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This study employed simple polystyrene-coated magnetite nanoparticles (PS@MNPs)-assisted batch adsorption process for the removal of two antidepressant active ingredients (amitriptyline HCl and sertraline HCl) from hospital wastewater. Dominant parameters of the adsorption process including pH, adsorbent amount, and contact period were optimized through the univariate approach to enhance the adsorption efficiency. Upon reaching optimum adsorption conditions, equilibrium experiments were performed by spiking the adsorbates in hospital wastewater in the concentration range of 100-2000 μg/L. The concentrations of the adsorbates in the effluent were calculated using the matrix-matching calibration strategy to enhance the accuracy of quantification. A validated switchable solvent-based liquid phase microextraction (SS-LPME) method was employed to enrich the two active pharmaceutical ingredients (APIs) prior to sensitive determination with GC-MS (gas chromatography-mass spectrometry). The equilibrium data were mathematically modeled employing the Langmuir and Freundlich adsorption isotherm models. The isotherm constants were calculated, and the results showed that both the isotherm models fitted well with the experimental data. The efficient and simple batch adsorption strategy reported in this study was successfully employed to remove amitriptyline HCl and sertraline HCl from hospital wastewater at low concentrations., (© 2023. The Author(s), under exclusive licence to Springer Nature Switzerland AG.)

This study reports a liquid phase microextraction method based on binary extraction solvents, which were used to preconcentrate chlorbenside and fenobucarb from aqueous samples for determination by gas chromatography mass spectrometry. Parameters including the type, ratio, and volume of binary solvents, disperser solvent type and volume, and vortex period were optimized systematically to achieve high enrichment for the analytes. The optimum conditions obtained were used to validate the method, and the detection limits calculated for chlorbenside (0.71 ng/mL) and fenobucarb (0.33 ng/mL) correlated to enrichment factors of 399- and 912-folds, respectively. The optimum method was applied to lake water and wastewater samples in spike recovery experiments, and the results obtained (96-104%) verified the method as accurate and applicable to the aqueous sample matrices. Matrix matching calibration method was used to boost the accuracy of quantifying the two analytes in the wastewater sample, which presented interference effects. Assessment of the method's green profile based on penalty points confirmed the method's compliance with green analytical chemistry., (© 2023. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)

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., (© 2022. The Author(s), under exclusive licence to Springer Nature Switzerland AG.)

This study presents the preconcentration of diflufenican and azaconazole from domestic wastewater samples by using dispersive solid-phase extraction (dSPE) for determination by gas chromatography-mass spectrometry (GC-MS). Stearic acid-coated magnetic nanoparticles were used as adsorbents for dSPE method. In order to maximize the efficiency of the extraction process, parameters such as magnetic nanoparticle (MNP) type and amount, eluent type and volume, mixing type, and mixing period were all optimized. The linear range obtained for azaconazole and diflufenican was 7.50-500 ng/mL and 7.50-750 ng/mL, and their limits of detection/quantification (LOD/LOQ) were calculated as 1.3/4.3 ng/mL and 1.4/4.7 ng/mL, respectively. By comparing the LOD values of direct GC-MS and the developed dSPE method, azaconazole and diflufenican recorded approximately 35 and 38 folds enhancement in detection power. Recovery experiments with domestic wastewater were carried out to certify the proposed method's accuracy and applicability. By using the matrix matching calibration strategy, the good percent recovery results between 98 and 105% were obtained., (© 2022. The Author(s), under exclusive licence to Springer Nature Switzerland AG.)

