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1.
Spectrochim Acta A Mol Biomol Spectrosc ; 321: 124751, 2024 Nov 15.
Article in English | MEDLINE | ID: mdl-38959689

ABSTRACT

Spatially offset Raman scattering (SORS) line-mapping was explored as a versatile tool to examine accuracy variations in compositional analyses of tablets with different particle sizes. SORS spectra collected near the laser irradiation were less representative of tablet composition due to the limited spectroscopic sampling volume, while the signal-to-noise (S/N) ratios of corresponding spectra were higher. On the other hand, SORS spectra at longer offset distances were better representative of tablet composition, while their S/N ratios were decreased considerably. Therefore, the use of only a certain portion of sliced (line-mapped) spectra balanced with the sample representation and S/N ratio could be advantageous to enhance accuracy. Moreover, a group of optimal slice spectra is expected to vary when the particle size of the tablet changes since the characteristics of internal photon propagation also would change. For the overall examination, SORS spectra of 30 Anaprox tablets (composed of 4 constituents including naproxen sodium) with 2 particle sizes (88.4 ± 11.8 µm and 118.9 ± 38.8 µm) were analyzed, and the concentrations of three components in these tablets were determined. A total of 6 cases (3 components and 2 particle sizes) were examined. When the average optimal slice spectra were employed in each case, the errors were lower compared to those using the average of all slice spectra. The demonstrated scheme was versatile to study the offset distance-dependent accuracy variations according to particle size and target component.


Subject(s)
Particle Size , Spectrum Analysis, Raman , Tablets , Spectrum Analysis, Raman/methods , Naproxen/analysis , Naproxen/chemistry , Signal-To-Noise Ratio
2.
J Pharm Biomed Anal ; 249: 116336, 2024 Oct 15.
Article in English | MEDLINE | ID: mdl-38981249

ABSTRACT

In this study, a new magnetic solid phase extraction based on magnetic composite modified with biochar obtained from pumpkin peel was developed for the enrichment and extraction of Naproxen in lake water, tablet and urine samples. The effects of main parameters such as pH, extraction time, amount of adsorbent and sample volume, which affect magnetic solid phase extraction, were investigated. Under optimal conditions, intraday and interday precision values for naproxen were below 5.9, with accuracy (relative error) better than 7.0 %. The detection limit and preliminary concentration factor were 12 ng/mL and 10, respectively. The method proposed here can be used for routine analysis of naproxen in lake water, urine and tablets.


Subject(s)
Limit of Detection , Naproxen , Solid Phase Extraction , Tablets , Naproxen/analysis , Naproxen/urine , Solid Phase Extraction/methods , Chromatography, High Pressure Liquid/methods , Tablets/analysis , Lakes/chemistry , Water/chemistry , Water Pollutants, Chemical/analysis , Hydrogen-Ion Concentration , Magnetics , Reproducibility of Results , Adsorption , Charcoal/chemistry
3.
Talanta ; 277: 126353, 2024 Sep 01.
Article in English | MEDLINE | ID: mdl-38838561

ABSTRACT

In this study, deep UV resonance Raman spectroscopy (DUV-RRS) was coupled with high performance liquid chromatography (HPLC) to be applied in the field of pharmaceutical analysis. Naproxen, Metformin and Epirubicin were employed as active pharmaceutical ingredients (APIs) covering different areas of the pharmacological spectrum. Raman signals were successfully generated and attributed to the test substances, even in the presence of the dominant solvent bands of the mobile phase. To increase sensitivity, a low-flow method was developed to extend the exposure time of the sample. This approach enabled the use of a deep UV pulse laser with a low average power of 0.5 mW. Compared to previous studies, where energy-intensive argon ion lasers were commonly used, we were able to achieve similar detection limits with our setup. Using affordable lasers with low operating costs may facilitate the transfer of the results of this study into practical applications.


