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  • P-ISSN 2233-4203
  • E-ISSN 2093-8950

Determination of Ceftiofur Residues by Simple Solid Phase Extraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry in Eel, Flatfish, and Shrimp

Mass Spectrometry Letters / Mass Spectrometry Letters, (P)2233-4203; (E)2093-8950
2019, v.10 no.2, pp.43-49
https://doi.org/10.5478/MSL.2019.10.2.43
Kim Joohye (National Institute of Food and Drug Safety Evaluation)
Shin Dasom (National Institute of Food and Drug Safety Evaluation)
Kang Hui-Seung (National Institute of Food and Drug Safety Evaluation)
Lee Eunhye (Busan Regional Office of Food and Drug Administration)
Choi Soo Yeon (National Institute of Food and Drug Safety Evaluation)
Lee Hee-Seok (National Institute of Food and Drug Safety Evaluation)
Cho Byung-Hoon (National Institute of Food and Drug Safety Evaluation)
Lee Kang-Bong (National Institute of Food and Drug Safety Evaluation)
Jeong Ji Yoon (National Institute of Food and Drug Safety Evaluation)
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Abstract

The aim of this study was conducted to develop an analytical method to determine the concentration of ceftiofur residue in eel, flatfish, and shrimp. For derivatization and extraction, the sample was hydrolyzed with dithioerythritol to produce desfuroylceftiofur, which was then derivatized by iodoacetamide to obtain desfuroylceftiofur acetamide. For purification, the process of solid phase extraction (Oasis HLB) was used. The target analytes were confirmed and quantified in C 18 column using liquid chromatography-tandem mass spectrometry with 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B) as the mobile phase. The linearity of the standard calibration curve was confirmed by a correlation coefficient, r 2 > 0.99. The limit of quantification for ceftiofur was 0.002 mg/kg; the accuracy (expressed as the average recoveries) was 80.6-105%; the precision (expressed as the coefficient of variation) was below 6.3% at 0.015, 0.03, and 0.06 mg/kg. The validated method demonstrated high accuracy and acceptable sensitivity to meet the Codex guideline requirements. The developed method was tested using market samples. As a results, ceftiofur was detected in one sample. Therefore, it can be applied to the analysis of ceftiofur residues in fishery products.

keywords
ceftiofur, residue, analytical method, fish, shrimp, LC-MS/MS


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Submission Date
2019-02-02
Revised Date
2019-03-25
Accepted Date
2019-03-29
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