Zinc oxide–aluminum oxide nanocomposite solid phase microextraction for diazepam and oxazepam trace determination

Abstract

A new efficient ZnO-Al2O3 nanocomposite (ZANC) was synthesized to form solid-phase microextraction (SPME) fiber. The prepared fiber was used for trace determination of benzodiazepines by gas chromatography-flame ionization detector in urine samples. The effective parameters on the extraction process including extraction time, salt percentage, desorption time and sample pH were optimized by a factorial design method.The method was evaluated at the optimum conditions and limits of detection (LODs) were calculated 20 µg/L for diazepam and oxazepam. The method repeatability for oxazepam and diazepam (50 µg/L, n = 4) was calculated at 8.8 % and 6.4 %. Also, the method reproducibility was obtained, 7.45 % and 6.61 % for oxazepam and diazepam (50 µg/L, n = 4). Also, fiber-to-fiber relative standard deviation (RSDs%) for the target analytes were less than 15.5 %. The method linearity is within the range of 62–500 µg/L for diazepam and oxazepam. The ZANC-SPME fiber showed a good lifetime (60 times) with high chemical stability. The high thermal stability of ZANC-SPME fiber was attained at 280 °C. The extraction results of poly dimethylsiloxan/divinyl benzene (PDMS/DVB) fiber were compared by ZANC-SPME fiber. Therefore, the method is proposed as a suitable technique for benzodiazepines detection in the urine sample.