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liquid chromatography-mass spectrometry/mass spectrometry determination appendix d chloramphenicols appendix b chloramphenicols appendix e determination method liquid chromatography-mass spectrometry/mass spectrometry total ion current chromatogram sub-item project quality appendix c acceptance record lead extraction technical requirements audio format
GB/T 22338-2008 in English

GB/T 22338-2008 in English

VALID

Determination of Multi-residues of Chloramphenicols in Animal-original Food

  • Issued on:2008-09-01
  • Implemented on:2008-12-01
  • File Format:PDF
  • Delivery:Via email within 1~3 business days
Price(USD): $100.00
$97.00
Standard No: GB/T 22338-2008
Document status: VALID
Title in English: Determination of Multi-residues of Chloramphenicols in Animal-original Food
Title in Chinese: 动物源性食品中氯霉素类药物残留量测定
Language: English
File Format: Electronic (PDF)
Delivery: Via email within 1~3 business days
Issued on: 2008-09-01
Implemented on: 2008-12-01
ICS Classification: 67.120-Meat, meat products and other animal produce
Chinese Classification: X22-Meat processing and products
Professional Classification: GB-National Standard
Related Keywords: liquid chromatography-mass spectrometry/mass spectrometry determination appendix d
chloramphenicols appendix b
chloramphenicols appendix e
determination method
liquid chromatography-mass spectrometry/mass spectrometry total ion current chromatogram
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《GB/T 22338-2008动物源性食品中氯霉素类药物残留量测定》由424-cnca(国家认证认可监督管理委员会)归口,主管部门为国家市场监督管理总局。
本标准规定了动物源性食品中氯霉素类残留量的气相色谱�仓势缀鸵合嗌�谱�仓势祝�质谱测定方法。
本标准适用于水产品、畜禽产品和畜禽副产品中氯霉素、氟甲砜霉素和甲砜霉素残留的定性确证和定量测定。


1 Scope

This standard specifies the determination method of gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry/mass spectrometry for multi-residues of chloramphenicols in animal-original food.
This standard is applicable to qualitative confirmation and quantitative determination of chloramphenicol, florfenicol and thiamphenicol residues in aquatic products, livestock and poultry products and byproducts.

2 Gas Chromatography-Mass Spectrography

2.1 Principle
Extract the sample with ethyl acetate, distribute and purify 4% sodium chloride solution and N-hexane solution-solution, purify through Florisil, and then take methylbenzene as reaction medium, use N, O BSTFA-TMCS (BSTFA+TMCS, 99+1) to silanize at 70℃, determine with gas chromatography/negative chemical ionization source mass spectrometry, and then quantify through internal standard working curve method.
2.2 Reagents and materials
Unless otherwise specified, only confirmed analytical reagent and secondary deionizer water or water with equivalent purity may be used in analysis.
2.2.1 Methanol: chromatographic pure.
2.2.2 Methylbenzene: pesticide residue.
2.2.3 N-hexane: pesticide residue.
2.2.4 Ethyl acetate.
2.2.5 Ethyl ether.
2.2.6 Sodium chloride.
2.2.7 Standard chloramphenicol (CAP), florfenicol (FF) and thiamphenicol (TAP): purity≥99%.
2.2.8 Standard m-chloramphenicol (m-CAP): purity≥99%.
2.2.9 Sodium chloride solution (4%): weight a right amount of sodium chloride to prepare 4% sodium chloride solution with water, store at ambient temperature, and use for 1 week.
2.2.10 Stock standard solution of chloramphenicols: accurately weigh a right amount of standard chloramphenicol, florfenicol and thiamphenicol (with the accuracy of 0.1mg), and prepare with methanol into stock standard solution with a concentration of 100μg/mL.
2.2.11 Internal standard working solution of m-CAP: accurately weigh a right amount of standard m-CAP (with the accuracy of 0.1mg), and prepare with methanol into 10ng/mL standard working solution.
2.2.12 Standard working solution of chloramphenicol substrate: select six portions of samples not containing chloramphenicols, respectively add 1mL internal standard working solution (2.2.11), use these six portions of extracting solutions to respectively prepare the solutions that the concentrations of chloramphenicol, florfenicol and thiamphenicol are 0.1ng/mL, 0.2ng/mL, 1ng/mL, 2ng/mL, 4ng/mL and 8ng/mL, extract according to this method (2.4.1) and purify (2.4.2), prepare into sample extracting solution, slowly dry with nitrogen, silanize, and then prepare into standard working solution.
2.2.13 Derivatization reagent: N, O BSTFA-TMCS (BSTFA+TMCS, 99+1).
2.2.14 Solid-phase extraction column: Florisil column (6.0mL, 1.0g).
2.3 Instruments and equipment
2.3.1 Gas chromatography/mass spectrometry chromatograph: equipped with chemical ionization source (CI).
2.3.2 Tissue blender.
2.3.3 Solid-phase extraction device.
2.3.4 Oscillator.
2.3.5 Rotary evaporator.
2.3.6 Vortex mixer.
2.3.7 Centrifuge.
2.3.8 Thermotank.
2.4 Determination procedures
2.4.1 Extraction

Foreword I
1 Scope
2 Gas Chromatography-Mass Spectrography
3 Liquid Chromatography-Mass Spectrometry/Mass Spectrography
Appendix A (Informative) Gas Chromatography-Mass Spectrometry Total Ion Current Chromatogram and Mass Spectrogram of Derivatives of Standard Substances of Chloramphenicols
Appendix B (Informative) Average Recovery and Precision of Medicines of Chloramphenicols in Different Substrates (GC/MS Method)
Appendix C (Informative) Reference Conditions of Liquid Chromatography-Mass Spectrometry/Mass Spectrometry Determination
Appendix D (Informative) Liquid Chromatography-Mass Spectrometry/Mass Spectrometry Total Ion Current Chromatogram and Remodeling Ion Chromatogram of Standard Substances of Chloramphenicols
Appendix E (Informative) Average Recovery and Precision of Medicines of Chloramphenicols in Different Substrates (LC-MS/MS Method)

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