title: Electrochemically controlled in-tube solid phase microextraction of naproxen from urine samples using an experimental design.
abstract: A new in-tube solid phase microextraction approach named electrochemically controlled in-tube solid phase microextraction (EC in-tube SPME) has been reported. In this approach, in which electrochemistry and in-tube SPME were combined, the total analysis time was decreased and the sensitivity was increased. After electropolymerization of pyrrole on the inner surface of a stainless steel tube, the polypyrrole (PPy)-coated in-tube SPME was coupled on-line to high performance liquid chromatography (HPLC) to achieve automated in-tube SPME-HPLC analysis. After the completion of the EC-in-tube SPME-HPLC system, the PPy-coated tube was used as a working electrode for the uptake of naproxen. It was found that the extraction efficiency could be significantly enhanced using the constant potential. Plackett-Burman design was employed for screening, to determine the variables significantly affecting the extraction efficiency. The significant factors were then optimized using a Box-Behnken design. The linear range and detection limit (S/N = 3) were 0.5-1000 and 0.07 μg L(-1), respectively. Urine samples were successfully analyzed by the proposed method.
authors.affiliation: Chemistry & Chemical Engineering Research Center of Iran, P.O. Box 14334-186, Tehran, Iran. ahmadi@ccerci.ac.ir.
authors.forename: Seyyed Hamid
authors.initials: SH
authors.lastname: Ahmadi
authors.forename: Ahmad
authors.initials: A
authors.lastname: Manbohi
authors.forename: Kourosh Tabar
authors.initials: KT
authors.lastname: Heydar
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D055664:Electrochemical Techniques / Q000379:methods*; D064368:Healthy Volunteers; D006801:Humans; D057230:Limit of Detection; D009288:Naproxen / Q000652:urine*; D011108:Polymers / Q000737:chemistry*; D011758:Pyrroles / Q000737:chemistry*; D052617:Solid Phase Microextraction / Q000379:methods*
chemical_list: D011108:Polymers; D011758:Pyrroles; C067635:polypyrrole; D009288:Naproxen