Implementation of simple and effective fine droplet formation-based spray-assisted liquid phase microextraction for the simultaneous determination of twenty-nine endocrine disruptor compounds and pesticides in rock, soil, water, moss, and feces samples from antarctica using gas chromatography-mass spectrometry.

This study established the simultaneous determination of the selected endocrine-disrupting compounds (EDCs) and pesticides in rock, soil, water, moss, and feces samples collected from the Antarctic region. The spray-assisted droplet formation-based liquid phase microextraction (SADF-LPME) coupled to GC-MS system was developed and validated for the screening and monitoring of 29 selected EDCs and pesticides. Binary solvent system, 1:1 (v/v) dichlormethane: 1,2-dichloroethane mixture was employed as an extraction solvent and sprayed onto sample or standard solutions using a straightforward and practical spray apparatus. The factors affecting the extraction process such as extraction solvent type and ratio, extraction solvent volume (spray repetition), vortexing period, and sample pH were properly optimized. Analytical figures of the merit of the method were recorded under the optimal extraction/chromatographic conditions. The LOD, LOQ, and enhancement factor were in the range of 1.0 to 6.6 ng/g, 3.2 to 22.1 ng/g, and 3.7 to 158.9, respectively. The method demonstrated a good linear working range for all the selected analytes with proper coefficients of determination. The usability and reliability of the microextraction strategy was confirmed using seawater, moss, and soil samples, and the %recoveries were within an acceptable range (> 70%) for all examined samples. The environmental samples collected from the Horseshoe and Faure Islands of the Antarctica region were analyzed to assess the potential pollution of EDCs and pesticides. This method has the potential to be employed for the analysis of EDCs in routine analytical laboratories and for controlling and screening the organic pollutant content of different environmental samples.

Quantification of palladium in wastewater samples by matrix-matching calibration strategy assisted deep eutectic solvent based microextraction.

An efficient, sensitive, and easy deep eutectic solvent based (DESb) liquid phase microextraction (LPME) method was developed to preconcentrate palladium for quantification at trace level by a flame atomic absorption spectrometry (FAAS) system, equipped with a lab made slotted quartz tube (SQT). All parameters of the DESb-LPME-SQT-FAAS system were optimized to lower the detection limit of the system. Using the optimized conditions, quantification and detection limits were obtained as 24.7 and 7.4 µg L-1, respectively, which are compatible with the literature findings. Detection power of the FAAS system was enhanced by almost 50-fold using the optimum method based on LOD comparison. Recovery experiments were also performed with spiked wastewater matrix to examine the applicability/validity of the proposed method. The % recovery results were calculated between 85 and 91%. This established that the applicability of the developed method is high, and determination of this element in complex matrix can be performed accurately using the developed method.

A basic and effective liquid phase microextraction with a novel automated mixing system for the determination of cobalt in quince samples by flame atomic absorption spectrometry.

A new, green, and simple liquid-phase microextraction method namely sieve conducted two syringe-based pressurized liquid-phase microextraction methods was combined with flame atomic absorption spectrometry for the preconcentration and determination of cobalt. For this aim, a novel automated syringe mixing system was developed to be used in the developed extraction procedure. Two syringes were connected to each other by an apparatus having six holes to produce efficient dispersion of the extractant. The pressure created between the two syringes by the forward and backward movements of the syringe plungers created an efficient dispersion of the extractant. In the present study, ligand as complexing agent was synthesized in our laboratory. Limits of detection and quantification were determined to be 1.8 and 6.0 µg L-1, respectively. A 33.7-fold enhancement in detection power was obtained with the developed method. Method was effectively applied for the determination of cobalt in quince samples.

An accurate and sensitive effervescence-assisted liquid phase microextraction method for the determination of cobalt after a Schiff base complexation by slotted quartz tube-flame atomic absorption spectrophotometry in urine samples.