This paper presents the removal of nine potential endocrine disruptors including pesticides, pharmaceuticals and industrial chemicals using a submerged membrane bioreactor (MBR) system. Two lab-scale submerged MBRs having ceramic membranes were operated at three different sludge retention times (SRT: 15, 45, 90 days) and two hydraulic retention times (HRT: 12, 6 h) and the effects of SRT and HRT on both micropollutant removal and membrane fouling were investigated. While the effect of SRT and HRT change was observed on the removal of atrazine, fluoxetine, penconazole, no significant change was detected for the other micropollutants studied. It was determined that physicochemical properties such as distribution coefficient (LogD) and hydrophobicity of micropollutants are also effective on the removal efficiency of micropollutants. High removal efficiencies ([Formula: see text] 97.5%) were observed for hydrophobic pollutants (logD > 3.2) except for penconazole (72.1%) and for hydrophilic pollutants (logD < 3.2) except for atrazine (42.5%). Membrane fouling was significantly affected by different operational parameters applied, with the slowest fouling occurring at 45 days of SRT and 12 h of HRT. However, micropollutant addition did not have a significant effect on membrane fouling. It has been shown that the simultaneous and effective treatment performance for micropollutants makes the membrane bioreactor system a promising wastewater treatment process., (© 2022. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)

A sensitive, accurate and simple analytical method was developed to determine cadmium by slotted quartz tube-flame atomic absorption spectrometry after preconcentration/extraction with polystyrene coated magnetic nanoparticles based dispersive solid phase extraction. The surface of Fe 3 O 4 based magnetic nanoparticles was modified with polystyrene to yield higher selectivity and sensitivity in adsorption efficiency of cadmium. The nanoparticles were dispersed into the aqueous solution to extract/separate cadmium. Significant parameters of the method including magnetic nanoparticle amount, mixing effect, effect of ionic strength, eluent concentration and sonication period were optimized to achieve optimal conditions for the analyte. The limit of detection and quantification values of the developed method were found to be 0.62 and 2.1 ng/mL, respectively. Under the optimum conditions, enhancement of the detection power for cadmium were calculated as 102 folds for the developed method. The developed method was then applied to cigarette ash to test its accuracy and applicability. Total cadmium was found to be between 402 and 450 ng/g in the ashes of different cigarette brands commercially available in Turkey. The accuracy of quantifying cadmium in the complex ash samples was enhanced by using the matrix matching calibration strategy. The developed method provides sensitive and selective determination of cadmium at ng/mL levels even at complex cigarette ash samples. High percent recovery results (90-102%) were obtained from spiked real samples., (© 2022. The Author(s), under exclusive licence to The Japan Society for Analytical Chemistry.)

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%., (© 2022. The Author(s), under exclusive licence to Springer Nature Switzerland AG.)

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%., (© 2022. The Author(s), under exclusive licence to Springer Nature Switzerland AG.)

Traditional copper coffee pots are widely used in these modern times and daily consumption of coffee brewed in overused/old pots increases the risk of copper ingestion. This study employed a green switchable solvent-based liquid-phase microextraction (SS-LPME) method to isolate and preconcentrate copper from water boiled in coffee pots. Copper was determined by a flame atomic absorption spectrometry (FAAS) system coupled with a slotted quartz tube (SQT). 1,5-Diphenylcarbazone was added to aqueous samples to form a complex with copper before the extraction step. Box-Behnken experimental design was applied to select optimum conditions of the extraction method that were used to validate the analytical method. The limits of quantification and detection of the optimized SS-LPME-SQT-FAAS method were determined as 9.1 and 2.7 μg/L, respectively. Water samples boiled in traditional coffee pots were spiked at different concentrations and analyzed to ascertain the method's accuracy and applicability to real samples. Satisfactory recovery results obtained in the range of 92-107% established good accuracy, and percent relative standard deviations lower than 8.0% also proved high precision.

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.

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 R 2 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%.

This study describes the development of a sensitive and accurate dispersive liquid-liquid microextraction strategy for the preconcentration and determination of selected pesticides in wastewater and lake water samples by gas chromatography-mass spectrometry. Determination of these pesticides at high accuracy and precision is important because they can be still be found in environmental samples. The type of extraction solvent and type of disperser solvent were optimized using the univariate approach. Furthermore, a Box-Behnken experimental design was used to set up a working model made up of 18 combinations of three variables, tested at three levels. The parameters fitted into the design model were volume of extraction solvent, disperser solvent volume, and mixing period. Analysis of variance was used to evaluate the experimental data to determine the significance of extraction variables and their interactions, before selecting optimum extraction conditions. The method was then applied to aqueous standard solutions between 2.0 and 500 μg L -1 , and the limit of detection (LOD) and quantification (LOQ) values obtained for the analytes were between 0.37-2.8 and 1.2-9.4 μg L -1 , respectively. The percent recoveries were calculated in the range of 92-114 and 96-110% for wastewater and lake water, respectively. These results validated the accuracy and applicability of the method to the selected matrices.

