Background: Solid-phase microextraction (SPME) is a simple and
rapid extraction method that was introduced by Pawliszyn. During the ages significant
developments were made in fiber types in order to overcome the traditional
SPME fibers limitations.
Objective: In this project, a new application of a solid sorbent was introduced for
head-space SPME (HS-SPME) determination of phenolic compounds. In this
sorbent, MWCNTs were covalently functionalized and were attached chemically
to the PDMS by the sol-gel method. Moreover, ionic liquids were used as porogenic
agents in order to increase the fiber porosity.
Method: HS-SPME mode was used for analytes determination. The most important affecting parameters
on method’s efficiency were investigated and optimized.
Results: At the optimized conditions, linear ranges were from 0.002-200 ng mL-1 with limits of detection
(LODs) from 0.0005 to 0.005 ng mL-1 and limits of quantitation (LOQs) between 0.002-0.02
ng mL-1. Two different relative standard deviations (RSDs) were defined and calculated at three different
concentrations (0.05, 2 and 100 ng mL-1). The first RSDs were for one fiber (repeatability) that
were from 4.6 up to 6.7%. The secondary RSDs were between different fibers (reproducibility) that
were from 5.7 to 7.8%.
Conclusion: The prepared fiber showed high thermal stability (over than 320 °C) with good lifespan
(more than 210 times). Eventually, the phenolic compounds were determined in the real urine samples
with this method. According to our results, the proposed method showed acceptable relative recovery
percentages between 90.7 to 102.1% for the spiked urine samples at 0.5 ng mL-1.