Subject(s)
Spectrum Analysis, Raman , Spectrum Analysis, Raman/methods , Chromatography, High Pressure Liquid/methods , Pharmaceutical Preparations/analysis , Pharmaceutical Preparations/chemistry , Naproxen/analysis , Metformin/analysis , Metformin/chemistry , Epirubicin/analysis , Ultraviolet Rays , Bulk Drugs
4.
J Pharm Biomed Anal ; 246: 116201, 2024 Aug 15.
Article in English | MEDLINE | ID: mdl-38788621

ABSTRACT

Patient can be exposed to the photodegradation products of a drug after skin application of topical formulations. NSAIDs, with analgesic and anti-inflammatory properties, are known for the potential photoinstability, and are applied often in the form of creams, gels or liquids, commonly used among athletes, elderly people, geriatric patients and patients treated with multidrug therapies. Susceptibility to photodegradation hazard of those group arises the need for development of a new approach, with the ability to evaluate the patient safety. We planned to use a rapid assessment procedure (RAP) of safety by testing the photostability of popular skin medicinal products. This method, proposed many years ago by WHO, is now reintroduced to analytical applications in industry, when emergency drugs (e.g. for Covid) are implemented to the market in accelerated procedures. In the health care system, qualitative evaluation of drugs is extremely valuable, therefore we have planned to identify photodegradation using the FTIR method - infrared spectroscopy and DSC - differential scanning calorimetry, whilst the risk of formation of genotoxic products using the Ames test. We have successfully demonstrated that changes in the chemical structure and physical form of both pure APIs and drug products containing the API be assessed in a short time. Another advantage of our work is the combination of the developed results from FTIR/NIR spectra with statistical analysis. As a result, full and quick qualitative assessment of the effects of photoexposure of selected NSAIDs is performed, fortunately showing no mutagenicity. Due to the popularity of NSAIDs applied to the skin, a gel containing naproxen and spray with indomethacin were selected for testing. The analysis carried out for various formulations of both preparations allows us to demonstrate the universality of the applied RAP methods in assessing the risk of hazard to the patient, thus we present research results that expand or widen the knowledge and assessment of risks related to the use of drugs on the skin.


Subject(s)
Anti-Inflammatory Agents, Non-Steroidal , Indomethacin , Naproxen , Photolysis , Skin , Anti-Inflammatory Agents, Non-Steroidal/chemistry , Naproxen/chemistry , Naproxen/analysis , Indomethacin/chemistry , Humans , Skin/drug effects , Skin/radiation effects , Spectroscopy, Fourier Transform Infrared/methods , Calorimetry, Differential Scanning/methods , Administration, Cutaneous , Drug Stability
5.
J AOAC Int ; 107(5): 749-760, 2024 Oct 01.
Article in English | MEDLINE | ID: mdl-38730542

