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GB 23200.93-2016 English PDF

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GB 23200.93-2016: Food safety national standard -- Determination of organophosphorus pesticide residues in foodstuffs by gas chromatography-mass spectrometry
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Standard similar to GB 23200.93-2016

GB/T 38211   GB/T 18418   GB/T 18419   GB 23200.102   GB 23200.84   GB 23200.101   

Basic data

Standard ID GB 23200.93-2016 (GB23200.93-2016)
Description (Translated English) Food safety national standard -- Determination of organophosphorus pesticide residues in foodstuffs by gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 12,186
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 0123-2010
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 23200.93-2016: Food safety national standard -- Determination of organophosphorus pesticide residues in foodstuffs by gas chromatography-mass spectrometry


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Food safety national standard - Determination of organophosphorus pesticide residues in foodstuffs by gas chromatography - mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 0123-2010 National standards for food safety Determination of organophosphorus pesticide residues in food Gas chromatography - mass spectrometry National food safety standards- Determination of organophosphorus multi pesticides residue in foods Gas chromatography - mass spectrometry 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 0123-2010 "Determination of organophosphorus pesticide residues in foodstuffs for import and export of animals by gas chromatography-mass spectrometry". Compared with SN/T 0123-2010, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name and scope of the "export food" to "food"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 0123-2010. National standards for food safety Determination of organophosphorus pesticide residues in foodstuffs by gas chromatography - mass spectrometry

1 Scope

This standard provides for the import and export of animal food in the 10 kinds of organophosphorus pesticide residues (dichlorvos, diazine phosphorus, dolphin phosphorus, fenitrothion, Maltophos, chlorpyrifos, fenthion, parathion, ethionophos, and phosphorus) were determined by gas chromatography-mass spectrometry. This standard applies to the determination and confirmation of organophosphorus pesticide residues in canned beef, pork, chicken, beef and fish. Goods 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 samples were extracted with water-acetone solution homogenized, dichloromethane liquid-liquid distribution, gel column purification, and then by graphite carbon black solid phase extraction column Purification, gas chromatography - mass spectrometry, external standard method.

4 reagents and materials

Unless otherwise specified, the reagents used are analytical pure, water for the GB/T 6682-1992 prescribed a water. 4.1 Reagents 4.1.1 Acetone (C3H6O). Residue level. 4.1.2 dichloromethane (CH2Cl2). residual grade. 4.1.3 Cyclohexane (C6H12). Residue level. 4.1.4 ethyl acetate (C4H8O2). residual grade. 4.1.5 n-hexane (C6H14). residual grade. 4.1.6 Sodium chloride (NaCl). 4.2 solution preparation 4.2.1 anhydrous sodium sulfate. 650 ℃ burning 4 h, stored in a sealed container in reserve. 4.2.2 Sodium chloride aqueous solution (5%). Weigh 5.0 g of sodium chloride, dissolve in water and set to 100 mL. 4.2.3 Ethyl acetate - n-hexane (1 1, V/V). Take 100 mL of ethyl acetate and 100 mL of n-hexane. 4.2.4 Cyclohexane-ethyl acetate (1 1, V/V). Measure 100 mL of cyclohexane and 100 mL of n-hexane. 4.3 standards 4.3.1 10 kinds of organophosphorus pesticide standards. purity ≥ 95%. 4.4 standard solution preparation 4.4.1 Standard stock solution. Accurately weigh the appropriate amount of each pesticide standard (see Appendix A), with acetone were prepared into the concentration of 100-1000 g/mL standard stock solution. 4.4.2 mixed standard working solution. according to the need to further use acetone diluted to the appropriate concentration of a series of mixed standard working solution. Save on 4 ℃ inside the refrigerator. 4.5 Materials 4.5.1 Fluoresa Silica Solid Phase Extraction Column. Florisil, 500 mg, 6 mL, or equivalent. 4.5.2 Graphitized Carbon Black Solid Phase Extraction Column. ENVI-Carb, 250 mg, 6 mL, or equivalent, prior to use with 6 mL of ethyl acetate Pre-leaching. 4.5.3 Organic phase microporous membrane. 0.45 m. 4.5.4 graphitized carbon black. 60-80 mesh.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. Equipped with an electron impact source (EI). 5.2 Electronic balance. 0.01 g and 0.0001 g. 5.3 Gel Chromatograph. equipped with unit pump, fraction collector. 5.4 Homogenizer. 5.5 Rotary evaporator. 5.6 stoppered conical flask. 250 mL. 5.7 separatory funnel. 250 mL. 5.8 Concentrated bottles. 250 mL. 5.9 Centrifuge. 4000r/min or more.

