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%.

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%).

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.

Accurate and Sensitive Analytical Strategy for the Determination of Antimony: Hydrogen Assisted T-Shaped Slotted Quartz Tube-Atom Trap-Flame Atomic Absorption Spectrometry.

Antimony is known to have some adverse health effects on human health. Flame atomic absorption spectrometry (FAAS) is a widely used instrumental for the determination of antimony and other metals. However, it lacks the sensitivity to determine these metals at trace levels. This study was aimed at overcoming this setback by using hydrogen assisted T-shaped slotted quartz tube technique to preconcentrate and determine antimony by FAAS. All the system parameters were optimized to enhance the detection power of the system. Under the optimum experimental conditions, the limits of detection and quantification were found to be 0.75 and 2.49 µg L-1, respectively with R2 value of 0.9999. Accuracy of the developed method was validated by experimental results agreeing to the certified value of a standard reference material. Recovery studies were also carried out to determine the method's applicability to tap and mineral water samples, and the results obtained were appreciable.

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 Analytical Method for the Determination of Amoxicillin in Commercial Drugs and Wastewater Samples, and Assessing its Stability in Simulated Gastric Digestion.

A highly sensitive analytical HPLC-UV method was developed for the determination of amoxicillin in drugs and wastewater samples at a single wavelength (230 nm). In order to substantially predict the in vivo behavior of amoxicillin, drug samples were subjected to simulated gastric conditions. The calibration plot of the method was linear from 0.050 to 500 mg L-1 with a correlation coefficient of 0.9999. The limit of detection and limit of quantitation were found to be 16 and 54 µg L-1, respectively. The percentage recovery of amoxicillin in wastewater was found to be 97.0 ± 1.6%. The method was successfully applied for the qualitative and quantitative determination of amoxicillin in drug samples including tablets and suspensions.