Spectrophotometric Determination of Paracetamol in Urine with Tetrahydroxycalix[4]arene as a Coupling Reagent and Preconcentration with Triton X-114 Using Cloud Point Extraction

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概要

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• In the present paper, conventional spectrophotometry in conjunction with cloud point extraction-preconcen-tration were investigated as alternative methods for paracetamol (PCT) assay in urine samples. Cloud point extraction (CPE) was employed for the preconcentration of p-aminophenol (PAP) prior to spectrophotometric determination using the non-ionic surfactant Triton X-114 (TX-114) as an extractant. The developed methods were based on acidic hydrolysis of PCT to PAP, which reacted at room temperature with 25,26,27,28-tetrahydroxycalix[4]arene (CAL4) in the presence of an oxidant (KIO_4) to form an blue colored product. The PAP-CAL4 blue dye formed was subsequently entrapped in the surfactant micelles of Triton X-114. Cloud point phase separation with the aid of Triton X-114 induced by addition of Na_2SO_4 solution was performed at room temperature as an advantage over other CPE assays requiring elevated temperatures. The 580nm-absorbance maximum of the formed product was shifted bathochromically to 590nm with CPE. The working range of 1.5-12μg ml^<-1> achieved by conventional spectrophotometry was reduced down to 0.14-1.5μg ml^<-1> with cloud point extraction, which was lower than those of most literature flow-through assays that also suffer from nonspecific absorption in the UV region. By preconcentrating 10ml sample solution, a detection limit as low as 40.0ng ml^<-1> was obtained after a single-step extraction, achieving a preconcentration factor of 10. The stoichiometric composition of the dye was found to be 1:4 (PAP:CAL4). The impact of a number of parameters such as concentrations of CAL4, KIO_4, Triton X-100 (TX-100), and TX-114, extraction temperature, time periods for incubation and centrifugation, and sample volume were investigated in detail. The determination of PAP in the presence of paracetamol in micellar systems under these conditions is limited. The established procedures were successfully adopted for the determination of PCT in urine samples. Since the drug is rapidly absorbed and excreted largely in urine and its high doses have been associated with lethal hepatic necrosis and renal failure, development of a rapid, sensitive and selective assay of PCT is of vital importance for fast urinary screening and antidote administration before applying more sophisticated, but costly and laborious hyphenated instrumental techniques of HPLC-SPE-NMR-MS.

• 2006-06-01

著者

• Cekic Sema

  Department Of Chemistry Faculty Of Engineering Istanbul University

• Apak Resat

  Department Of Chemistry Faculty Of Engineering Istanbul University

• Kilic Emine

  Department Of Chemistry Faculty Of Science Ankara University

• FILIK Hayati

  Department of Chemistry, Faculty of Engineering, Istanbul University

• SENER Izzet

  Department of Chemistry, Faculty of Science and Arts, Pamukkale University

• Sener Izzet

  Department Of Chemistry Faculty Of Science And Arts Pamukkale University

• Filik Hayati

  Department Of Chemistry Faculty Of Engineering Istanbul University

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