ABSTRACT
A new microwave-assisted derivatisation and LC-MS/MS method has been developed for the analysis of nitrofuran metabolites - 3-amino-5-morpholino-methyl-1,3-oxa-zolidinone (AMOZ), 3-amino-2-oxazolidinone (AOZ), 1-aminohydantoin (AHD) and semicarbazide (SEM) - in farm-raised prawns (Penaeus monodon) from the coastal regions of South India. Analysis was carried out by reverse-phase column (Phenomenex Luna C18) with gradient elution using mobile phase A (0.02% acetic acid in water) and mobile phase B (0.02% acetic acid in acetonitrile), at a flow rate of 200 µl min(-1) and an injection volume of 20 µl. Microwave-assisted derivatisation was achieved in 6 min with good recovery. The results showed that the samples collected from Andhra Pradesh and Karnataka contained residues of nitrofuran metabolites in the range from 5.0 to 40 ng g(-1). This work emphasises the importance of ensuring the safety of seafood and that a new method of derivatisation is applicable for the analysis of nitrofuran metabolites in seafood.
Subject(s)
Anti-Bacterial Agents/analysis , Drug Residues/analysis , Food Contamination/analysis , Nitrofurans/analysis , Penaeidae/chemistry , Shellfish/analysis , Animals , Anti-Bacterial Agents/adverse effects , Anti-Bacterial Agents/metabolism , Aquaculture , Drug Residues/adverse effects , Drug Residues/metabolism , India , Microwaves , Nitrofurans/adverse effects , Nitrofurans/metabolism , Penaeidae/metabolism , Shellfish/adverse effects , Tandem Mass SpectrometryABSTRACT
Sulphonamides and chloramphenicol antibiotics were analysed by using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in sea and farmed prawn (Penaeus monodon) samples obtained from the coastal region of southern India during 2011-2012. Average recoveries were 77-99% and precision was between 1% and 8%. The results revealed that in sea prawn samples neither of the two antibiotics was detected, but in farmed samples from coastal Andhra Pradesh some sulphonamides were detected in a concentration range greater than the maximum residual limit as set by Council Directive 2377/90 EC.
Subject(s)
Anti-Bacterial Agents/analysis , Drug Residues/analysis , Food Contamination , Food Inspection/methods , Penaeidae/metabolism , Shellfish/analysis , Animals , Aquaculture , Chloramphenicol/analysis , Chromatography, High Pressure Liquid , European Union , Food Inspection/standards , Guideline Adherence , Health Policy , Health Promotion , Humans , India , Indian Ocean , Limit of Detection , Penaeidae/growth & development , Reproducibility of Results , Shellfish/standards , Sulfonamides/analysis , Tandem Mass SpectrometryABSTRACT
Andrographis paniculata has a long history of use in traditional medicine and andrographolide is one of its potent compounds. In this study, a rapid isolation of andrographolide (colourless, bitter and crystalline diterpene lactone) was carried out by a newly developed microwave-assisted extraction. The extraction intensity, time and amount of solvent were optimised prior to this. The conventional heating method provided a 0.4452% yield of andrographolide and microwave heating at 210 W for 40 min provided a 0.589% yield. Compared to conventional extraction procedures, the results suggested that the proposed method was an effective alternative for the extraction of andrographolide. The isolated compounds were found to be the same by UV, HPTLC and 1H-NMR studies. The isolated andrographolide was tested for in vitro antioxidant activity, and showed a potent free radical scavenging activity.
