Nickel hydroxide nanoflower-based dispersive solid-phase extraction of copper from water matrix.

In this work, a dispersive solid-phase extraction method based on Ni(OH)2 nanoflowers (Ni(OH)2-NFs-DSPE) was developed to separate and preconcentrate copper ions from tap water samples for determination by flame atomic absorption spectrometry (FAAS). Ni(OH)2-NFs was synthesized using a homogeneous precipitation technique and used as sorbent for copper preconcentration. X-ray diffraction, scanning electron microscopy, and Fourier-transform infrared spectroscopy were used to characterize the synthesized sorbent. All experimental variables were carefully optimized to achieve a high enhancement factor of 107.5-folds with respect to the detection sensitivity of the conventional FAAS. The proposed method's analytical parameters including LOD, LOQ, and linear range were determined as 1.33 µg/L, 4.42 µg/L, and 3.0-40 µg/L, respectively. To assess the applicability and reliability of the developed method, optimal conditions were applied to tap water samples and satisfactory percent recoveries (94-103%) were obtained for the samples spiked at 20 and 30 µg/L. This validated the accuracy and feasibility of the developed method to real samples. The developed method can be described as a simple, efficient, and rapid analytical approach for the accurate determination of trace copper ions in water samples.

Development and validation of dispersive liquid-liquid microextraction method for the determination of 15 polycyclic aromatic hydrocarbons in 200 Antarctica samples by gas chromatography mass spectrometry.

Antarctica has seen an increase in scientific research and tourism, and anthropogenic activities such as incineration of waste products and fuel combustion for energy and transportation are potential contamination sources to the ecosystem. Polycyclic aromatic hydrocarbons are common products of incomplete combustion of organic compounds and could be among accumulating contaminants in Antarctica. Thus, this study sought to develop a sensitive dispersive liquid-liquid microextraction method for the determination of 15 polycyclic aromatic hydrocarbons by gas chromatography mass spectrometry. Parameters that were relevant to the extraction method were carefully optimized and validated using aqueous standard solutions. The optimum method recorded detection limits in the range of 0.20-6.1 µg/L for the analytes. Spike recovery experiments were carried out on artificial seawater, rock-soil, and moss samples, using matrix matching calibration to mitigate effects of the sample matrices. The samples analyzed included seawater, lake, rock-soil, moss, seaweed, and feces samples all collected from the Horseshoe and Faure Islands in Antarctica. The percent recovery results obtained for the samples spiked at different concentrations ranged between 86 and 115%.

Removal of selected pesticides, alkylphenols, hormones and bisphenol A from domestic wastewater by electrooxidation process.

In this study, seven compounds of environmental and health concern were treated by electrooxidation to determine their removal efficiencies from domestic wastewater. A batch type lab-scale reactor was used for the treatment process, and the analytes studied included two obsolete pesticides, two alkylphenols, two hormones, and bisphenol A. Titanium oxide and graphite electrodes were used as anode and cathode, respectively. Parameters of the electrooxidation process including pH of wastewater, ionic strength, applied current and treatment period were optimized by the univariate approach to maximize the removal efficiency of the analytes from wastewater. The optimum conditions were determined as nonadjusted pH of wastewater, 1.5 A current, 15 min treatment period and 5.0 g/L sodium chloride. Dispersive liquid-liquid microextraction was used to preconcentrate analytes before and after treatment in order to calculate the removal efficiency of analytes. The removal efficiency obtained under the optimum conditions was satisfactory for all seven analytes at different influent concentrations.

Trace level determination of eleven nervous system-active pharmaceutical ingredients by switchable solvent-based liquid-phase microextraction and gas chromatography-mass spectrometry with matrix matching calibration strategy.

This study utilized switchable solvent liquid-phase microextraction (SS-LPME) to enrich eleven nervous system active pharmaceutical ingredients (APIs) from aqueous samples for their determination at trace levels by gas chromatography mass spectrometry. The analytes selected for the study included APIs utilized in antidepressant, antipsychotic, antiepileptic, and anti-dementia drugs. Parameters of the microextraction method including switchable solvent volume, concentration and volume of the trigger agent (sodium hydroxide), and sample agitation period were optimized univariately to boost extraction efficiency. Under the optimum conditions, the detection limits calculated for the analytes were in the range of 0.20-8.0 ng/mL, and repeatability for six replicate measurements as indicated by percent relative standard deviation values were below 10%. Matrix matching calibration strategy was used to enhance quantification accuracy for the analytes. The percent recovery results calculated for the eleven analytes ranged between 86 and 117%.

Surface modified iron magnetic nanoparticles assisted Fenton digestion and extraction method for cadmium determination.

This study presents a Fenton digestion method for milk samples based on UV irradiation for cadmium determination using flame atomic absorption spectrometry. The method was developed as an alternative to microwave digesters, using very basic apparatus and easy to acquire chemicals. Fenton digestion process was performed by the help of citric acid coated magnetic nanoparticles. Optimum conditions of the digestion process were applied to milk samples to evaluate analytical performance of the method. Limit of detection and limit of quantification values calculated for cadmium in milk were 0.53 and 1.8 mg/L, respectively. The method was applied to three different milk samples to validate the method's suitability and accuracy. Percent recovery values calculated for the samples spiked at two different concentrations ranged between 86 and 111%. Due to differences in the content of the spiked and control/standard milk samples, exact matrix matching calibration strategy using the same brand of milk sample in the preparation of calibration standard was employed and the accuracy of cadmium quantification was greatly enhanced (≈100%).

