Cloud-point extraction followed by high pressure liquid chromatography with UV spectrophotometric detection for determination of permethrin in urine samples

• Published in: Analytical methods 2015-01, Vol.7 (18), p.7758-7764
• Main Authors: Madej, Katarzyna, Sekiewicz, Agnieszka, Kalenik, Tatyana K, Piekoszewski, Wojciech
• Format: Article
• Language: English
• Subjects: Acetonitrile; Dissolution; Extraction; Liquid chromatography; Mathematical analysis; Pesticides; Spectrophotometry; Urine
• ISSN: 1759-9660; 1759-9679
• DOI: 10.1039/c5ay01396h

A new, effective cloud-point extraction (CPE) method for determination of the pesticide, permethrin, from the pyrethroid group, in human urine, by high-pressure liquid chromatography with UV spectrophotometric detection, was developed and validated. The key extraction conditions were as follows: surfactant 5% (w/v) Triton X-114, temperature and incubation time of 40 °C and 30 min, respectively, and 100 μL organic solvent (acetonitrile) for dissolving the micellar phase. The acetonitrile micellar phase with the isolated permethrin was analyzed by reverse-phase high-pressure liquid chromatography using the gradient flow of a mobile phase consisting of water and acetonitrile. The main analytical parameters of the developed method were mean extraction recovery (89.9%), intra- (7.1, 9.1 and 13.6% RSD for 0.25, 0.5 and 1.0 μg mL −1 concentrations of permethrin, respectively) and interday (6.1, 10.3 and 14.1% RSD for 0.25, 0.5 and 1.0 μg mL −1 concentrations of permethrin, respectively) repeatability, limit of detection (0.025 μg mL −1 ) and limit of quantification (0.075 μg mL −1 ), as well as the linear range (0.075-2.000 μg mL −1 , r 2 = 0.9975). The evaluated parameters have enabled the proposed method to be hopefully useful for the monitoring of permethrin in urine samples taken from individuals exposed to this pesticide. A new, effective cloud-point extraction method for the determination of permethrin in human urine was developed.