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GB 23200.88-2016 English PDF

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GB 23200.88-2016: Food safety national standard -- Detection of Organochlorine Pesticide Residues in Aquatic Products
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GB 23200.88-2016English199 Add to Cart 3 days [Need to translate] Food safety national standard -- Detection of Organochlorine Pesticide Residues in Aquatic Products Valid GB 23200.88-2016

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Basic data

Standard ID GB 23200.88-2016 (GB23200.88-2016)
Description (Translated English) Food safety national standard -- Detection of Organochlorine Pesticide Residues in Aquatic Products
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 10,191
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN 0598-1996
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 23200.88-2016: Food safety national standard -- Detection of Organochlorine Pesticide Residues in Aquatic Products


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Food safety national standard - Detection of Organochlorine Pesticide Residues in Aquatic Products Instead of SN/T 0598-1996 National Standards of People's Republic of China GB National standards for food safety Detection of Organochlorine Pesticide Residues in Aquatic Products National food safety standards- Determination of the multiple residue of organochlorine pesticides in aquatic 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/T 598-1996 "Test methods for the determination of multiple organochlorine pesticide residues in aquatic products". Compared with SN/T 598-1996, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name of the "export aquatic products" to "aquatic products"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 598-1996. National standards for food safety Detection of Organochlorine Pesticide Residues in Aquatic Products

1 Scope

This standard specifies the six or six (BHC) and isomers of aquatic products, hexachlorobenzene (HCB), heptachlor, epoxidized heptachlor, aldrin, (DDT) and isomers and analogues (DDD, DDE), Samples, and Gas Chromatography law. This standard is applicable to 14 kinds of organochlorine pesticides (α-BHC, β-BHC, γ-BHC, δ-BHC, hexachlorobenzene, heptachlor, ring O, p'-DDT, p, p'-DDT, p, p'-DDD, p, p'-DDE) were measured, its It can refer to the implementation of food.

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

After the sample was dried and dried with anhydrous sodium sulfate, the pesticide residue was extracted with acetone-petroleum ether, and the extract was purified by florisil The sample was purified by a gas chromatograph equipped with an electron capture detector and quantified by 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 petroleum ether. boiling range 60-90 ° C after purification by alumina column distillation with an all-glass distiller, collecting 60-90 ° C fractions. 4.1.3 ether (C4H10O). re-distillation. 4.1.4 anhydrous sodium sulfate (Na2SO4). analytical pure; 650 ℃ burning 4 h, stored in a sealed container in reserve. 4.2 solution preparation 4.2.1 ether - petroleum ether leaching solution (15 85). take 150 mL of ether, add 850 mL of petroleum ether, shake back. 4.3 standards 4.3.1 Organochlorine pesticide standards (α-BHC, β-BHC, γ-BHC, δ-BHC, hexachlorobenzene, heptachlor, epoxidized heptachlor, aldrin O, p'-DDT, p, p'-DDT, p, p'-DDD, p, p'-DDE). purity ≥99%. 4.4 standard solution preparation 4.4.1 14 kinds of organochlorine pesticide standard solution. accurately weighed the right amount of each pesticide standard, respectively, with a small amount of benzene dissolved, and then use petroleum ether A standard stock solution with a concentration of 0.100 mg/mL was prepared. According to the need to then prepare the appropriate concentration of petroleum ether mixed standard working solution. Store in 4 ℃ refrigerator. 4.5 Materials 4.5.1 Alumina. chromatography, neutral, 100-200 mesh, 800 ℃ burning 4 h, cooled to room temperature stored in a sealed container in reserve. before use Should be dried at 130 ° C for 2 hours. 4.5.2 Fluorine Silica. 60-100 mesh, 650 ℃ burning 4 h, stored in a sealed container in reserve. And dried at 130 ° C for 1 hour before use. Note. Each batch of florisil should be used before the leaching curve.

5 instruments and equipment

5.1 Gas Chromatograph. Electron Capture Detector (ECD). 5.2 Alumina purification column. 300 mm × 20 mm (inner diameter) glass column, filled with alumina 40 g, the top into the 10 g anhydrous sodium sulfate dry method The column is rinsed with 40 mL of petroleum ether before use. 5.3 Analysis of balance. 0.01 g and 0.0001 g. 5.4 Soxhlet extractor. 250 m L. 5.5 All glass re-distillation unit. 5.6 glass mortar. caliber 11.5 cm 5.7 Rotary Evaporator or Nitrogen Flow Concentrator. 250 mL of vials. 5.8 Microiner. 10 μL. 5.9 absorbent cotton. after acetone a petroleum ether (2 8) mixture solution 6 h treatment. 5.10 meat grinder.

6 Preparation and storage of samples

The extracted sample was thoroughly crushed and mixed. Divided out by 1 points, divided equally For the two, respectively, into the clean container, as a sample. Sealed and marked with mark. The sample is stored at a temperature below 18 ° C. During sample and sample preparation, it is necessary to prevent contamination of the sample or the change in the content of the residue. Note. The above sample sampling site according to GB 2763 Appendix A implementation.

