Chemometrics assisted dispersive liquid-liquid microextraction for quantification of seven UV filters in urine samples by HPLC-DAD

J Sep Sci. 2012 Dec;35(24):3575-85. doi: 10.1002/jssc.201200564.

Abstract

In the present study, dispersive liquid-liquid microextraction followed by high performance liquid chromatography-diode array detection has been developed as simple, rapid, accurate, and efficient sample preparation method for simultaneous determination of seven organic UV filters in urine samples. The influence of the main effects as well as their interactions was studied through a 2((6-2)) fractional factorial design. The candidate parameters were: type and volume of dispersant and extraction solvents, sample pH, and salt concentration. Under final optimal conditions, the analytes were extracted from 5 mL of samples by addition of 0.5 mL of acetonitrile (dispersing solvent) containing 70 μL of carbon tetrachloride (extraction solvent), without modifying the pH of the solution and applying the (+1) level of salt concentration (10% w/v NaCl). The assay was linear (R(2) > 0.997), relative recoveries ranged from 86.9 up to 97.3% and the LOQs between 3 and 45 ng mL(-1) were obtained. The intra- and interday RSDs were lower than 5 and 8% at the middle point of the linear range, respectively. The proposed method was successfully applied to different volunteer urine samples and it was shown that the extraction efficiency was not affected by the type of urine samples.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Chromatography, High Pressure Liquid / methods*
  • Humans
  • Hydrogen-Ion Concentration
  • Liquid Phase Microextraction / methods*
  • Spectrophotometry, Ultraviolet / methods*
  • Ultraviolet Rays*
  • Urinalysis*