Development of A Liquid-Phase Microextraction Method for Simultaneous Determination of Parabens in Lipstick Samples at Trace Levels by High-Performance Liquid Chromatography.

The endocrine-disrupting potential of parabens, as well as their relation to cancer, has sparked significant discussions over their impact. Consequently, analyses of cosmetic products are an essential necessity, particularly in terms of human health and safety. In this study, a highly accurate and sensitive liquid-phase-based microextraction method was developed to determine the five parabens at trace levels by high-performance liquid chromatography. All prominent parameters of the method such as extraction solvent type and amount (1,2-dichloroethane/250 µL), and dispersive solvent type and amount (isopropyl alcohol/2.0 mL) were optimized to enhance the extraction efficiency of the analytes. The mobile phase consisting of 50 mM ammonium formate aqueous solution (pH 4.0) and acetonitrile (60:40, v/v) was used to elute the analytes at a flow rate of 1.2 mL min-1 in the isocratic mode. Analytical performance of the optimum method for methyl, ethyl, propyl, butyl and benzyl parabens were determined and the analytes recorded detection limit values of 0.78, 0.75, 0.34, 0.33 and 0.75 µg kg-1, respectively. Four different lipstick samples were analyzed under optimum conditions of the developed method, and the amount of parabens quantified in the samples using matrix matched calibration standards was in the range of 0.11-1.03%.

Development of a double monitoring system for the determination of Cr(VI) in different water matrices by HPLC-UV and digital image-based colorimetric detection method with the help of a metal sieve-linked double syringe system in complexation.

This study reports a cheap, efficient, sensitive, and simple double monitoring analytical method for trace determination of Cr(VI), which is toxic and harmful even at very low concentrations. A metal sieve-linked double syringe (MSLDS) system was used to help the formation of chromium complex (Cr-diphenyl carbazide, DPC) subsequently determined by high-performance liquid chromatography-ultraviolet (HPLC-UV) and digital image-based colorimetry (DIC) systems. The metal complex was eluted through a Phenomenex-Aqua C18 with a mobile phase comprising of 50 mM ammonium formate solution (pH 4.0):acetonitrile (78:22, v/v) and detected by the UV detector at the wavelength of 581 nm. Under their optimum conditions, the HPLC-UV and DIC systems exhibited good linearity in ranges of 10-500 µg L-1 and 100-1000 µg L-1, respectively. The percent relative standard deviations (RSD%s) calculated for the lowest concentrations of both systems fell below 10%, and this confirmed good repeatability for replicate measurements. The accuracy of the proposed methods was evaluated by performing spike recovery experiments on wastewater, river water, and tap water samples. The calculated recovery results were in the range of 81.5-105.5% for HPLC-UV system and 93.8-111.1% for the DIC system. These results indicate that the proposed methods are suitable for routine Cr(VI) determination in terms of their rapidness, simplicity, good repeatability, and low cost.

Development of a metal sieve-linked double syringe liquid phase microextraction method for the determination of copper in olive leaf extract samples by flame atomic absorption spectrometry.

This work reports the development of a simple, sensitive and low-cost analytical method for the trace determination of copper. A metal sieve-linked double syringe liquid phase microextraction method was used to preconcentrate copper into measurable quantities for FAAS system. The pressurized mixing offered by the automated syringe system and the sieve connector enhanced surface area for analyte and extraction solvent interaction, this significantly increased the extraction efficiency for copper. There was therefore no need for auxiliary organic solvents as disperser solvents for the extractant dichloromethane. The limits of detection and quantification, linear dynamic range and percent relative standard deviation values calculated for copper under optimum conditions of the method were 1.5 and 5.1 µg L-1, 5.0-500 µg L-1 and 8.4%, respectively. The developed method was successfully employed to determine copper (0.75-8.06 mg kg-1) in unspiked olive leaf samples.

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.

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.

A Novel Liquid-Liquid Extraction for the Determination of Sertraline in Tap Water and Waste Water at Trace Levels by GC-MS.

A simple, green and fast analytical method was developed for the determination of sertraline in tap and waste water samples at trace levels by using supportive liquid-liquid extraction with gas chromatography-mass spectrometry. Different parameters affecting extraction efficiency such as types and volumes of extraction and supporter solvents, extraction period, salt type and amount were optimized to get lower detection limits. Ethyl acetate was selected as optimum extraction solvent. In order to improve the precision, anthracene-D10 was used as an internal standard. The calibration plot of sertraline was linear from 1.0 to 1000 ng/mL with a correlation coefficient of 0.999. The limit of detection value under the optimum conditions was found to be 0.43 ng/mL. In real sample measurements, spiking experiments were performed to check the reliability of the method for these matrices. The spiking experiments yielded satisfactory recoveries of 91.19 ± 2.48%, 90.48 ± 5.19% and 95.46 ± 6.56% for 100, 250 and 500 ng/mL sertraline for tap water, and 85.80 ± 2.15% and 92.43 ± 4.02% for 250 and 500 ng/mL sertraline for waste water.

Sensitive Determination of Sertraline in Commercial Drugs and Its Stability Check in Simulated Gastric Juice.

A sensitive analytical method was developed for the determination of sertraline in commercial drug samples by using GC-MS. The selected-ion monitoring mode was used at the most sensitive m/z 274 to obtain a lower detection limit. LOD/LOQ values were obtained as 1.6/5.4 ng/mL for sertraline under the optimum conditions. The calibration plot was linear between 5.0 and 2000 ng/mL with the correlation coefficient of 0.9999. The validated method was successfully applied to three different brands of drug samples for both qualitative and quantitative measurement of sertraline. In this experiment, four replicate extractions were performed for each brand, and the results were compared to the values written on the labels of the drug brands. Spiking experiments were also performed to check the effect of the matrixes on the determination, and it was observed that there was no shift in the retention time of the analyte. In addition, simulated gastric juice experiments were performed to check the stability of sertraline in the stomach for 240 min, and it was observed that there was no change in the structure of the analyte.

Molecular characterization of silver-stearate nanoparticles (AgStNPs): A hydrophobic and antimicrobial material against foodborne pathogens.

In this study, silver-stearate nanoparticles (AgStNPs) have been produced from silver nitrate solutions by replacing the nitrate by stearate ions and then reducing by thermal treatment. AgStNPs were characterized by particle size, zeta-potential, ATR-FTIR, contact angle and SEM (scanning electron microscopy) analyses. The mean particle size and zeta potential of AgStNPs were determined to be 69.22±7.30nm and +8.02±0.88mV. ATR-FTIR analysis showed characteristic IR bands of stearate, revealing the two strong peaks at 2848 and 2915cm-1 associated to symmetric (νs(CH2)) and asymmetric (νas(CH2)) stretching vibrations of methylene groups, respectively. On the other hand, the scissoring and rocking modes of methylene group were observed at 1470 and 718cm-1, respectively. Nanomorphological characterization by SEM revealed a layered morphology of AgStNPs. Contact angle measurements demonstrated that a contact angle of water drop on glass coated with AgStNPs was found to be 108.76°, which proved the strong hydrophobic properties of AgStNPs. AgStNPs seemed to be very effective in inhibiting foodborne pathogens (Salmonella Typhimurium, Escherichia coli O157:H7, Staphylococcus aureus, Listeria monocytogenes and Candida albicans). The results suggest the use of AgStNPs as a coating material to reduce biofilm or biofouling formation in terms of achieving appropriate food contact surfaces and higher hygiene/easier sanitation due to their strong hydrophobic and antimicrobial properties.