The main aim of the present study is the in-situ electrodeposition of Zn-Al-LDH on the surface of the conductive graphite pencil substrate together with the modification with ibuprofen. For this purpose, the electrodeposition method was employed using two electrode systems in the constant potential to produce Zn-Al-LDH on the surface of a pencil graphite substrate as working electrode. The electrochemically prepared Zn-Al-LDH will then be modified by ibuprofen [1]. The prepared modified adsorbent was used as the extracting fiber in the solid micro phase extraction (SPME) of selected drugs such as aspirin and naproxen from urine samples. The extracted analytes were eventually injected into the HPLC-UV for quantitative measurement and determination. In order to reach the maximum efficiency and obtain the optimal conditions for extraction of the selected analytes, the response surface methodology (RSM) was used. Based on the obtained results and the small RSD% (6.7%) for the method presented, it can be concluded that this absorbent has a high ability to pre-concentrations and selective extractions of testing analytes in biological samples.
