A simple method for the determination of chloramphenicol in 22 matrices was prepared based on the QuEChERS and HPLC-MS/MS combination. Following a hydrolysis step, the homogenized samples were extracted and partitioned after adding sodium chloride with acetonitrile. Chloramphenicol was analysed by HPLC-MS/MS in negative electrospray mode by monitoring the daughter ions m/z: 321→194 and 321→152. The limit of decision (CCα) was calculated at the range of 0.10 μg kg−1 to 0.15 μg kg−1 and detection capability (CCβ) from 0.12 μg kg−1 to 0.18 μg kg−1. Validation results showed that this method is suitable for the determination and confirmation of chloramphenicol in various matrices.
A quantitative method for the determination of chloramphenicol in milk samples was developed based on the QuEChERS (quick, easy, cheap, effective, rugged, and safe) approach for liquid chromatography–tandem mass spectrometry (LC–MS/MS). Homogenized milk samples were extracted with acetonitrile. The partitioning step was performed after the addition of magnesium sulfate and sodium chloride. Chloramphenicol was determined using the electrospray negative ionization mode with tandem mass spectrometry. The procedure was validated according to the requirements of Commission Decision 2002/657/EC. The apparent recovery ranged from 90% to 110% and within-laboratory reproducibility was lower than 12%. The calculated limit of decision was 0.10 μg kg−1 and the detection capability was 0.15 μg kg−1. Validation results demonstrated that this method fulfills criteria for the determination of chloramphenicol in milk.
1 September 2014 in Bulletin of the Veterinary Institute in Pulawy
The occurrence of commonly used veterinary antimicrobial agents was investigated in 159 fresh water, 443 fish, and 150 sediment samples from Polish rivers and lakes. The agents included aminoglycosides, ß-lactams, diaminopyrimidines, fluoroquinolones, lincosamides, macrolides, pleuromutilins, sulfonamides, and tetracyclines. The analysis was performed by three different sample preparation procedures for each matrix and it was performed by liquid chromatography-tandem mass spectrometry with electrospray ionisation source in positive mode, under the same conditions. All analytical methods used were validated and showed good sensitivity, accuracy, and precision. The LOQ was in the range from 5 μg/kg to 125 μg/kg for fish samples, from 0.02 μg/L to 10 μg/L for fresh water samples, and from 1 μg/kg to 8 μg/kg for sediment samples.