Fe3O4-SiO2-MIL-53 (Fe) nanocomposite for magnetic dispersive micro-solid phase extraction of cadmium (II) at trace levels prior to HR-CS-FAAS detection.

A magnetic metal-organic framework Fe3O4-SiO2-MIL-53 (Fe) nanocomposite was synthesized for magnetic dispersion micro-solid phase extraction (M-d-µSPE) of cadmium in water, spice, chocolate, tea, and tobacco samples prior to the detection by flame atomic absorption spectrometry. Fe3O4-SiO2-MIL-53 (Fe) nanocomposite fabricated using the solvothermal technique was characterized using a field emission scanning electron microscope and X-ray diffraction. The extraction efficiency of the method was improved by optimizing the experimental factors. After optimization, the linearity range for Cd (II) was 4.3-500 µgL-1. The limits of detection and quantification were 1.3 and 4.3 µgL-1, respectively. The presented magnetic dispersion-micro solid phase extraction method was applied to Cd (II) analysis in food and some environmental samples.

Assessment of environmental pollutants at trace levels using ionic liquids-based liquid-phase microextraction.

Sample preparation is the crucial and most challenging part of analytical chemistry for the speciation of environmental pollutants' traces. Along with the development of the sample preparation methods, the ionic liquid-based microextraction technique plays an important role. Due to the unequivocally unique "green" characteristic of ionic liquids (ILs), they owe their tunable properties, such as highly selective and high reaction efficiency, reusability, and good thermal stability, to present advancements in the sample preparation process. The ionic liquid-based microextraction techniques miniaturize the sample preparation process. Liquid phase microextraction intermediate solvents, desorption solvent extractants, and mediators have been used. They are quoting the benefits and limitations of each method. A few essential sample preparation methods covered the microextraction technique. In this context, miniaturized microextraction methods have been developed. They are generally used for their unlimited positive features, including easy, simple, and environmentally friendly; they also extract inorganic and organic species with low-cost instrumentation. This review advances the sample preparation process using ILs-based liquid phase microextraction as an intermediate solvent, extractant desorption, and mediator solvents.

Dual-response electrochemical electrode for sensitive monitoring of topotecan and mitomycin as anticancer drugs in real samples.

This research paper employed an innovative electrochemical electrode to simultaneously determine topotecan (TPT) and mitomycin (MMC) as anticancer agents. For this purpose, a novel nanocomposite was synthesized using a hydrothermal procedure. The nanocomposites were characterized using FTIR, STEM, FESEM, mapping analysis, EDX, and XRD methods. The novelty of this work is the successful synthesis of Fe3O4 decorated on the surface of CuCo2S4 (Fe3O4@CuCo2S4) nanocomposites showed two separate anodic peaks at 0.8 V for TPT and 1.0 V for MMC with potential separation of 0.2 V. This was enough for the simultaneous electrochemical determination of topotecan and mitomycin on a glassy carbon electrode (GCE), simultaneously. At optimized conditions, the developed electrode exhibited linear responses with TPT and MMC concentration in the ranges of 0.01-0.89 and 0.89-8.95 µM for topotecan and 0.1-19.53 µM for mitomycin. The detection limits were observed as 6.94 nM and 80.00 nM for topotecan and mitomycin, respectively. The fabricated Fe3O4@CuCo2S4/GCE showed high sensitivity, long-term stability, and repeatability towards the sensing of TPT and MMC simultaneously and can be utilized in real samples. The obtained results confirmed that the fabricated Fe3O4@CuCo2S4/GCE nanocomposites can be utilize in the simultaneous electrochemical determination of topotecan and mitomycin in real samples.

Sample Preparation Methods for Metal Containing Pesticides in Food and Environmental Samples.

Metal-containing pesticides are used in many areas for purposes such as harvest efficiency and keeping pests away from the vegetable environment. Metal-containing pesticides are in the form of dithiocarbamate complexes and are named differently according to the type of metal they contain and are used for different purposes. Since the presence of these pesticides even at residue level threatens human and environmental health, their determination at trace level is important. In this review, studies on the determination of metal-containing dithiocarbamate pesticides in different matrices are discussed. This review on the analysis of dithiocarbamate pesticides with different techniques will shed light on the studies to be carried out for the determination of these pesticides one by one in different matrices.

Switchable-hydrophilicity solvent liquid-liquid microextraction prior to magnetic nanoparticle-based dispersive solid-phase microextraction for spectrophotometric determination of erythrosine in food and other samples.

A combination of switchable-hydrophilicity liquid-liquid microextraction prior to magnetic nanoparticle-based dispersive solid-phase microextraction is proposed for the determination of erythrosine using UV/Vis spectrophotometry at 520 nm. Under optimum conditions (i.e., 1.0 mL octylamine as the extraction solvent, 1.5 mL of 10.0 M sodium hydroxide as the phase separation trigger, pH 4.0, 750 µL of acetone as the eluent, 10.0 mg of Fe3O4@XAD-16 as the adsorbent, and 15.0 mL of the sample solution), the method showed a superior analytical performance with limits of detection less than 25.9 ng mL-1, limits of quantitation less than 86.3 ng mL-1 and linear dynamic ranges ranging between 86.3 and 1000 ng mL-1. Percentage relative standard deviations were less than 4.1 and 7.2% for intra-day and inter-day, respectively. The method was successfully applied for the extraction and determination of erythrosine in food samples and other consumer products with recoveries in the range of 94.6-103.9% and within extraction time of 7.8 min per sample.

Ultrasound assisted supramolecular liquid phase microextraction procedure for Sudan I at trace level in environmental samples.

A method based on supramolecular liquid phase microextraction has been developed for the preconcentration and determination of trace levels of Sudan I. 1-decanol and tetrahydrofuran were used as supramolecular solvent components. Trace levels of Sudan I were extracted into the extraction solvent phase at pH = 4.0 Analytical parameters such as pH value, supramolecular solvent volume, ultrasonication, centrifugation, model solution volume, matrix effects have been optimized. The limit of detection and the limit of quantification values for Sudan I were calculated as 1.74 µg L-1 and 5.75 µg L-1, respectively. In order to determine the accuracy of the method, addition and recovery studies were carried out to environmental samples.

Application of magnetic nanomaterials in bioanalysis.

The importance of magnetic nanomaterials and magnetic hybrid materials, which are classified as new generation materials, in analytical applications is increasingly understood, and research on the adaptation of these materials to analytical methods has gained momentum. Development of sample preparation techniques and sensor systems using magnetic nanomaterials for the analysis of inorganic, organic and biomolecules in biological samples, which are among the samples that analytical chemists work on most, are among the priority issues. Therefore in this review, we focused on the use of magnetic nanomaterials for the bioanalytical applications including inorganic and organic species and biomolecules in different biological samples such as primarily blood, serum, plasma, tissue extracts, urine and milk. We summarized recent progresses, prevailing techniques, applied formats, and future trends in sample preparation-analysis methods and sensors based on magnetic nanomaterials (Mag-NMs). First, we provided a brief introduction of magnetic nanomaterials, especially their magnetic properties that can be utilized for bioanalytical applications. Second, we discussed the synthesis of these Mag-NMs. Third, we reviewed recent advances in bioanalytical applications of the Mag-NMs in different formats. Finally, recently literature studies on the relevance of Mag-NMs for bioanalysis applications were presented.