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doi:10.1016/j.chroma.2006.03.099 
Copyright © 2006 Elsevier B.V. All rights reserved.
Determination of chloramphenicol residues in meat, seafood, egg, honey, milk, plasma and urine with liquid chromatography–tandem mass spectrometry, and the validation of the method based on 2002/657/EC
Received 25 November 2005;
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Abstract
A simple and rapid method for the determination and confirmation of chloramphenicol in several food matrices with LC–MS/MS was developed. Following addition of d5-chloramphenicol as internal standard, meat, seafood, egg, honey and milk samples were extracted with acetonitrile. Chloroform was then added to remove water. After evaporation, the residues were reconstituted in methanol/water (3 + 4) before injection. The urine and plasma samples were after addition of internal standard applied to a Chem Elut extraction cartridge, eluted with ethyl acetate, and hexane washed. Also these samples were reconstituted in methanol/water (3 + 4) after evaporation. By using an MRM acquisition method in negative ionization mode, the transitions 321 → 152, 321 → 194 and 326 → 157 were used for quantification, confirmation and internal standard, respectively. Quantification of chloramphenicol positive samples regardless of matrix could be achieved with a common water based calibration curve. The validation of the method was based on EU-decision 2002/657 and different ways of calculating CCα and CCβ were evaluated. The common CCα and CCβ for all matrices were 0.02 and 0.04 μg/kg for the 321 → 152 ion transition, and 0.02 and 0.03 μg/kg for the 321 → 194 ion transition. At fortification level 0.1 μg/kg the within-laboratory reproducibility is below 25%.
Keywords: Food analysis; Chloramphenicol; LC–MS/MS
Article Outline
- 1. Introduction
- 2. Experimental
- 2.1. Chemicals
- 2.2. Sample homogeneity
- 2.3. Sample preparation for meat, scampi, egg, honey and milk
- 2.4. Sample preparation for urine and plasma
- 2.5. HPLC
- 2.6. ESI-MS/MS
- 2.7. Blank and spiked samples
- 2.8. Calibration curves
- 2.9. Validation protocol
- 3. Results and discussion
- 3.1. Sample preparation
- 3.2. Ion transitions and ion ratios
- 3.3. Selectivity and within-laboratory reproducibility
- 3.4. Sensitivity, quantification and trueness
- 3.5. Decision limit (CCα) and detection capability (CCβ)
- 3.6. Application
- 4. Conclusion
- References
