CONFIRMATION AND ESTIMATION OF CHLORAMPHENICOL RESIDUES IN GALDA (MACROBRACHIUM ROSENBERGII) BY ULTRA PERFORMANCE LC® (UPLC) AND MS/MS (TQD) SYSTEM
Journal Title: International Research Journal of Pharmacy (IRJP) - Year 2014, Vol 5, Issue 2
Abstract
An Ultra performance liquid chromatography – tandem quadrupole mass spectrometry (UPLC–MS/MS) method was developed for the determination of chloramphenicol in Galda shrimp (Macrobrachium rosenbergii). The UPLC separation was achieved on an AQUITY UPLC BEH C18 Column (2.1 x 50 mm; 1.7 µm) with gradient 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 monitoring (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 decision 2002/657/EC. The calibration curve showed a good linearity in the concentration range from 0.05 to 1.0 ng/g with the correlation coefficient above 0.9995. The decision limits (CCα) and a detection capability (CCβ) were 0.041 and 0.070 ng/g respectively. The mean recoveries were in the range of 85–110 %.
Authors and Affiliations
Md. Ashraful, Muhammad Talukdar , Mst Akter
Keywords
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- EP ID EP152073
- DOI 10.7897/2230-8407.050219
- Views 93
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