase, below 45 ℃ in the water bath under reduced pressure to near dry, to be purified. 7.2 Purification The residue in the concentrated flask was washed twice with 3 mL of n-hexane and transferred to a Florisil solid phase extraction column. With 5 mL of n-hexane The eluate was discarded and eluted with 10 mL of n-hexane + diethyl ether (9 + 1, v/v) mixed solvent. The eluate was collected in 10 mL of glass Centrifuge tube, in the 45 ℃ water bath with nitrogen blowing slowly blown to dry, with n-hexane dissolved and set to 0.5 mL, for gas chromatography. 7.3 Determination 7.3.1 Gas Chromatographic Reference Conditions A) Column. HP-50 quartz capillary column, 30 m x 0.32 mm (inner diameter) x 0.25 μm (film thickness), or equivalent; B) column temperature. 70 ℃ for 1 min, at 20 ℃/min heating rate rose to 270 ℃, keep 1 min, at 2 ℃ / Min heating rate rose to 280 ℃, keep 10 min; C) Inlet temperature. 270 ° C; D) Tester temperature. 325 ° C; E) Carrier gas. nitrogen, purity 99.999%, flow rate 2.0 mL/min, tail blow 60 mL/min; F) Injection volume. 2 μL; G) Injection method. splitless injection, open valve time 0.75 min. 7.3.2 Chromatographic determination Depending on the amount of various pyrethrins in the sample solution, a standard working solution with similar levels is selected. Standard working solution and sample in a variety of pyrethroids Should be within the linear range of the instrument. Standard working solution and sample volume and other volume interspersed injection determination. Under the above chromatographic conditions The retention time of bifenthrin was about 12.9 min; the retention time of fenpropathrin was about 13.6 min; the retention time of cyhalothrin was About 14.0 min; the retention time of the isomers of permethrin was about 16.0, 16.2 min; the retention time of the cyfluthrin was about 16.6 Min, 16.7 min, 16.9 min; the retention time of cypermethrin is about 17.5 min, 17.6 min, 17.8 min; The retention time of the isomers of cypermethrin was about 18.6 min and 18.8 min. The retention time of the fenvalerate was about 19.9 min, 20.5 min; deltamethrin retention time is about 23.0 min. The chromatogram of the standard is shown in Appendix B, Figure B.1. 7.4 blank test In addition to the sample, according to the above determination steps.

8 results are calculated and expressed

Use the chromatographic data processing software or calculate the residual content of various pyrethrins in the sample according to formula (1) Ai × Ci × V X = ---------------------- (1) ASi × m Where. X - the number of permethrin residues in the sample in milligrams per kilogram (mg/kg); The sum of the peaks of the isomers in the sample solution (the isomers of isomers are calculated). Ci  Concentration of various pyrethroids in standard working fluid in micrograms/ml (g/mL); V - Final volume of the final volume in milliliters (mL); ASi - the area of various pyrethroids in the standard working fluid (the isomers of isomers have to calculate the peak area of the isomers); 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.

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 D 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 E requirements. 10% limit and recovery rate 10.1 Quantitation limits The quantification limit of this method is. 0.01 mg/kg. 10.2 Recovery rate The experimental data on the concentration and recovery of the sample are given in Appendix C.

Appendix A

(Informative) 9 kinds of pyrethroid pesticides in English common name, chemical formula, CAS No. information Table A.1 9 kinds of pyrethroid pesticides in English common name, chemical formula, CAS No. information Chinese generic name English generic name chemical formula CAS number Bifenthrin C23H22ClF3O2 82657-04-3 Fenpropathrin C22H23NO3 39515-41-8 Enriched cyhalothrin Lambda-Cyhalothrin C23H19ClF3NO3 91465-08-6 Permethrin C21H20Cl2O3 52645-53-1 Cyfluthrin C22H18Cl2FNO3 68359-37-5 Cypermethrin C22H19Cl2NO3 97955-44-7 Fenpropathrin tau-fluvalerate C26H22ClF3N2O3 69409-94-5 Fenvalerate C25H22ClNO3 51630-58-1 Deltamethrin C22H19Br2NO3 52918-63-5

Appendix B

(Informative) Chromatogram of standard substance Figure B.1 Chromatogram of 9 Pyrethroid Pesticide Standards 1. Bifenthrin 2. Fenpropathrin 3. Highly effective cyhalothrin 4. Permethrin I 5. Permethrin II 6. Cyfluthrin I 7. Cyfluthrin Ⅱ 8. Cyfluthrin III 9. Cypermethrin Ⅰ 10. Cypermethrin II Cypermethrin III 12. Fenpropathrin I 13. Fenpropathrin II 14. Fenvalerate I 15. Fenvalerate II 16 deltamethrin

Appendix C

(Informative) Sample concentration and recovery of the experimental data Table C.1 Experimental data on the concentration and recovery of the sample Pesticide name Add concentration (mg/kg) Recovery rate range% Precision range Pesticide name Add concentration (mg/kg) Recovery rate range% Precision range% Bifenthrin 0.01 76.0 to 91.0 10.6 Cypermethrin 0.01 77.2 to 109 9.6 0.02 70.0 to 97.5 8.7 0.02 77.5 to 110 8.4 0.05 77.8 ~ 103 8.1 0.05 73.6 ~ 106 12.3 Fenpropathrin 0.01 78.4 to 101 11.6 Fenpropathrin 0.01 72.4 to 99.8 7.4 0.02 79.5 to 107 10.8 0.02 77.5 to 109 6.9 0..05 80.4 to 109 7.2 0.05 73.0 to 106 11.3 Cyhalothrin 0.01 78.8 to 108 13.4 fenvalerate 0.01 71.5 to 104 8.2 0.02 78.0 to 104 8.9 0.02 78.5 to 106 9.6 0.05 77.6 to 104 7.6 0.05 76.8 to 103 7.2 Permethrin 0.01 78.3 ~ 97.4 12.1 Deltamethrin 0.01 72.4 ~ 110 11.6 0.02 80.8 ~ 13.2 0.02 77.5 to 112 10.0 0.05 76.4 ~ 9.5 0.05 78.8 to 108 8.9 Cyfluthrin 0.01 71.3 ~ 14.0 0.02 78.5 ~ 13.1 0.05 73.2 ~ 8.9

Appendix D

(Normative appendix) Laboratory repeatability requirements Table D.1 Laboratory repeatability requirements Measured component content Mg/kg Precision 0.001 36 > 0.01 > 1 14

Appendix E

(Normative appendix) Inter-laboratory reproducibility requirements Table E.1 Inter-laboratory reproducibility requirements Measured component content Mg/kg Precision 0.001 54 > 0.01 > 1 19 ......

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