Zirconium oxide/titanium oxide nanorod decorated nickel foam as an efficient sorbent in syringe filter based solid-phase extraction of pesticides in some vegetables

In the present study, an interesting, rapid and innovative syringe filter solid-phase extraction method was developed based on the novel sorbent of zirconium oxide/titanium oxide nanorod decorated over nickel foam (ZrO2-TiO2 NR @Ni foam SF-SPE). The extraction process was conducted based on a pulled-up and pushed-down process. The proposed ZrO2-TiO2 NR @Ni foam was prepared based on one-pot method and accordingly SEM, EDX and FT-IR techniques were utilized for characterization. The main parameters which affect the extraction process including pH, the number of sample solution pulled-pushed times, ionic strength, sample volume, elution solvent type and volume on the extraction efficiency of the target pesticides were investigated via matrix match method in samples. Under the optimum condition using matrix match strategy, the linear range of 5-400 mu g kg -1, LODs and LOQs in the range of 0.45-0.55 mu g kg- 1 and 1.52-1.76 mu g kg- 1 for cucumber and 0.36-0.54 mu g kg- 1 and 1.23-1.75 mu g kg -1 for tomato were achieved. The intra-day and inter-day precisions were evaluated at two different concentration levels (50 and 100 mu g kg-1 of each analyte) on the same day and five distinct days respectively. The obtained RSD (%) values were <= 3.7 % for intra-day (n = 7) and <= 4.2 % inter-day (n = 5) precisions. The relative recoveries of 91.8-99.1 % were acquired which confirmed high potential of the method in simultaneous extraction of the pesticides in cucumber, tomato.

Automated summary

A rapid and innovative syringe filter solid-phase extraction method using zirconium oxide/titanium oxide nanorod decorated over nickel foam (ZrO2-TiO2 NR @Ni foam) as the sorbent was developed. The extraction process involved a pulled-up and pushed-down process. The optimized conditions achieved a linear range of 5-400 μg/kg, LODs and LOQs ranging from 0.45-0.55 μg/kg and 1.52-1.76 μg/kg for cucumber, and 0.36-0.54 μg/kg and 1.23-1.75 μg/kg for tomato. The intra-day and inter-day precisions were satisfactory with RSD values below 3.7% and 4.2%, respectively. The method showed high potential for simultaneous extraction of pesticides in cucumber and tomato with relative recoveries of 91.8-99.1%.