This study presents the use of Quick Easy Cheap Efficient Rugged and Safe (QuEChERS) as an effective sample cleaning procedure and switchable solvent liquid phase microextraction (SS-LPME) as a preconcentration tool for the determination of fenazaquin by gas chromatography mass spectrometry (GC-MS) at ultratrace levels. After a thorough optimization process, 0.50 mL of switchable solvent, 1.5 mL of 1.0 M sodium hydroxide, and 15 s of vortexing were determined as optimum conditions of the SS-LPME method. The limit of detection (LOD) and limit of quantitation (LOQ) determined using the optimum method (SS-LPME/GC-MS) were 0.05 and 0.18 ng/mL, respectively. Compared with direct GC-MS determination of fenazaquin, the optimum method yielded about 800-fold enhancement in detection power of GC-MS. The method was applied to lake, irrigation canal, well, and wastewater samples. In order to test the method's applicability on fresh tomato samples, a QuEChERS method was used before applying the SS-LPME method. Matrix-matched calibration standards were used to enhance the accuracy of fenazaquin quantification in spiked tomato samples to obtain recovery results close to 100%.

Presented in this study is a simple but efficient switchable polarity solvent microextraction strategy for etrimfos preconcentration from water and food samples for quantification by gas chromatography mass spectrometry. Repeatability of the extraction process and instrumental measurements were enhanced by using deuterated bisphenol A as internal standard. Significant parameters of the extraction method were fitted into an experimental design model to study the effects of parameters on extraction output, as well as mutual effects of combined parameters. The design model was formed with 51 experimented data obtained from the combination of sodium hydroxide volume, switchable solvent volume, and vortex period at three levels. The method was validated by applying optimum conditions attained from the model predictor. The detection limit was found to be 1.3 ng/mL and it corresponded to an enhancement factor of about 54 folds when compared to direct GC-MS measurement. Etrimfos was not detected in the water and food samples tested but the results (92-107%) obtained from spiked recovery experiments established that etrimfos when present in the selected matrices can be accurately and precisely quantified.

This study reports the optimization of a binary dispersive liquid-liquid microextraction method for the determination of iprodione, procymidone, and chlorflurenol by gas chromatography mass spectrometry. The study was aimed at using two extraction solvents to increase the extraction efficiency of all analytes. The binary solvents recorded results higher than the mono-solvents. After examining the effects of main experimental parameters and their interactions by analysis of variance, 200 μL of binary mixture (dichloromethane and 1,2-dichloroethane), 2.5 mL of ethanol, and 15 s vortex were obtained as optimum parameters. The detection and quantification limits calculated for the analytes were found to be between 0.30-1.6 and 1.0-5.3 ng/mL, respectively. Enhancement in detection power calculated as a ratio of the binary extraction detection limit to the detection limit of direct GC-MS analysis was 105-, 214-, and 233-fold for chlorflurenol, iprodione, and procymidone, respectively. In order to check the accuracy of the developed method, recovery study was performed. Water sampled from a lake and two wastewater samples from treatment facilities were spiked at two concentrations, and the percent recovery calculated for the samples ranged between 87 and 116%. These results confirmed the suitability of the method to real samples for accurate determination of the analytes at trace levels.

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.

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%.

In this study, a switchable solvent was used to preconcentrate trace amounts of Cd from aqueous solution for its determination by flame atomic absorption spectrometry (FAAS). Protonation of N,N-dimethylbenzylamine by dry ice (solid CO 2 ) made it water soluble, and addition of sodium hydroxide converted it back to its original nonionic state for phase separation and subsequent extraction of Cd. A slotted quartz tube (SQT) was attached to the flame burner head to increase the residence time of Cd atoms in the light path. Under the optimum conditions, limits of detection and quantification were determined as 0.7 and 2.6 μg L -1 , respectively. Low relative standard deviations calculated from seven replicate measurements of the lowest concentration indicated high precision. Accuracy of the developed method was checked by using a standard reference material (SRM 1633c). Spiked recovery tests were also performed on lake water and wastewater samples at different concentrations to check the applicability of the developed method, and the results obtained (90-103%) established high recovery.