In this study, an accurate analytical method development for cobalt determination in urine samples was described. The method is based on the mass transfer of the target analytes to the organic phase from the aqueous phase by the dispersing extractant throughout the solution with the aid of CO2 bubbles prior to sample measurement by using a slotted quartz tube flame atomic absorption spectrophotometer. An extractor (1-decanol) dropped effervescent tablet (anhydrous sodium carbonate and sodium dihydrogen phosphate dihydrate mixture) was used in order to separate/preconcentrate cobalt after complexation of cobalt ions in aqueous solution with the Schiff base ligand. The parameters affecting the extraction output such as complexing conditions (pH, ligand concentration, and volume) and extraction conditions (extraction solvent type and volume, extraction temperature, and heating duration, NaOH volume and mixing period) were optimized to lower the detection limit. The limit of detection and quantification values under optimized experimental and instrumental conditions were determined as 3.7 µg L-1 and 12 µg L-1, respectively with high linearity with respect to the dynamic range between 15 and 300 µg L-1. The enhancement factor obtained with the developed method was calculated as 83 fold. The pretreatment process was applied to urine samples in order to test the convenience of the developed method in urine samples for the determination of cobalt at low levels. The high percentage recovery results of 96-97% for four different concentrations of spiked urine samples indicated the proposed method's sufficient sensitivity for analyte determination in such a complex matrix.

A green, accurate and sensitive analytical method based on vortex assisted deep eutectic solvent-liquid phase microextraction for the determination of cobalt by slotted quartz tube flame atomic absorption spectrometry.

Preconcentration of cobalt was carried out with deep eutectic solvent based liquid phase microextraction (DES-LPME) for trace determination by a slotted quartz tube (SQT) attached flame atomic absorption spectrometry (FAAS) system. Choline chloride and phenol in a 1:2 M ratio was used as a green solvent to extract cobalt from the aqueous sample solution. Key parameters influencing the extraction efficiency of cobalt were examined and optimized. Under the conditions optimized, the linear dynamic range was found between 5.0 and 50 µg L-1, and the limits of detection and quantification (LOD and LOQ) were calculated as 2.0 and 6.6 µg L-1, respectively. The detection power of the conventional FAAS was improved upon by 67 folds using the optimized DES-LPME-SQT-FAAS method. The developed analytical method was successfully applied for the determination of cobalt in linden tea samples and the recovery results obtained for different spiked concentrations (20, 30 and 40 µg L-1) were remarkable (≈100%).

In Vitro Cytotoxicity Studies on Human Thyroid Gland Undifferentiated Carcinoma Cells Using the Nickel Complex of (Z)-3-Bromo-5-((p-tolylimino)methyl)phenol.

Metal complexes for medical applications are the promising area of research and metallo-drugs have been developed and evaluated to enhance the efficiency of drugs and minimize their side effects. This study describes the synthesis of a Schiff base ligand (Z)-3-bromo-5-((p-tolylimino)methyl)phenol from the reaction of 5-bromosalicilaldehyde and p-toluidine, and its subsequent complexation with nickel. Characterization and cell viability studies were performed for both Schiff base ligand and its metal complex with 1H-NMR, FTIR, TG analysis, and UV-VIS spectrometry. With the aim of proving the Ni complex formation, quantitative analysis was done with flame atomic absorption spectrometry. The recovery result obtained for the formed complex was 103.9%. The cell viability of human thyroid gland undifferentiated carcinoma cells (8305C) treated with the Ni-ligand complex was determined as 12.7 ± 0.17%. It was observed that the nickel complex could be a significant anticancer agent as tested by the MTT assay method. Graphical Abstract .

An accurate and sensitive analytical strategy for the determination of palladium in aqueous samples: slotted quartz tube flame atomic absorption spectrometry with switchable liquid-liquid microextraction after preconcentration using a Schiff base ligand.

This study presents a green analytical method for palladium determination by slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) following switchable liquid-liquid microextraction (SLLME). Efficient extraction of palladium was facilitated by complexation with a Schiff base ligand, synthesized specifically for this study. A three-stage thorough optimization procedure was carried out to boost the absorbance output of palladium. Complex formation was the first stage, and parameters evaluated included buffer solution pH and amount, concentration of ligand, and mixing period. The amount of switchable solvent and concentration and amount of sodium hydroxide and acid amount were optimized in the second stage. Optimization of sample and fuel flow rates and SQT parameters completed the third stage of optimization, and all optimum parameters were used to determine analytical performance of the method. The method had a broad linear dynamic range, and the calibration plots showed good linearity with R2 values greater than 0.9991. The limits of detection and quantification of the SLLME-SQT-FAAS method were 15 and 50 µg/L, respectively. The precision of the method, expressed as percent relative standard deviation, was below 9.0% for all measurements. Spiked recovery results performed for a palladium electroplating bath solution gave poor results when quantified against aqueous calibration standards. Matrix matching was therefore used to improve recovery results which ranged between 97 and 105% for four different spike concentrations.

