CONFI RMATION AND ESTIMATION OF CHL ORAMPHENICOL RESIDUES IN GALDA ( MACROBRACHIUM ROSENBERGII ) BY ULTRA PERFORMANCE LC ® (UPLC) AND MS/MS (TQD ) SYSTEM

An Ultra performance liquid chromatography – tandem quadrupole mass spectrometry (U PLC – MS / MS) method was developed for the determination of chloramphenicol in Galda shrimp ( Macrobrachium rosenbergii ). The UPLC separation was achieve d on a n AQUITY UPLC BEH C 18 Column (2.1 x 50 mm; 1.7 µm) with gra d ient elution using a mobile phase of methanol and water only . Mass spectral acquisition was done using electro spray ionization in the negative ion mode applying multiple reaction monitorin g (MRM) of two diagnostic transition reactions for CAP ( m/z 321 152 and m/z 321 257) and for d5_ CAP ( m/z 326 .03 157) . Shrimp samples were finally extracted with ethylacetate and evaporated to dryness, followed by a clean - up step using the liquid – liquid extraction with acetonitrile / hexane (1:1 v/v) mixture and reconstituted with 50 % methanol and water . The method validation was carried out according to the criteria of Commission d ecision 2002/657/EC. The calibration cur ve showed a good linearity in t he concentration range from 0.05 to 1 .0 n g/g with the correlation coefficient above 0.9 9 95. The decision limits (CCα ) an d a detection capability (CCβ) were 0.04 1 and 0.0 7 0 n g/g respectively. The mean recoveries were in the range of 85 – 11 0 %.

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