A sensitive and accurate analytical method based on dispersive liquid-liquid microextraction was developed for the simultaneous determination of selected pesticides, hormones, and endocrine disruptors by GC-MS. The optimum conditions of the extraction procedure were determined using an experimental design of factors significantly affecting the extraction output. Analysis of variance (ANOVA) was used to evaluate the main effects of experimental factors and their interactions. The limit of detection values determined for the analytes under optimum experimental conditions were found to be between 0.30-2.0 ng/mL. The linear calibration plot of analytes span across a wide concentration range and low %RSD values from replicate measurements indicated good precision of the developed method. Spiked recovery tests were also performed on municipal wastewater, well water, lake water, sea water, and tap water matrices to determine the method's accuracy and applicability to water samples. The recovery results obtained were satisfactory for all water samples.

Polycyclic aromatic hydrocarbons are known for their carcinogenic and mutagenic effects on human health. This therefore calls for the regulation of their concentrations in air, water, and soil. Naphthalene as the simplest in structure of the polycyclic aromatic hydrocarbons is mainly used as a starter material for other chemicals but also has impacts on human health. A method is therefore proposed for the determination of naphthalene in water samples by gas chromatography mass spectrometry after liquid-liquid extraction. The extraction method was optimized to improve the extraction output, thereby lowering the limit of detection. The limits of detection and quantification obtained for naphthalene were 4.4 and 14.6 ng mL -1 , respectively. Deuterated anthracene was used as internal standard to enhance the precision of the method, for which a relative standard deviation of 4.3% was obtained. The percent recovery of naphthalene obtained from tap water was ranged between 93.8 and 102.2.

In this study, solidified floating organic drop microextraction (SFODME) by 1-undecanol was combined with slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) for the determination of cadmium at trace levels. Formation of a complex with 4,4'-dimethyl-2,2'-bipyridine facilitated the extraction of cadmium from aqueous solutions. Several chemical variables were optimized in order to obtain high extraction outputs. Parameters such as concentration of the ligand, pH, and amount of buffer solution were optimized to enhance the formation of cadmium complex. The SFODME method was assisted by dispersion of extractor solvent into aqueous solutions using 2-propanol. Under the optimum extraction and instrumental conditions, the limit of detection and limit of quantitation values obtained for cadmium using the combined methods (SFODME-SQT-FAAS) were found to be 0.4 and 1.3 μg L -1 , respectively. Matrix effects on the method were also examined for tap water and wastewater, and spiked recovery results were found to be very satisfactory. Graphical Abstract SFODME-SQT-FAAS system for sensitive determination of cadmium.

The need to enhance food safety has led to major advancements in pesticide productions, and though many benefits have been gained, environmental contamination has also risen from these chemicals that tend to persist in the environment. Some pesticides, together with other chemicals commonly called endocrine disruptor compounds, block the receptor sites of hormones or mimic displaced hormones, leading to imbalanced hormonal levels that result in health disorders and diseases. These chemicals occur at trace levels and are not directly detected by conventional analytical methods. A dispersive liquid-liquid microextraction method was therefore developed for preconcentration of 12 analytes including hormones, endocrine disruptor compounds, and pesticides, to be analyzed by gas chromatography mass spectrometry. This was achieved by optimizing parameters such as extractor solvent type and amount, dispersive solvent type and amount, pH, and salt effect that affect extraction output. The limits of detection and quantification of the developed method were between 0.09 and 3.36 and 0.31 and 11.19 ng mL -1 , respectively. The calibration plots of the analytes also showed good linearity and low percent relative standard deviations. Recovery studies were performed for tap water and wastewater samples, and the percent recoveries recorded were between 84 and 109%.