7 Analysis steps

7.1 Extraction Weigh the sample 10.0 g (accurate to 0.1 g) in a mortar, add 15 g of anhydrous sodium sulfate for several minutes, the sample made of dry powder. Into the filter tube. Into the Soxhlet extractor. Add 100 mL of acetone-petroleum ether (2 8) to the vial of the extractor on a water bath Extraction for 6 h (reflow rate 10-12 times per hour). The extract was concentrated to about 5 mL under reduced pressure or a nitrogen stream. 7.2 Purification The extract was completely transferred to a florisil silica column. Discard the effluent. Into.200 mL of ether-oil ether eluent for elution. At the beginning, take part of the ether-petroleum ether mixture to clean the extraction bottle, and the lotion into the purification column. Elution flow rate of 2-3 ML/min, and the effluent was collected in a 250 mL vial. Concentrated in a reduced pressure or nitrogen stream and set to 10 mL, for gas chromatographic determination. 7.3 Determination 7.3.1 Gas Chromatographic Reference Conditions A) Column. SGE capillary column (or equivalent column), 25 m x 0.53 mm (inner diameter), film thickness. 0.15 μm. Fixed phase. HT5 (not Polar) bond phase; B) Carrier gas. nitrogen (purity ≥99.99%), 10 mL/min; C) Auxiliary gas. nitrogen (purity ≥99.99%), 40 mL/min; D) Column temperature. the program temperature is as follows. 100 ° C 140 ° C.200 ° C 230 ° C E) Inlet temperature..200 ° C; F) detector temperature. 300 ° C; G) Injection method. Stem injection method. 7.3.2 Determination of gas chromatography According to the organic chlorine in the sample solution, according to the type and content of the organochlorine pesticide in the sample solution, the corresponding standard working mixture with similar peak height is selected. The reaction value of each organochlorine pesticide in standard working mixture and sample solution should be within the linear range of instrument detection. On the standard working mixture and sample solution Measurement of volume injection. Under the above chromatographic conditions, the sequence and retention time of each organochlorine pesticide were as follows. 1.14 kinds of organochlorine pesticides The chromatogram of the standard is shown in Appendix A. Table 1 Peak sequence and retention time of organochlorine pesticides Pesticide name retention time min pesticide name retention time min Α-BHC, 10.55 Epoxy Hexachlor 15.04 HCB 10.76 Dieldrin 16.28 Γ-BHC 11.75 p, p'-DDE 16.44 Β-BHC 12.10 Endrin 16.75 Δ-BHC 12.90 o, p'-DDT 17.12 Heptachlor 13.08 p, p'-DDD 17.44 Aldrin 13.97 p, p'-DDT 17.92 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 calculate the content of the organochlorine pesticide in the sample according to formula (1). The calculation result shall be deducted from the blank value. Hi × c × V HiS × m Xi = (1) 5 ° C/min 10 ° C/min 15 ° C/min 2min 5min Where. Xi - Residues of organochlorine pesticides in samples, mg/kg, mg/kg; C - concentration of organochlorine pesticides in standard working solutions in micrograms/ml, μg/mL; Hi - peak height of organochlorine pesticides in sample solution, mm; His - the peak of the organochlorine pesticides in the standard working solution, mm; V - the final volume of the sample solution, in milliliters, mL; M - the amount of sample weighed, 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 the requirements of D. 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 E. 10% limit and recovery rate 10.1 Quantitation limits Quantitative limits for organochlorine pesticides in this method Appendix B. 10.2 Recovery rate The concentration and recovery of the sample by gas chromatography are shown in Appendix C.

Appendix A

(Informative) Standard Chromatography and Mass Spectrometry

Appendix B

(Informative) Quantitative limits of organochlorine pesticides Table B.1 Quantitative limits of organochlorine pesticides Pesticide name quantitative limit, mg/kg pesticide name quantitative limit, mg/kg Α-BHC, 0.005 Epoxy Hexachlor 0.02 HCB 0.005 Dieldrin 0.01 Γ-BHC 0.005 p, p'-DDE 0.02 Β-BHC 0.005 Endrin 0.02 Δ-BHC 0.005 o, p'-DDT 0.025 Heptachlor 0.01 p, p'-DDD 0.025 Aldrin 0.01 p, p'-DDT 0.025

Appendix C

(Informative) Sample concentration and recovery of the experimental data Table C.1 Determination of the concentration and recovery of the sample by gas chromatography Name of pesticide Add concentration (Mg/kg) Recovery rate (%) Name of pesticide Add concentration (Mg/kg) Recovery rate (%) Α-BHC 0.005 89.28 Epichlorohydrin 0.02 94.57 0.01 91.15 0.04 92.80 0.05 90.16 0.2 93.00 HCB 0.005 86.24 Dieldrin 0.01 90.04 0.01 89.84 0.02 93.11 0.05 89.93 0.1 93.57 Γ-BHC 0.005 92.86 P, p'-DDE 0.02 94.71 0.01 93.06 0.04 94.73 0.05 91.26 0.2 95.65 Β-BHC 0.005 89.5 Endrin 0.02 92.15 0.01 88.54 0.04 91.91 0.05 90.28 0.2 93.45 Δ-BHC 0.01 86.14 o, p'-DDT 0.025 93.64 0.02 89.99 0.05 93.54 0.05 90.44 0.25 94.22 Heptachlor 0.05 91.88 p, p'-DDD 0.025 92.00 0.01 92.00 0.05 94.8 0.02 91.91 0.25 96.29 Aldrin 0.01 91.91 p, p'-DDT 0.025 92.89 0.02 91.92 0.05 94.27 0.1 92.67 0.25 94.08

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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