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.

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.

Sensitive Determination of Acetochlor, Alachlor, Metolachlor and Fenthion Utilizing Mechanical Shaking Assisted Dispersive Liquid-Liquid Microextraction Prior to Gas Chromatography-Mass Spectrometry.

A green, sensitive and accurate dispersive liquid-liquid microextraction (DLLME) method was used to preconcentrate four selected pesticides in dam lake water samples for determination by gas chromatography-mass spectrometry (GC-MS). Conditions of the DLLME method were comprehensively investigated and optimized according to type/volume of extraction solvent, type/volume of dispersive solvent, and type/period of mixing. The developed method was validated according to the limits of detection and quantitation, accuracy, precision and linearity. Under the optimum conditions, limit of detection values calculated for alachlor, acetochlor, metolachlor and fenthion were 1.7, 1.7, 0.2 and 7.8 µg/kg (mass based), respectively. The method recorded 202, 104, 275 and 165 folds improvement in detection power values for acetochlor, alachlor, metolachlor and fenthion, respectively, when compared with direct GC-MS measurements. In order to evaluate the accuracy of the developed method, real sample application with spiking experiments was performed on dam lake water samples, and satisfactory percent recovery results in the range of 81%-120% were obtained.

Determination of iron in hair samples by slotted quartz tube-flame atomic absorption spectrometry after switchable solvent liquid phase extraction.

In this study, a green switchable solvent based liquid phase extraction (SS-LPE) method was developed for the determination of iron in human hair matrix at very low concentrations. The switchable solvent was synthesized from N,N-Dimethlybenzylamide (DMBA) and ultrapure water with the addition of dry ice for protonation, and used as the extraction solvent. The optimum conditions obtained for 8.0 mL aqueous solution after univariate optimization were 1.5 mL of pH 4.0 buffer solution, 0.75 mL of 0.015 % ligand solution, 0.75 mL of switchable solvent, 45 s vortex period for complexation and extraction, 1.25 mL of 1.50 M NaOH and 30 s vortex period after the addition of NaOH. Under the optimum conditions, a 92-fold improvement was obtained in the detection power of the flame atomic absorption spectrometry (FAAS). The limit of detection (LOD) and limit of quantification (LOQ) values were found to be 2.6 and 8.6 µg/L, respectively. Linear range of the developed method was between 11 and 75 µg/L, with a correlation coefficient (R2) value of 0.9992. Accuracy and the applicability of the proposed method were verified by recovery studies and the results obtained for 15, 20, 30 and 40 µg/L spiked concentrations were 113.3 ±â€¯4.9, 90.6 ±â€¯4.4, 102.8 ±â€¯8.2 and 98.1 ±â€¯7.5 %, respectively.

A sieve-conducted two-syringe-based pressurized liquid-phase microextraction for the determination of indium by slotted quartz tube-flame atomic absorption spectrometry.

In this study, a new liquid-phase microextraction method termed sieve-conducted two-syringe-based pressurized liquid-phase microextraction (SCTS-PLPME) was developed as a preconcentration tool for indium. Here, two syringes were connected to each other by an apparatus to produce an environment subject to pressure. The pressure created between the two syringes by simultaneous movements of the syringe plungers (to and fro) generated an efficient dispersion and this eliminated the need for dispersive solvents. Determination of indium after preconcentration was carried out with a slotted quartz tube attached flame atomic absorption spectrometer (SQT-FAAS). The detection limit (LOD) and quantification limit (LOQ) of the developed method were calculated as 19.2 and 72.2 µg L-1, respectively. The reliability and accuracy of the developed method was tested by performing recovery studies on lake water spiked at different concentrations and the obtained percent recoveries were between 101.2 and 106.9%.

Determination of lead in milk samples using vortex assisted deep eutectic solvent based liquid phase microextraction-slotted quartz tube-flame atomic absorption spectrometry system.

Determination of lead at trace levels was achieved by slotted quartz tube-flame atomic absorption spectrometry (SQT-FAAS) after the preconcentration with deep eutectic solvent-based liquid phase microextraction (DES-LPME). A green solvent was used to extract lead from the aqueous solution. Parameters affecting the extraction efficiency and determination were optimized in the aim to lower the detection limit. Under the optimum experimental and instrumental conditions, the proposed method exhibited a linear range between 50 and 1000 µg L-1, and the limits of detection and quantitation (LOD and LOQ) were found to be 8.7 and 29.0 µg L-1, respectively. The detection power was improved by 48 times using DES-LPME-SQT-FAAS method with respect to conventional FAAS system. Recovery studies were carried out in raw milk samples to check the accuracy and the applicability of the developed method and the percent recoveries obtained were between 102.5 and 103.2% for the spiked raw milk samples.

A rapid and sensitive reversed phase-HPLC method for simultaneous determination of ibuprofen and paracetamol in drug samples and their behaviors in simulated gastric conditions.

Paracetamol is a widely used drug for fever and pain relief. Ibuprofen is a common nonsteroidal anti-inflammatory drug. In this study, a sensitive and accurate reversed phase high performance liquid chromatography method was developed for the simultaneous determination of ibuprofen and paracetamol. The chromatographic separation was achieved on a Phenomenex C18 (250 mm, 4.6 mm, 5 µm) column. Fifty milli molar phosphate buffer (pH 7.5) and methanol were used as mobile phase in a gradient elution mode. The retention times of paracetamol and ibuprofen were 5.7 and 10.4 min, respectively. The linearity of the developed method was established in the range of 0.25 - 250 mg/L with a correlation coefficient of 0.9998 for both analytes. The limit of detection/quantification values were found to be 0.06/0.19 and 0.08/0.26 mg/L for ibuprofen and paracetamol, respectively. The method was successfully applied in drug samples in the form of tablets and suspensions. The calculated concentrations matched with the claimed values on their prospectuses. The drug samples were studied under simulated gastric conditions to determine the behaviors of the analytes in the human body. The obtained results showed no change in the retention time of the analyte peak shapes throughout the 210 minutes.