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GB 23200.106-2016 English PDF

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GB 23200.106-2016: Food safety national standard -- Determination of residual residues in meat and meat products -- Gas chromatographic method
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GB 23200.106-2016English199 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of residual residues in meat and meat products -- Gas chromatographic method Valid GB 23200.106-2016

PDF similar to GB 23200.106-2016


Standard similar to GB 23200.106-2016

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Basic data

Standard ID GB 23200.106-2016 (GB23200.106-2016)
Description (Translated English) Food safety national standard -- Determination of residual residues in meat and meat products -- Gas chromatographic method
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 10,195
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 0642-2011
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 23200.106-2016: Food safety national standard -- Determination of residual residues in meat and meat products -- Gas chromatographic method


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Food safety national standard - Determination of residues residues in meat and meat products - Gas chromatographic method ICS National Standards of People's Republic of China GB GB/T 23200.106-2016 Instead of SN/T 0642-2011 National standards for food safety Determination of Residual Residue in Meat and Meat Products Gas chromatography National food safety standards- Determination of propoxur residue in meat and meat products 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 GB/T 23200.106-2016

Foreword

This standard replaces SN/T 0642-2011 "Method for the determination of residues in residues of meat and meat products by gas chromatography". Compared with SN/T 0642-2011, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name of the "export of meat and meat products" to "meat and meat products"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 0642-2011. GB/T 23200.106-2016 National standards for food safety Determination of residual residues in meat and meat products - Gas chromatographic method

1 Scope

This standard specifies the method for the determination of the residues of residues in meat and meat products by gas chromatography. This standard applies to the detection of residual residues in pork, chicken and beef, and other foods may be prescribed.

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 2763-2014 National Standard for Food Safety - Maximum Residue Limits for Pesticides in Foodstuffs GB/T 6682 Analytical laboratory water specifications and test methods

3 principle

The samples were extracted with cyclohexane-ethyl acetate (1 + 1, volume ratio). The extract was purified by gel permeation chromatography, Determination by gas chromatography, external standard method quantitative.

4 reagents and materials

Unless otherwise specified, the reagents used are analytically pure and water is the primary water specified in GB/T 6682. 4.1 Reagents 4.1.1 Cyclohexane (C6H12). Chromatographic Purification. 4.1.2 Ethyl acetate (C4H8O2). Chromatographic purity. 4.1.3 n-hexane (C6H14). chromatographic purity. 4.1.4 Toluene (C7H8). Chromatographic pure. 4.1.5 anhydrous sodium sulfate (Na2SO4). before burning at 650 ℃ for 4 h, stored in a dryer, cooling and standby. 4.2 reagent preparation 4.2.1 Cyclohexane-ethyl acetate mixed solvent (1 +1, volume ratio). take 100mL cyclohexane, add 100mL ethyl acetate, shake spare. 4.3 standards 4.3.1 Propoxur; C11H15NO3; CAS No.114-26-1). purity ≥99%. 4.4 standard solution preparation 4.4.1 Residue Granville standard reserve solution. accurately weighed the amount of the standard material (accurate to 0.1 mg), with toluene concentration of 1.0 mg/mL of standard stock solution. Store in 4 ℃ refrigerator. 4.4.2 Propoxurized standard working solution. According to the testing requirements, respectively, the above standard stock solution with n-hexane diluted to the appropriate concentration of the standard Quasi-working solution. Store in 4 ℃ refrigerator. 4.5 Materials 4.5.1 Filtration. 0.45 μm, organic. 4.5.2 anhydrous sodium sulfate column. in the cylindrical funnel (diameter 1.5 cm), containing about 5 cm high anhydrous sodium sulfate.

5 instruments and equipment

5.1 Gas Chromatograph. equipped with nitrogen and phosphorus detector (NPD). 5.2 Analysis of balance. 0.01 g and 0.0001 g. GB/T 23200.106-2016 5.3 Gel Permeation Chromatography. 5.4 Centrifuge. 5.5 Rotary Evaporator. 5.6 nitrogen dryers. 5.7 homogenizer.

6 Sample preparation and storage

6.1 Preparation of the sample Samples were minced with a meat grinder, and the sample samples were carried out in accordance with GB 2763 Appendix A, mixed thoroughly, dashed to a ratio of not less than 500 g, Into the cleaning container, sealed, marked mark. 6.2 Storage of samples The sample was stored at -18 ° C or lower.

