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Determination of chloramphenicol residue in milk by liquid chromatography tandem mass spectrometry (LCMSMS) Update: 9/20/2012 4:30:34 PM (GMT+7)

Chu Van Tuat, Dau Ngoc Hao ,Tran Thi Mai Thao, Phan Thi Hue, Vu Dung Minh and Pham Thi Trang, - The method for determination of chloramphenicol residue in milk by liquid chromatography tandem mass spectrometry was successfully developed and validated. The method is ‘fit for purpose’ to detect trace amount of the CAP at Minimum Required Performance Limit (MRPL, 0.3 µg/kg).

 

SUMMARY

The method for determination of chloramphenicol residue in milk by liquid chromatography tandem mass spectrometry was successfully developed and validated. The method is ‘fit for purpose’ to detect trace amount of the CAP at Minimum Required Performance Limit (MRPL, 0.3 µg/kg).

The trace amount of CAP in milk was extracted by ethyl acetate, filtered and injected onto the LC-MS/MS system. Detection of CAP was achieved by negative ionization electrospray (ESI) in the selected ionization monitoring (SIM) mode. For confirmation, three characteristic mass transitions were monitored each for the CAP and the CAP-d5 standard. The method was validated according to the decision 657/2002/EC of European Union criteria for the analyses of veterinary drug residues in food. The repeatability and the recovery at all three fortification levels at 0.3, 0.45, 0.6 μg kg-1 at different days of the method was 7.6% and within the ranges of -50 ÷ +20%, respectively. The within-laboratory reproducibility on different milk matrices was 16.5%. The decision limit (CCα) and the detection capability (CCβ) were at 0.10 and 0.12 μg kg-1, respectively. The meaurement uncertainty of the method was 33.1%.

Key words: Chloramphenicol, Residue, Validation method, Milk, Liquid chromatography tandem mass spectrometry.

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