6 Preparation and storage of samples

6.1 Preparation of the sample To take a sample of about 1 kg sample sampling site according to GB 2763 Appendix A implementation, the mashed machine fully mashed evenly, into the clean capacity Seal, mark. 6.2 Sample storage Samples were stored at -18 ° C. During sample and sample preparation, the sample should be protected from contamination or changes in the residue content.

7 Analysis steps

7.1 Extraction Weigh 20g (accurate to 0.01g) of the thawed sample in a 250 mL stoppered flask with 20 mL of water and 100 mL of acetone, Homogeneous extraction 3min. The extract was filtered and the residue was extracted again with 50 mL of acetone. The filtrate was combined in a 250 mL concentration flask. 40 & lt; 0 & gt; C in a water bath to about 20 mL. The concentrated extract was transferred to a 250 mL separatory funnel, 150 mL of sodium chloride aqueous solution and 50 mL of dichloromethane were added, shaking 3 Min, and the layers were separated and the dichloromethane phase was collected. The aqueous phase was extracted twice with 50 mL of dichloromethane and the combined dichloromethane phases were combined. Without water The sodium sulfate was dehydrated and collected in a 250 mL concentrated flask and concentrated in a 40 ° C water bath to near dryness. Add 10 mL of cyclohexane-ethyl acetate to dissolve The residue was filtered through a 0.45 m filter and purified by gel chromatography (GPC). 7.2 Purification 7.2.1 Gel chromatography (GPC) purification 7.2.1.1 Gel chromatographic conditions A) Gel purification column. Bio Beads S-X3,700 mm × 25 mm (id), or equivalent; B) Mobile phase. ethyl acetate-cyclohexane (1 1, V/V); C) flow rate. 4.7 mL/min; D) Sample loop. 10 mL; E) Pre-leaching time. 10 min; F) Gel chromatographic equilibration time. 5 min; G) Collection time. 23 ~ 31 min. 7.2.1.2 Gel Chromatographic Purification Procedure 10 mL of the purified liquid was purified under the conditions specified in 6.2.1.1, and the components of the 23 to 31 min interval were collected and concentrated at 40 ° C To near dry, and with 2mL ethyl acetate - n-hexane dissolved residue, to be solid phase extraction purification. 7.2.2 Solid phase extraction (SPE) purification A graphitized carbon black solid phase extraction column (1.5 cm high graphitization on a graphitized carbon black solid phase extraction column for deeper pigments) Carbon black) was rinsed with 6 mL of ethyl acetate-n-hexane to remove the eluent; 2 mL of the solution to be purified was poured into the above column and treated with 3 mL Ethyl acetate-n-hexane was washed three times and the flask was poured into a graphitized carbon black solid phase extraction column and then 12 mL of ethyl acetate- N-hexane elution, the above eluate was collected in a vial, washed in a 40 ° C water bath and evaporated to near dryness, dissolved with ethyl acetate and allowed to settle to 1.0 mL, for gas chromatography-mass spectrometry and confirmation. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. 30 m × 0.25 mm (id), film thickness 0.25 m, DB-5 MS quartz capillary column, or equivalent; B) Column temperature. 50 ° C (2 min) 30 ° C/min 180 ° C (10 min) 30 ° C/min 270 ° C (10 min); C) Inlet temperature. 280 ° C; D) chromatographic - mass spectrometer interface temperature. 270 ° C; E) Carrier gas. helium, purity ≥99.999%, flow rate 1.2 mL/min; F) Injection volume. 1 μL; G) Injection method. no split injection, 1.5 min after the opening valve; H) ionization mode. EI; I) ionization energy. 70 eV; J) Measurement method. Select the ion monitoring mode; K) Select the monitoring ions (m/z). see Table 1 and Appendix B; L) solvent delay. 5 min; M) ion source temperature. 150 ° C; N) four pole temperature..200 ℃. Table 1 Select the mass spectrometry parameters for the ion monitoring mode Channel time (tR/min) Select ion (amu) 1 5.00 109, 125, 137, 145, 179, 185,.199, 220, 270, 285, 2 17.00 109, 127, 158, 169, 214, 235, 245, 247, 258, 260, 261, 263, 285, 286, 3 19.00 153, 125, 384, 226, 210, 334 7.3.2 Determination and confirmation of gas chromatography-mass spectrometry According to the sample solution content of the sample, the selected concentration of similar standard working solution, the standard working solution and sample volume and other volume into the The response values of each organophosphorus pesticide in the standard working solution and the sample to be measured shall be within the linear range of the instrumentation. If there is a chromatographic peak at the same retention time in the selective ion chromatogram of the sample solution with the standard working solution, The type of each organophosphorus pesticide selection ion and its abundance ratio were confirmed. Under the above gas chromatographic - mass spectrometric conditions, 10 organophosphorus pesticides The reference retention time of the standard and the gas chromatographic-mass spectrometry ion chromatogram are shown in Appendix B and Appendix C in Figure C.1.