ABSTRACT

BACKGROUND: Chemometrics is a discipline that allows the spectral resolution of drugs in a pharmaceutical formulation along with degradation product and it is an alternative to chromatographic methods. OBJECTIVE: Sumatriptan (SUM) is co-formulated with naproxen (NAP) and used in acute migraine attacks. SUM, which has physiological importance, has not been subjected to any stability-indicating chemometric approaches yet, so there is a need for an accurate and safe method for the assay of the cited drug in its preparations. The greenness and blueness assessment was applied using different ecological metrics, including the Green Analytical Procedure Index (GAPI), Analytical Greenness Metric (AGREE), Analytical Eco-Scale (AES) and new "blueness" evaluation using the Blue Applicability Grade Index (BAGI) tool. METHODS: SUM was determined in pharmaceutical formulation along with NAP and in presence of alkali-induced degradation product with simple and cost-effective multivariate approaches using spectrophotometric data. Three chemometric approaches were applied for the stability-indicating determination of SUM in the presence of NAP. Classical least-squares (CLS), partial least-squares regression (PLS), and principal components regression (PCR)-three multivariate calibration numerical models that were applied to the UV spectra of the mixtures-were used to achieve the best resolution. RESULTS: Sumatriptan was analyzed with mean accuracies for PLS (100.29% ± 1.318) and for PCR (100.60% ± 1.564). The presented methods were compared and validated for their quantitative analyses. Moreover, statistical comparison between the results obtained by the proposed models and the official methods showed no significant differences. CONCLUSION: The proposed multivariate calibrations were accurate and specific for quantitative analysis of the studied component. PLS is the best method that has the capacity for qualitative analysis of SUM and it is suitable for routine analysis and stability studies of SUM in QC laboratories. Various ecological assessment metrics confirmed the long-standing eco-friendliness of the suggested models. HIGHLIGHTS: Severally overlapped mixtures of SUM along with co-formulated drug NAP and an alkali-induced degradation product were analyzed by three chemometric approaches. The analytical performance of PLS and PCR was compared and validated in terms of root-mean-square error of calibration (RMSEC), SE of prediction, and recoveries. PLS gave the highest predicted concentrations with the lowest RMSEC and root-mean-square error of prediction. The standard addition was applied for accuracy assessment and the results were compared to those of official methods. Proposed models determined SUM in synthetic mixtures and pharmaceutical formulation in QC laboratories and stability studies. Ecological evaluation tools for measuring the environmental friendliness of chemicals were utilized for the first time in the analysis of SUM.


Subject(s)
Naproxen , Spectrophotometry, Ultraviolet , Sumatriptan , Sumatriptan/analysis , Sumatriptan/chemistry , Naproxen/analysis , Naproxen/chemistry , Spectrophotometry, Ultraviolet/methods , Least-Squares Analysis , Drug Stability , Principal Component Analysis
6.
Sci Total Environ ; 898: 165317, 2023 Nov 10.
Article in English | MEDLINE | ID: mdl-37419350

ABSTRACT

Non-steroidal anti-inflammatory drugs (NSAIDs) are among the most frequently used pharmaceuticals for human therapy, pet therapeutics, and veterinary feeds, enabling them to enter into water sources such as wastewater, soil and sediment, and seawater. The control of NSAIDs has led to the advent of the novel materials for treatment techniques. Herein, we review the occurrence, impact and toxicity of NSAIDs against aquatic microorganisms, plants and humans. Typical NSAIDs, e.g., ibuprofen, ketoprofen, diclofenac, naproxen and aspirin were detected at high concentrations in wastewater up to 2,747,000 ng L-1. NSAIDs in water could cause genotoxicity, endocrine disruption, locomotive disorders, body deformations, organs damage, and photosynthetic corruption. Considering treatment methods, among adsorbents for removal of NSAIDs from water, metal-organic frameworks (10.7-638 mg g-1) and advanced porous carbons (7.4-400 mg g-1) were the most robust. Therefore, these carbon-based adsorbents showed promise in efficiency for the treatment of NSAIDs.


Subject(s)
Wastewater , Water Pollutants, Chemical , Humans , Anti-Inflammatory Agents, Non-Steroidal/toxicity , Anti-Inflammatory Agents, Non-Steroidal/analysis , Naproxen/analysis , Ibuprofen , Diclofenac , Water , Water Pollutants, Chemical/toxicity , Water Pollutants, Chemical/analysis
7.
Environ Pollut ; 331(Pt 1): 121939, 2023 Aug 15.
Article in English | MEDLINE | ID: mdl-37263567