Experimental Design of Vortex Assisted Switchable Solvent Homogeneous Liquid-Liquid Microextraction for Simultaneous Determination of Four Pesticides in Wastewater.

BACKGROUND: Pesticides are chemicals used mainly to protect plant crops in order to increase their production efficiency and quality. OBJECTIVE: Switchable-solvent homogeneous liquid-liquid microextraction was optimized using a Box-Behnken experimental design and validated on a gas chromatography mass spectrometry system for the determination of analytes. METHOD: The significance of independent variables (switchable solvent volume, sodium hydroxide volume, and vortex period) and their interactions were evaluated by analysis of variance at 95% confidence limits (α = 0.05). RESULTS: The LOD and LOQ ranges of the analytes were found to be 0.42-1.90 µg/L and 1.36-6.33 µg/L, respectively. Percentage recovery results were found to be in the range of 87-113% in spiking experiments. CONCLUSIONS: A simple, efficient, and accurate analytical method was developed for the simultaneous determination of the selected pesticides. Highlights: Matrix matching was used to enhance quantification accuracy for real samples. HIGHLIGHTS: Matrix matching was used to enhance quantification accuracy for real samples.

Development of a sensitive and accurate method for the simultaneous determination of selected insecticides and herbicide in tap water and wastewater samples using vortex-assisted switchable solvent-based liquid-phase microextraction prior to determination by gas chromatography-mass spectrometry.

In this study, a switchable solvent-based liquid-phase microextraction method was developed to preconcentrate selected pesticides from tap water and wastewater matrices for determination by gas chromatography-mass spectrometry. A thorough optimization process was performed for prominent extraction parameters such as switchable solvent amount, concentration/amount of sodium hydroxide, salt type and mixing period. Optimum parameters obtained at the end of the optimization process were applied to aqueous standard solutions to validate the method. The linear dynamic ranges of all four analytes were appreciably wide with coefficient of determination values greater than 0.9997. The limits of detection and quantification (LOD and LOQ) were calculated for the analytes in the ranges of 0.38-2.0 ng/mL and 1.3-6.5 ng/mL, respectively. Spiked recovery experiments were used to validate the accuracy of the developed method and to determine the performance of the method in different sample matrices. Tap water, municipal wastewater and medical wastewater were spiked at three different concentrations and analyzed under the method's optimum conditions. The percent recovery results calculated for the samples were in the range of 79-107%, and this validated the method's accuracy and applicability to complex matrices such as municipal and medical wastewater samples.

Combination of vortex assisted binary solvent microextraction and QuEChERS for the determination of prothiofos, oxadiargyl, and gamma-cyhalothrin in water and pineapple samples by gas chromatography mass spectrometry.

An accurate and sensitive dispersive liquid-liquid microextraction method based on binary solvents was used to enrich prothiofos, oxadiargyl, and gamma-cyhalothrin for quantification by GC-MS. The combination of two extraction solvents (binary mixture) resulted in higher extraction efficiencies compared to the single solvent extraction systems. Parameters of the binary extraction method where optimized to enhance the extraction output of the analytes. The limits of detection calculated for the analytes ranged between 0.59 and 1.6 ng/mL. Linear calibration plots of the analytes covered wide concentration ranges with R2 values greater than 0.9996 and percent relative standard deviation lower than 10%. Spiked recovery experiments were performed well and wastewater at two different concentrations and satisfactory results (89-104%) were obtained. The binary solvent microextraction method was combined with QuEChERS to quantify the analytes in pineapple matrix, using matrix matching method to enhance the accuracy of the method to almost 100%.

Dispersive liquid-liquid microextraction based preconcentration of selected pesticides and escitalopram oxalate, haloperidol and olanzapine from wastewater samples prior to determination by GC-MS.

A multivariate experimental design was used to attain optimum conditions of a dispersive liquid-liquid microextraction (DLLME) method for preconcentration of pesticides and pharmaceuticals for determination by gas chromatography mass spectrometry (GC-MS). Experimental design enabled parameters to be evaluated for their effects on extraction output as well as their interactive effects. The optimum parameters suggested by the design model were 200 µL of chloroform, 1.96 mL of ethanol and 40 s vortexing period. Limits of detection and quantification (LOD and LOQ) were calculated using linear calibration plots of the analytes developed in the standard concentration range of 2.0 µg/L-2.0 mg/L. Enhancement in detection power of the analytes recorded by the optimized method with respect to direct GC-MS determination (based on LOD values) was in the range of 3.6 and 539 folds. Spiked recovery experiments for municipal, medical and synthetic wastewater samples yielded low recovery results when calculated against aqueous standard solutions. Matrix matched calibration standards were used to mitigate interferences from the waste samples, and the percent recoveries obtained were close to 100%. This established accuracy and applicability of the developed method.