8 results are calculated and expressed

The amount of each organophosphorus pesticide residue in the sample is calculated as follows. Ai × ci × V Xi = ------------------------------ Ais × m Where. Xi - the amount of each organophosphorus pesticide residue in the sample, mg/kg; The peak area (or peak height) of each organophosphorus pesticide in the sample solution; Ais - the peak area (or peak height) of each organophosphorus pesticide in standard working fluids; Ci - the concentration of each organophosphorus pesticide in standard working fluid, g/mL; V - the final volume of the sample solution, mL; M - the final sample represents the sample mass, 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 The quantification of the 10 organophosphorus pesticide residues in food by this method is given in Appendix B. 10.2 Recovery rate 10.2.1 The recoveries of 10 organophosphorus pesticides in steamed pork cans were 70.0-94.9% at 0.02-1.00 mg/kg. 10.2.2 The recoveries of 10 organophosphorus pesticides in pork were 71.2-97.1% at 0.02-1.00 mg/kg. 10.2.3 The recoveries of 10 organophosphorus pesticides in chicken were 0.02.3.00 mg/kg, and the recoveries were 74.3-94.8%. 10.2.4 The recoveries of 10 organophosphorus pesticides in beef were between 70.6 and 96.9% at 0.02-1.00 mg/kg. 10.2.5 The recovery rate of 10 organophosphorus pesticides in fish was 0.02.3.00 mg/kg 76.3-93.3%.

Appendix A

(Informative) Table A.1 List of 10 Organophosphorus Pesticides No. pesticide name English name CAS.No chemical formula Dichlorvos 000062-73-7 C4H7Cl2O4P 2 Diazinon 000333-41-5 C12H21N2O3PS 3 Flies Phosphorus Fenchlorphos 000299-84-3 C8H8Cl3O3PS 4 Fenitrothion 000122-14-5 C9H12NO5PS 5 malathion 000121-75-5 C10H19O6PS2 Chlorpyrifos 002921-88-2 C9H11Cl3NO3PS 7 times thiophosphate Fenthion 000055-38-9 C10H15O3PS2 8 Parathion 000056-38-2 C10H14NO5PS 9 Ethiophenes Ethion 000563-12-2 C9H22O4P2S4 10 Flies Phosphorus Coumaphos 000056-72-4 C14H16ClO5PS

Appendix B

(Informative) 10 kinds of organophosphorus pesticide retention time, quantitative and qualitative selection of ions and quantitative limit table No. pesticide name keep time (Min) Characteristic fragment ion (amu) quantitative limit (g/g) quantitative qualitative abundance ratio 1 dichlorvos 6.57 109 185, 145, 220 37. 100. 12. 07 0.02 2 diazepine 12.64 179 137,.199, 304 62. 100. 29. 11 0.02 3 Pigeon Phosphorus 16.43 285 125, 109, 270 100. 38. 56. 68 0.02 4 fenitrothion 17.15 277 260, 247, 214 100. 10. 06. 54 0.02 5 malathion 17.53 173 127, 158, 285 07. 40. 100. 10 0.02 6 chlorpyrifos 17.68 197 314, 258, 286 63. 68. 34. 100 0.01 7 times thiophosphate 17.80 278 169, 263, 245 100. 18. 08. 06 0.02 8 parathion 17.90 291 109, 261, 235 25. 22. 16. 100 0.02 9 Ethionophos 20.16 231 153, 125, 384 16. 10. 100. 06 0.02 10 Phytotoxin 23.96 362 226, 210, 334 100. 53. 11. 15 0.10

Appendix C

(Informative) Gas Chromatography - Mass Spectrometry of 10 Kinds of Organophosphorus Pesticide Reference Materials 1. dichlorvos 2. diazinophos 3. dolphin phosphate 4. fenitrothion 5. malathion 6. chlorpyrifos 7. times thiophosphate 8. parathion 9. Ethosulfurophos 10. Flies phosphorus Figure C.1 Gas Chromatography-Mass Spectrometry Ion Chromatography (GC-MSD) for 10 organophosphorus pesticide standards

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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