ABSTRACT

Non-steroidal anti-inflammatory drugs (NSAIDs) are widely used globally to treat and prevent illness. Biosolids change physico-chemical characteristics of soil and can affect the mobility of NSAIDs. A field-based lysimeter study evaluated the effect of three rates (0, 7, and 28 Mg ha-1) of alkaline treated biosolids (ATB) on the leaching potential of naproxen (NPX), ibuprofen (IBF), and ketoprofen (KTF) over 34 days in a sandy loam textured soil. Although all three NSAIDs in the lysimeter cells vertically migrated to deeper soil depths after spiking, the sum of all NPX, IBF, and KTF detected in the leachate samples from all treatments were only 0.03%, 0.02%, and 0.04% of the initial spiking mass to the surface soil, respectively. A mass balance analysis indicated a low accumulation of these compounds in the soil at the end of the study (Day 34) from all treatments with only 4.8%, 0.5%, and 0.7% of initial spiked NPX, IBF, and KTF, respectively. Application of ATB significantly increased soil pH and organic matter (OM) content of the soils but did not impact retention of the compounds in the soil profile. Overall, all three NSAIDs in the present study presented low mobility in the loamy sand textured agricultural soil.


Subject(s)
Ketoprofen , Soil Pollutants , Biosolids , Anti-Inflammatory Agents, Non-Steroidal/analysis , Naproxen/analysis , Ibuprofen , Soil/chemistry , Sand , Soil Pollutants/analysis
8.
Article in English | MEDLINE | ID: mdl-36293682

ABSTRACT

There are several techniques for the removal of pharmaceuticals (drugs) from wastewater; however, strengths and weaknesses have been observed in their elimination processes that limit their applicability. Therefore, we aimed to evaluate the best techniques for the removal of pharmaceuticals from municipal and hospital wastewater. For this, a non-experimental, descriptive, qualitative-quantitative design was used, corresponding to a systematic review without meta-analysis. Based on established inclusion and exclusion criteria, 31 open-access articles were selected from the Scopus, ProQuest, EBSCOhost, and ScienceDirect databases. The results showed that high concentrations of analgesics such as naproxen (1.37 mg/L) and antibiotics such as norfloxacin (0.561 mg/L) are frequently found in wastewater and that techniques such as reverse osmosis, ozonation, and activated sludge have the best removal efficiency, achieving values of 99%. It was concluded that reverse osmosis is one of the most efficient techniques for eliminating ofloxacin, sulfamethoxazole, carbamazepine, and diclofenac from municipal wastewater, with removal rates ranging from 96 to 99.9%, while for hospital wastewater the activated sludge technique proved to be efficient, eliminating analgesics and antibiotics in the range of 41-99%.


Subject(s)
Ozone , Water Pollutants, Chemical , Wastewater/analysis , Sewage , Diclofenac , Naproxen/analysis , Norfloxacin , Water Pollutants, Chemical/analysis , Carbamazepine/analysis , Hospitals , Ozone/analysis , Sulfamethoxazole , Anti-Bacterial Agents , Ofloxacin , Pharmaceutical Preparations , Waste Disposal, Fluid/methods
9.
Environ Res ; 211: 112971, 2022 08.
Article in English | MEDLINE | ID: mdl-35276188

ABSTRACT

The contamination of water by pharmaceutical pollutants is a major issue these days due to excessive use of these ingredients in modern life. This study evaluated the adsorption and effectiveness of a low-cost composite prepared from heavy sugarcane ash (HSA) fused with polyethylene terephthalate (PET) and functionalized with iron (Fe3+) in a dynamic system through a fixed-bed column. The solution of synthetic drugs was prepared and placed in a reservoir, using a peristaltic pump the solution is run onto the fixed bed column at a flow rate of 2 mL min-1. Saturation time and adsorption capacity were evaluated by centrifugation and extraction after a regular interval of 2 h from the adsorption column. The samples were analyzed using high-performance liquid chromatography (HPLC) and the data was modeled for quantification. For DIC removal, an adsorption capacity of 324.34 µg. g-1 and a saturation time of 22 h were observed, while the adsorption capacity of NAP was 956.49 µg. g-1, with a saturation time of 8 h. Thus, the PETSCA/Fe3+ adsorbent proved to be quite efficient for removing the pharmaceutical pollutants, with a longer period of operation for DIC removal. These findings suggested that a highly efficient bed column made from a less expensive waste material and could be used to remove hazardous pharmaceutical contaminants.


