Simultaneous extraction and preconcentration of aniline, phenol, and naphthalene using magnetite-graphene oxide composites before gas chromatography determination.

The coextraction of acidic and basic compounds from different mediums is a significant concept in sample preparation. In this work, simultaneous extraction of acidic, basic, and neutral analytes in a single step was carried out for the first time. This procedure employed the dispersive solid-phase microextraction of analytes with magnetic graphene oxide (graphene oxide/Fe3 O4 ) sorbent followed by gas chromatography with flame ionization detection. After the adsorption of analytes by vortexing and decantation of the supernatant with a magnet, the sorbent was eluted with acetonitrile/methanol (2:1) mixture. The parameters affecting the extraction efficiency were optimized and obtained as follows: sorbent amount 60 mg, desorption time 1 min, extraction time 5 min, pH of the sample 7, sample volume 20 mL, and elution solvent volume 0.3 mL. Under the optimum conditions, linear dynamic ranges were achieved in the range of 0.5-4, 0.25-4, and 0.25-2 µg/mL and limits of detection were 0.341, 0.110, and 0.167 µg/mL for aniline, phenol, and naphthalene, respectively. The relative standard deviations were in the range of 3.3-5.7% in eight repeated extractions. Finally, the applicability of the method was evaluated by the extraction and determination of analytes in stream water and drinking water samples and satisfactory results were obtained.

Silane modified magnetic nanoparticles as a novel adsorbent for determination of morphine at trace levels in human hair samples by high-performance liquid chromatography with diode array detection.

In this paper we report a novel, sensitive, and rapid method of magnetic solid phase extraction based on surface modified magnetic nanoparticles as a novel nano sorbent for HPLC determination of morphine with diode array detection in human hair samples. Factors affecting the extraction efficiency of the proposed method, including the sample pH, quantity of magnetic nanoparticles, sample volume, desorption solvent type and its volume, and extraction time were investigated and optimized. Under the optimized experimental conditions, a good linearity was observed in the range of 1-800 µgL(-1) for the morphine, with a correlation coefficient (R (2)) of 0.990. The pre-concentration factor of 208.69 was achieved in this method. The detection limit of the method was 0.1 µgL(-1) based on S/N = 3 and good reproducibility with a relative standard deviations lower than (n = 5) 2.59 %. The proposed method has been successfully applied to the analysis of trace amounts of morphine in human hair samples with satisfactory results. This method can be applied in medical toxicology research and forensic medical centers.

Fabrication of a novel nanocomposite based on sol-gel process for hollow fiber-solid phase microextraction of aflatoxins: B1 and B2, in cereals combined with high performane liquid chromatography-diode array detection.

The new pre-concentration technique, hollow fiber-solid phase microextraction based on carbon nanotube reinforced sol-gel and liquid chromatography-photodiode array detection was applied to determination of aflatoxins B(1), B(2) (AFB(1), AFB(2)) in rice, peanut and wheat samples. This research provides an overview of trends related to synthesis of solid phase microextraction (SPME) sorbnents that improves the assay of aflatoxins as the semi-polar compounds in several real samples. It mainly includes summary and a list of the results for a simple carbon nanotube reinforced sol-gel in-fiber device. This device was used for extraction, pre-concentration and determination of aflatoxins B1, B2 in real samples. In this technique carbon nanotube reinforced sol was prepared by the sol-gel method via the reaction of phenyl trimethoxysilane (PTMS) with a basic catalyst (tris hydroxymethyl aminomethan). The influences of microextraction parameters such as pH, ageing time, carbon nanotube contents, desorption conditions, desorption solvent and agitation speed were investigated. Optimal HPLC conditions were: C(18) reversed phase column for separation, water-acetonitril-methanol (35:10:55) as the mobile phase and maximum wavelength for detection was 370 nm. The method was evaluated statistically and under optimized conditions, the detection limits for the analytes were 0.074 and 0.061 ng/mL for B1 and B2 respectively. Limit of quantification for B1 and B2 was 0.1 ng/mL too (n=7). The precisions were in the range of 2.829-2.976% (n=3), and linear ranges were within 0.1 and 400 ng/mL. The method was successfully applied to the analysis of cereals (peanut, wheat, rice) with the relative recoveries from 47.43% to 106.83%.

The measurement of ecstasy in human hair by triple phase directly suspended droplet microextraction prior to HPLC-DAD analysis.

New pre-concentration technique, triple phase suspended droplet microextraction (SD-LPME) and liquid chromatography-photodiode array detection was applied to determine ecstasy, MDMA (3,4-methylendioxy-N-methylamphetamine) in hair samples. In this research MDMA in hair was digested and after treatment extracted. The effective parameters were investigated and method was evaluated. Under the optimal conditions, the MDMA was enriched by factor 98.11. Linearity (r=0.9921), was obtained in the range of 10-15,000 ng mL(-1) and detection limit was 0.1 ng mL(-1).