Non-steroidal Anti-inflammatory Drugs In Water Samples Research Articles

Development of efficient SALDI substrate based on Au–TiO2 nanohybrids for environmental and forensic detection of dyes and NSAIDs

Herein, a matrix-free approach is presented for comprehensive environmental and forensic analysis of dyes and nonsteroidal anti-inflammatory drugs (NSAIDs) using Au–TiO2 nanohybrids coupled with surface-assisted pulsed laser desorption ionization-mass spectrometry (SALDI-MS). The Au–TiO2 nanohybrids was prepared and characterized using inductively coupled plasma-optical emission spectrometry (ICP-OES), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), surface area measurements, ultraviolet–visible (UV–vis) spectroscopy, transmission electron microscopy (TEM), and scanning electron microscopy-energy dispersive spectrometry (SEM-EDS). Initially, the optimal Au content was assessed using the survival yield (SY) method, confirming that 7.5% Au content on the TiO2 surface offered the highest ionization efficiency. Subsequently, environmental analyses of dyes and NSAIDs in water samples were performed, and sensitive detection of all analytes was achieved with limits of detection (LODs) ranging from 10.0 ng mL−1 to 10.0 fg mL−1 and good spot-to-spot reproducibility. Additionally, the effect of potential contaminants commonly found in environmental samples, such as salts, surfactants and pesticides was also considered. Despite signal intensity reduction at high concentrations of some salts, the target analytes were detected, while the presence of surfactants and pesticides did not cause significant signal intensity reduction. Additionally, dyed and undyed Tetoron fibers and the effect of adhesive tape were evaluated. Direct analysis of the dyed Tetoron fibers on the target plate, using the nanohybrids, enabled higher detection sensitivity of the dyes, in addition to adducts of polystyrene and cellulose, the main components of the fiber. Finally, NSAIDs in oral fluid were analyzed and sensitive detection of the analytes was observed using the nanohybrids with LODs and LOQs in the range of 0.1–10 ng mL−1 and 1–20 ng mL−1, respectively. The trueness of the exact mass was in the range of 0.64–6.2 ppm while the recovery of the spiked samples was in the range of 82.90–107.54%% indicating the efficiency of the Au–TiO2 nanohybrids as SALDI substrate. Thus, the Au–TiO2 nanohybrids hold considerable promise in terms of sensitivity, reproducibility, and LOD, and may significantly contribute to environmental and forensic identification.

Self-assembling covalent organic framework functionalized poly (styrene-divinyl benzene-glycidylmethacrylate) composite for the rapid extraction of non-steroidal anti-inflammatory drugs in wastewater

The growing use of non-steroidal anti-inflammatory drugs (NSAIDs) has seriously affected human health and ecosystems, as a result, the World Health Organization (WHO) has regarded them as emerging contaminants. NSAID’s polar nature and trace amount present in wastewater make their extraction and determination challenging in modern analytical science. Therefore, regarding the need, we herein report a rapid, sensitive and selective in-syringe solid-phase extraction (SPE) method coupled with ultrahigh performance liquid chromatography and UV detector for the determination of seven NSAIDs in environmental water samples. Specifically, the NSAIDs in water samples were directly extracted by using synthesized porous covalent organic framework functionalized poly (styrene-divinyl benzene-glycidylmethacrylate) composite (COF@PS-GMA) without further cleanup procedures. The adsorption of NSAIDs on COF@PS-GMA sorbent was investigated by using adsorption isotherms and kinetic studies. Various parameters, including amount of sorbent, pH of the samples, the volume of desorption solvent, and desorption time that were involved in in-syringe SPE were optimized. Under the optimized conditions, good linearity was observed at 0.005–5.0 μg mL−1 with method quantification limits (LOQs) estimated between 0.54–2.74 μg L−1. The recoveries of the seven NSAIDs at the level of 0.5, 5.0 and 20.0 μg L−1 were ranging from 84.3% to 99.6%.