Trace determination of nickel in water samples by slotted quartz tube-flame atomic absorption spectrometry after dispersive assisted simultaneous complexation and extraction strategy.

This study presents a new method for the determination of nickel in aqueous samples by slotted quartz tube-flame atomic absorption spectrometry (SQT-FAAS) after a dispersive assisted simultaneous complexation and extraction (DASCE) process. Synthesized ligand was directly dissolved in the extraction solvent to eliminate the complex formation step prior to the extraction. All parameters of the SQT-FAAS and DASCE method were systematically optimized to improve the detection power of nickel for trace determinations. Under the optimum experimental conditions, the optimized method (DASCE-SQT-FAAS) recorded 137-fold enhancement in detection power over the conventional FAAS. The limits of detection and quantification were determined to be 1.6 µg/L and 5.2 µg/L, respectively. The calibration plot was linear over a wide concentration range and the precision for replicate measurements was appreciably high. Nickel was not detected in five different water samples but spiked recovery tests for three samples yielded results that were close to 100%, confirming the method's accuracy and applicability to the matrices tested.

Trace determination of cobalt in biological fluids based on preconcentration with a new competitive ligand using dispersive liquid-liquid microextraction combined with slotted quartz tube-flame atomic absorption spectrophotometry.

A new competitive ligand has been synthesized for the preconcentration to obtain lower detection limits by using dispersive liquid-liquid microextraction combined with slotted quartz tube-flame atomic absorption spectrophotometry (DLLME-SQT-FAAS). The proposed method is simple, eco-friendly and has high sensitivity. The preconcentration procedure was optimized on the basis of various parameters affecting the complex formation and extraction efficiency such as pH and volume of buffer solution, volume of ligand solution, mixing period, volume and type of extraction solvent, volume and type of dispersive solvent, and salt effect. Instrumental parameters were also optimized to get higher sensitivity. Under the optimum conditions, the calibration graph was linear in the range of 10-250 ng mL-1and the resulted limits of detection and quantification (LOD and LOQ) for combined method were 4.7 and 15.7 ng mL-1, respectively. The detection power was improved 48-fold using DLLME-SQT-FAAS method compared to conventional FAAS. The precision of the method was found to be high with a relative standard deviation of 2.5%. The accuracy of method was evaluated by recovery experiments using matrix matching study on spiked urine and blood samples. The recoveries for urine and blood samples ranged from 99.8 to 108.9% and 102.5 to 110.0%, respectively.

Development of an efficient and sensitive analytical method for the determination of copper at trace levels by slotted quartz tube atomic absorption spectrometry after vortex-assisted dispersive liquid-liquid microextraction in biota and water samples using a novel ligand.

This study describes the determination of trace levels of copper by slotted quartz tube atomic absorption spectrometry after dispersive liquid-liquid microextraction. A ligand synthesized from the reaction of salicylaldehyde and 1-naphthylamine was used to form coordinate copper complex prior to extraction. All parameters that influence the output of complex formation, extraction, and instrumental measurement were optimized to enhance the absorbance signal of copper. Under the optimum conditions, about 104-fold enhancement in sensitivity was recorded over the conventional flame atomic absorption spectrometer, corresponding to a 0.51 ng/mL detection limit. The percent relative standard deviation calculated for the lowest concentration (4.8%) indicated high precision for the experimental procedure. Accuracy and applicability of the optimum method were determined by performing spiked recovery tests on urine, lake water, and mineral water samples. Satisfactory recovery results were obtained between 82.2 and 106.3% at four different concentrations. Matrix matching method was also performed to increase the accuracy of quantification, and the percent recovery calculated for 175 ng/mL was 105.14%.