GNP/Al-MOF nanocomposite as an efficient fiber coating of headspace solid-phase micro-extraction for the determination of organophosphorus pesticides in food samples.

The synthesis and utilization of a high porous nanocomposite comprising MIL-53(Al) metal-organic framework (Al-MOF) and graphene nanopowder (GNP) is reported as a fiber coating for headspace solid-phase micro-extraction (HS-SPME) of selected organophosphorus pesticides (OPPs) from apple, potato, grape juice, tomato, and river water. The adsorbed OPPs on the coated fiber were subsequently determined using GC-MS. Several parameters affecting the efficiency of extraction including time and temperature of extraction, desorption condition of extracted analytes, pH and agitation of sample solution, and salt concentration were investigated. The optimum extraction condition was achieved at 70 °C with an extraction time of 40 min, pH = 4-8, and NaCl concentration of 6.0% (w/v). The best condition of desorption were observed at 280 °C for 2.0 min under a flow of helium gas in the GC inlet. Under optimal conditions, the detection limits ranged from 0.2 to 1.5 ng g-1 and the linear ranges between 0.8 and 600 ng g-1. The proposed method showed very good repeatability with RSD values ranging from 4.5 to 7.3% (n = 5). The relative recoveries were between 88% and 109% at the spiked level of 25.0 ng g-1 for the tomato sample. The fabricated fiber exhibited good enrichment factor (62-195) at optimum condition of HS-SPME. The applied HS-SPME technique is facile, fast, and inexpensive. The thermally stable GNP/Al-MOF exhibited a high sensitivity toward OPPs. So, this nanocomposite can be considered as a sorbent for the micro-extraction of other pesticides in food.

Development of a SPE/GC-MS method for the determination of organophosphorus pesticides in food samples using syringe filters packed by GNP/MIL-101(Cr) nanocomposite.

In this study, we report the synthesis and application of a nanocomposite comprising metal-organic framework MIL-101(Cr) and graphene nanopowder (GNP) as a promising sorbent for the extraction of organophosphorus pesticides (OPPs) in juices, water, vegetables and honey samples. A syringe filter, for the first time, was used to host the synthesized nanocomposite and extract the OPPs followed by GC-MS analysis. Different characterization methods including XRD, FTIR, TGA, BET and SEM were employed to confirm the formation of studied nanocomposite. The results indicated that the GNP/MIL-101(Cr) could provide higher capacity for adsorption of OPPs and lower detection limit compared to pristine MIL-101(Cr). The detection limits were 0.005 to 15.0 µg/Kg and the linear range found between 0.05 and 400 µg/Kg. The proposed method showed very good repeatability with the RSD values ranging from 2.9% to 7.1%. The recoveries were between 84% -110% with the spiked levels of 2.0-100.0 µg/Kg.

MIL-53(Al)/Fe2O3 nanocomposite for solid-phase microextraction of organophosphorus pesticides followed by GC-MS analysis.

A novel aluminum terephthalate/Fe2O3 nanocomposite was synthesized by the addition of Fe2O3 nanoparticles into a reaction solution containing aluminum terephthalate MOF. The synthesized nanocomposite was successfully used as a fiber coating material for solid-phase microextraction (SPME) of six organophosphorus compounds (OPPs) from river water, grape juice, and tea samples. The effect of different parameters on the efficiency of SPME including desorption temperature and time, extraction temperature and time, salt concentration, pH, and agitation were thoroughly studied. The OPPs were detected and determined using GC-MS. According to the findings, a wide linear range (0.15-800 µg kg-1), low limit of detection (0.04-10 µg kg-1), and high recoveries from spiked samples (87.5-112%) were achieved with low inter-day relative standard deviation (3.2-6.7%, n = 5). The MIL-53(Al)/Fe2O3 nanocomposite showed  a high extraction ability towards OPPs, and hence, it can be considered a promising adsorbent for the extraction of various pesticides in complex matrices like tea and juice.Graphical abstract.

Colorimetric detection of glucose using lanthanum-incorporated MCM-41.

In this study, lanthanum-containing mesoporous MCM-41 (La-MCM-41) with different amount of lanthanum were synthesized and were used for colorimetric detection of glucose. As prepared La-MCM-41 were characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). The quantitative amounts of incorporated lanthanum into MCM-41 structure were estimated by energy dispersive X-ray spectrometry. The prepared La-MCM-41 provided high intrinsic peroxidase-like activity in the presence of peroxidise 3,3',5,5'-tetramethylbenzidine (TMB) and H2O2 for accurate determination of glucose. This process produced a blue color in aqueous solution that directly relates to H2O2 concentration. The effect of different parameters such as the content of incorporated lanthanum, pH, temperature and time of reaction on the peroxidase-like activity was studied. The colorimetric detection of H2O2 was led to a linear dynamic range from 50 to 1000 µM (r2 = 0.9988) and low detection limit of 37.5 µM for glucose in aqueous solution. These results are comparable (close to) or better than some previous reports. Thus, La-MCM-41 can be used as admirable alternative design for colorimetric sensing of glucose.

Nickel (II) incorporated AlPO-5 modified carbon paste electrode for determination of thioridazine in human serum.

In this approach, synthesis of nickel (II) incorporated aluminophosphate (NiAlPO-5) was performed by using hydrothermal method. The diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), and Fourier transform infrared spectroscopy (FTIR) techniques were applied in order to characterize synthesized compounds. The NiAlPO-5 was used as a modifier in carbon paste electrode for the selective determination of thioridazine which is an antidepressant drug. This research is the first example of an aluminophosphate being employed in electroanalysis. The effective catalytic role of the modified electrode toward thioridazine oxidation can be attributed to the electrocatalytic activity of nickel (II) in the aluminaphosphate matrix. In addition, NiAlPO-5 has unique properties such as the high specific surface area which increases the electron transfer of thioridazine. The effects of varying the percentage of modifier, pH and potential sweep rate on the electrode response were investigated. Differential pulse voltammetry was used for quantitative determination as a sensitive method. A dynamic linear range was obtained in the range of 1.0×10(-7)-1.0×10(-5)mol L(-1). The determination of thioridazine in real samples such as commercial tablets and human serum was demonstrated.