Magnetic sporopollenin-cyanopropyltriethoxysilane-dispersive micro-solid phase extraction coupled with high performance liquid chromatography for the determination of selected non-steroidal anti-inflammatory drugs in water samples

A facile dispersive-micro-solid phase extraction (D-μ-SPE) method coupled with HPLC for the analysis of selected non-steroidal anti-inflammatory drugs (NSAIDs) in water samples was developed using a newly prepared magnetic sporopollenin-cyanopropyltriethoxysilane (MS-CNPrTEOS) sorbent. Sporopollenin homogenous microparticles of Lycopodium clavatum spores possessed accessible functional groups that facilitated surface modification. Simple modification was performed by functionalization with 3-cyanopropyltriethoxysilane (CNPrTEOS) and magnetite was introduced onto the biopolymer to simplify the extraction process. MS-CNPrTEOS was identified by infrared spectrometrywhile the morphology and the magnetic property were confirmed by scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM), respectively. To maximize the extraction performance of ketoprofen, ibuprofen, diclofenac and mefenamic acid using the proposed MS-CNPrTEOS, important D-μ-SPE parameters were comprehensively optimized. The optimum extraction conditions were sorbent amount, 40 mg; extraction time, 5 min; desorption time; 5 min; sample volume, 15 mL; sample pH 2.0; and salt addition, 2.5% (w/v). The feasibility of the developed method was evaluated using spiked tap water, lake water, river water and waste water samples. Results showed that ketoprofen and ibuprofen were linear in the range of 1.0–1000 μg L−1 whilst diclofenac and mefenamic acid were linear in the range 0.8–500 μg L−1. The results also showed good detection limits for the studied NSAIDs in the range of 0.21–0.51 μg L−1 and good recoveries for spiked water samples in the range of 85.1–106.4%. The MS-CNPrTEOS proved a promising dispersive sorbent and applicable to facile and rapid assay of NSAIDs in water samples.

Ionic liquids for improving the extraction of NSAIDs in water samples using dispersive liquid–liquid microextraction by high performance liquid chromatography-diode array–fluorescence detection

A rapid, sensitive and efficient analytical method based on the use of ionic liquids for determination of non-steroidal anti-inflammatory drugs (NSAIDs) in water samples was developed. High-performance liquid chromatography equipped with a diode array and fluorescence detector was used for quantification of ketoprofen, ibuprofen and diclofenac in tap and river water samples. This new method relies on the use of two ionic liquids with multiple functionalities: one functions as an extraction solvent (1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF6]), and the other changes the polarity in the aqueous medium (1-butyl-3-methylimidazolium tetrafluoroborate, ([BMIM][BF4]). Factors such as the type and volume of the ILs and dispersive solvent, sample volume, and centrifugation time were investigated and optimized. The optimized method exhibited good precision, with relative standard deviation values between 2% and 3%, for the three NSAIDs. Limits of detection achieved for all of the analytes were between 17 and 95ngmL−1, and the recoveries ranged from 89% to 103%. Furthermore, the enrichment factors ranged from 49 to 57. The proposed method was successfully applied to the analysis of NSAIDs in tap and river water samples.

Nonsteroidal Anti-Inflammatory Drug Determination in Water Samples by HPLC-DAD under Isocratic Conditions

Nonsteroidal anti-inflammatory drugs (NSAIDs) are a group of medications widely used by man to heal certain ailments. However, after consumption, they may be excreted in wastewaters with consequent environmental effects. NSAIDs are endocrine disruptors that can cause changes in animal physiology. The purpose of this study was to implement an analytical method that permits the determination of the presence of NSAIDs in water. Compound extraction was performed by solid-phase extraction (SPE) using an Oasis HLB cartridge. Analytes were analyzed by high-performance liquid chromatography with diode array detection (HPLC-DAD). The method was applied in water from the Maipo River and from a neighboring wastewater treatment plant in the Metropolitan Region of Pajaritos, Vina, Tuberia, Union and Gansos sampling points in Chile. This method turned out to be adequate for the determination of NSAIDs in water samples with recovery percentages above 80%. Naproxen and ibuprofen were mostly detected in the Maipo River water samples, with concentrations ranging from 0.33 to 0.83 µg L-1.