7 Analysis steps

7.1 Extraction Weigh 10 g of sample (accurate to 0.01 g) in a 100 mL centrifuge tube containing 20 g of anhydrous sodium sulfate, add 30 mL of cyclohexane-acetic acid Ethyl ester mixed solvent, homogenized at 15 000 r/min homogeneous extraction 1.5 min, centrifuged at 3000 r/min for 3 min. Supernatant is filled with An anhydrous sodium sulfate canister was collected in 100 mL pear bottles. The residue was extracted with 30 mL of cyclohexane-ethyl acetate mixed solvent The combined extracts were washed twice and the anhydrous sodium sulphate column was washed with a small amount of cyclohexane-ethyl acetate mixed solvent. The extract was washed with water at 40 ° C Turn to about 2 mL, to be purified. 7.2 Purification 7.2.1 Gel Permeation Chromatography Instrument Conditions A) Purification column. 400 mm × 25 mm, built with BIO-Beads S-X3 packing or equivalent. B) Mobile phase. cyclohexane-ethyl acetate (1 + 1, volume ratio). C) Flow rate. 5 mL/min. D) Injection volume. 5 mL. E) Start collection time. 1.200 s. F) End of collection time. 1 800 s. 7.2.2 Purification The concentrated extract (7.1) was transferred to a 10 mL graduated centrifuge tube and washed several times with a cyclohexane-ethyl acetate mixed solvent Shaped bottles, combined lotion and constant volume to the scale. After centrifugation at 4 000 r/min for 5 min, the supernatant was filtered through a 0.45 μm organic phase filter into gel permeation In the chromatograph of the chromatograph. Purified with a gel permeation chromatograph and collected effluent from 1.200 s to 1 800 s. The effluent was blown with a nitrogen blower Dry, add 1.0 mL n-hexane dissolved, mixed, gas chromatographic determination. 7.3 Determination 7.3.1 Chromatographic determination of reference conditions A) Column. HP-5, 30 m x 0.32 mm (id), film thickness 0.25 μm, or equivalent. B) column temperature. the initial temperature of 100 ℃, keep 0.5min; at 10 ℃/min speed up to 280 ℃, keep 10min. C) Carrier gas (N2). 1.5 mL/min. D) Hydrogen (H2). 3.0 mL/min. E) Air. 60 mL/min. F) Detector temperature. 280 ° C. G) Inlet temperature. 250 ° C. H) Injection volume. 1 μL. I) Injection method. no split injection, 1.5 min after opening the diverter valve. GB/T 23200.106-2016 7.3.2 Chromatographic determination According to the content of the product in the sample, select the appropriate concentration of the standard working solution and the sample to be measured volume of the sample. Standard working fluid and pending The response value of the killer in the sample solution should be within the linear range of the instrument response. Under the above chromatographic conditions, the retention time of propoxur was about 11.1 Min, according to the peak area external standard method. See Appendix A for standard chromatograms. 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 processor or calculate the residue content of the residue in the sample according to formula (1). MA VcA . (1) Where. X - Residue content in the sample in milligrams per kilogram (mg/kg); A - the peak area of the residue in the sample solution; Cs - the concentration of dexamethasone in standard working solutions in micrograms per milliliter (g/mL); V - the final volume of the sample solution in milliliters (mL); AS - the peak area of the killer chromatographic peak in standard working solution; M - the mass of the 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 reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the Record 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 the Record the requirements of D. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification for this method is 0.01 mg/kg. 10.2 Recovery rate The recoveries of the spikes at the level of 0.01 mg/kg, 0.02 mg/kg, 0.05 mg/kg are shown in Appendix B. GB/T 23200.106-2016

Appendix A

(Informative) Standard of Gas Chromatography Figure A.1 Halogen Granite Standard Gas Chromatogram GB/T 23200.106-2016

Appendix B

(Informative) Table B.1 Recovery of the three matrix samples Substrate Name Added Level/(mg/kg) Recovery Range/(%) pork 0.01 80.2 to 107.8 0.02 85.3 ~ 98.7 0.05 88.8 to 96.5 chicken 0.01 83.6 to 102.6 0.02 82.3 ~ 97.0 0.05 87.4 to 97.4 beef 0.01 83.6 to 99.1 0.02 86.6 ~ 99.1 0.05 86.3 ~ 98.8 GB/T 23200.106-2016

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 GB/T 23200.106-2016

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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