A solid phase microextraction—liquid chromatography with ultraviolet detection (SPME-LC-UV) method for the determination of the antimicrobial agent chloramphenicol was developed. The performances of three commercially available fibers were compared; the Carbowax/TPR-100 was found to provide the most efficient extraction. All the aspects influencing the fiber adsorption (extraction time, temperature, pH, salt addition) and desorption (desorption and injection time, desorption solvent mixture composition) of the analyte were investigated. The method was eventually applied to the determination of the drug in both biological (urine) and environmental (tap and sea water) samples. The optimized procedure required a simple sample pretreatment, isocratic elution, and provided enough sensitivity for the analyte determination in the considered samples. The investigated linear ranges were 37–1000 ng/ml (urine), 0.1–10 ng/ml (tap water), 0.3–30 ng/ml (sea water). Within-day and between-days RSD% ranged between 5.5–6.2 and 8.7–9.0 (urine), 5.1–6.0 and 8.4–8.8 (tap water), 5.4–5.7 and 8.6–8.9 (sea water). Estimated LOD and LOQ were 37 and 95 ng/ml (urine), 0.1 and 0.3 ng/ml (tap water), 0.3 and 0.7 ng/ml (sea water).
Solid phase microextraction - liquid chromatography (SPME-LC) determination of chloramphenicol in urine and environmental water samples
ARESTA, Antonella Maria;CALVANO, COSIMA DAMIANA;ZAMBONIN, Carlo
2010-01-01
Abstract
A solid phase microextraction—liquid chromatography with ultraviolet detection (SPME-LC-UV) method for the determination of the antimicrobial agent chloramphenicol was developed. The performances of three commercially available fibers were compared; the Carbowax/TPR-100 was found to provide the most efficient extraction. All the aspects influencing the fiber adsorption (extraction time, temperature, pH, salt addition) and desorption (desorption and injection time, desorption solvent mixture composition) of the analyte were investigated. The method was eventually applied to the determination of the drug in both biological (urine) and environmental (tap and sea water) samples. The optimized procedure required a simple sample pretreatment, isocratic elution, and provided enough sensitivity for the analyte determination in the considered samples. The investigated linear ranges were 37–1000 ng/ml (urine), 0.1–10 ng/ml (tap water), 0.3–30 ng/ml (sea water). Within-day and between-days RSD% ranged between 5.5–6.2 and 8.7–9.0 (urine), 5.1–6.0 and 8.4–8.8 (tap water), 5.4–5.7 and 8.6–8.9 (sea water). Estimated LOD and LOQ were 37 and 95 ng/ml (urine), 0.1 and 0.3 ng/ml (tap water), 0.3 and 0.7 ng/ml (sea water).I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.