LC-MS/MS-based determination of chloramphenicol, thiamphenicol, florfenicol and florfenicol amine in poultry meat from the Punjab-Pakistan

Abstract

A simple, reliable and sensitive liquid chromatography-tandem mass spectrometry-based confirmatory method was redeveloped and validated for the simultaneous determination of chloramphenicol, thiamphenicol, florfenicol and florfenicol amine in chicken muscles. The analytes were extracted from minced chicken muscle with acetonitrile and ammoniated water mixture. A second extraction with ethyl acetate was followed by evaporation and dissolution of the residue in ammoniated methanol before defatting with n-hexane. Finally, the extract was further cleaned up by dispersive solid phase extraction using C-18 end-capped dispersive material. The validation protocol was adapted from the European Commission Decision 2002/657/EC and all the performance characteristics were successfully satisfied. The recoveries of all the analytes were found to be in the range of 86.4-108.1% and the precision values, within day and between days, ranged from 2.7% to 11% and 4.4% to 16.3%, respectively. The method was tested in various incurred samples and applied to analyse a wide range of random poultry market samples (n = 120) collected from three cities of the Punjab, Pakistan. Chloramphenicol and florfenicol residues were detected at low levels in less than 11% of the samples. Chloramphenicol was detected only in 4 samples with the concentration range of 0.17-0.477 µg kg, whereas the levels of florfenicol/florfenicol amine residues detected in 9 samples ranged from 8.7 to 32.8 µg kg. Moreover, most of the florfenicol residues were identified as tissue bound, extractable only after strong acid hydrolysis.

Development and comparison of liquid–liquid extraction and accelerated solvent extraction methods for quantitative analysis of chloramphenicol, thiamphenicol, florfenicol, and florfenicol amine in poultry eggs

“…Different mobile phase compositions were used for the best separation of CAP, TAP, FF, and FFA on a C 18 column. FFA is a highly polar drug metabolite and is poorly retained on C 18 columns under neutral mobile phase conditions . Barreto et al reported that the addition of 2mM ammonium acetate to the mobile phase allowed good separation of CAP, TAP, FF, and FFA and favoured FFA retention on C 18 columns under alkaline conditions.…”

“…Various extraction methods were employed to extract CAP, TAP, FF, and FFA from animal-derived foods. These methods included LLE, 10,12,17,19,20 fabric-phase sorptive extraction (FPSE), 11 matrix solid-phase dispersion (MSPD), 15,22 LLE-solid-phase extraction (LLE-SPE), 16,24,25 QuEChERS extraction, 18 SPE, 21 and subcritical water extraction (SWE). 23 The LLE method for extracting samples is simple, but it consumes a large quantity of reagents and takes a long time and is thus not suitable for batch processing of samples.…”

“…FFA is a highly polar drug metabolite and is poorly retained on C 18 columns under neutral mobile phase conditions. 19 Barreto et al 17 In the MS/MS experiments, one precursor ion and two product ions for each target compound were used for the confirmatory analysis, and the most abundant of these ions was used for quantitative purposes in compliance with Decision 2002/657/EC. 27 The total ion chromatogram…”

“…To date, various methods have been used to measure CAP, TAP, FF, and FFA in animal-derived foods; these methods include the fluorescent microsphere lateral flow immunoassay (FM-LFA), 7 enzyme-linked immunosorbent assay (ELISA), 8,9 reversed-phase high-performance liquid chromatography with ultraviolet detection (RP-HPLC-UVD), 10 HPLC with diode array detection (DAD), 11 RP-HPLC with fluorescence detection (FLD), 12 LC-mass spectrometry (MS), 13,14 LC tandem mass spectrometry (MS/MS), [15][16][17][18][19][20] ultra-performance liquid chromatography (UPLC)-MS/ MS, [21][22][23][24] and gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS). 25 In previous research, we developed an LC-MS/MS 20 method for the simultaneous determination of CAP, TAP, FF, and FFA in eggs.…”

Simple, efficient, and eco‐friendly sample preparation for simultaneous determination of paracetamol and chloramphenicol in meat

“…For further evaluation, a comparison of the proposed method with the reported methods in literatures for determining PCM or CAP in animal‐origin foods with SPE is provided in Supporting Information Table S1 and S2. It can be seen that the targets were all extracted with organic solvents.…”