Rational design of heteropolyacid-based nanosorbent for hollow fiber solid phase microextraction of organophosphorus residues in hair samples

A novel heteropolyacid-based supported ionic liquid (IL) mediated sol–gel hybrid organic–inorganic material is presented for effective use in hollow fiber solid phase microextraction (HF-SPME). We examined a Keggin-based IL that was evaluated in conjunction with sol–gel. This study shows that Keggin-based IL sol–gel generated porous morphology pro effective extraction media. The method was developed for the extraction of the organophosphorus pesticides (OPs); diazinon, fenitrothion and malathion from human hair samples. The OPs were subsequently analyzed with high performance liquid chromatography and photodiode array detection (HPLC–PDA). In the basic condition (pH 10–11), the gel growth process in the presence of IL was initiated. Afterward, this sol was injected into a polypropylene hollow fiber segment for in situ-gelation process. Parameters affecting the efficiency of HF-SPME were thoroughly investigated. Linearity was observed over a range of 0.02–50,000 μg/g and 0.0001–25,000 ng/mL with detection limits between 0.0074–1.3000 μg/g and 0.00034–0.84 ng/mL for the OPs in hair and aqueous matrices, respectively. The relative recoveries in the real samples, for OPs in the storekeeper hair ranged from 86 to 95.2%.