Subject(s)
Saccharum , Water Pollutants, Chemical , Water Purification , Adsorption , Diclofenac , Naproxen/analysis , Pharmaceutical Preparations , Polyethylene Terephthalates , Water/chemistry , Water Pollutants, Chemical/analysis , Water Purification/methods
10.
Sci Total Environ ; 825: 153611, 2022 Jun 15.
Article in English | MEDLINE | ID: mdl-35151749

ABSTRACT

The extend of environment pollution by pharmaceuticals is in a stage that required more automatic and integrated solutions. The non-steroidal anti-inflammatory drugs (NSAIDs) are one of the most popular pharmaceutical in the world and emerging pollutants of natural waters. The aim of the paper was to check the correlation of the sales data of selected NSAIDs (ibuprofen, naproxen, diclofenac) and their concentration in the WWTP in order to enable predicting their loads, having only the sales data. For calculations, we apply three discharge scenarios (the fates between purchased to the presence in influents), having in mind that some part of sold mass can be improperly dispose to sewage system. To support predictions, chemical analysis was conducted in two conventional wastewater treatment plants (WWTPs) located in Poland during 2018 and 2020, thereby before and during pandemic situation. The NSAIDs concentration in the influent was higher than that which would be obtained if all of the administrated mass of the pharmaceutical went through the metabolic pathway of transformation. This means that substantial mass of sold NSAIDs in improperly dispose to sewage system, and this factor need to be taken into account in future predictions. Furthermore, results indicate that the variance of naproxen and diclofenac concentrations in the influent has no correlation with relatively stable sales throughout whole year. The pandemic situation had yet no direct effect to diclofenac concentrations in influents, despite observed increasing of sales. It was calculated that more than 60 kg of diclofenac was discharged into the Baltic Sea in 2018, and 20 kg in the first half of 2021 from two tested WWTPs. The presence of 4OH-diclofenac in effluents often in higher concentration compared to diclofenac mean that this still biologically active compound need to be taken into account in future risk assessment.


Subject(s)
Wastewater , Water Pollutants, Chemical , Anti-Inflammatory Agents, Non-Steroidal/analysis , Diclofenac , Naproxen/analysis , Pharmaceutical Preparations , Sewage , Wastewater/chemistry , Water Pollutants, Chemical/analysis
11.
Environ Sci Pollut Res Int ; 29(30): 45885-45902, 2022 Jun.
Article in English | MEDLINE | ID: mdl-35149949

ABSTRACT

In this study, a series of molecularly imprinted polymers (MIPs) have been synthesized using separately diclofenac, naproxen, and ibuprofen as templates with three different polymerization approaches. Two functional monomers, methacrylic acid (MAA) and 2-vinylpyridine (2-VP), were tested and ethylene glycol dimethacrylate (EGDMA) was used as crosslinker; also, template-free polymers (NIPs) were synthesized. It was found that the MIP with the highest retention percentage for diclofenac was the one prepared by the emulsion approach and with MAA (98.3%); for naproxen, the one prepared by the bulk polymerization with MAA (99%); and for ibuprofen, the one synthesized by bulk with 2-VP (97.7%). These three MIPs were characterized by scanning electron microscopy, thermogravimetric test, Fourier transform infrared, specific area measurements, and surface charge. It was found that the emulsion method allowed particle size control, while the bulk method gave heterogeneous particles. The three evaluated MIPs exhibited thermal stability up to 300 °C, and it was observed that 2-VP confers greater stability to the material. From the BET analysis, it was demonstrated that the MIPs and NIPs evaluated are mesoporous materials with a pore size between 10 and 20 nm. In addition, the monomer influenced the surface charge of the material, since the MAA conferred an acidic point of zero charge (PZC), while the 2-VP conferred a PZC of basic character. Through adsorption isotherms, it was determined  that there is a higher adsorption capacity of the MIPs at acidic pH following a pseudo-second-order kinetic model. Finally, the MIPs were used to determine the non-steroidal anti-inflammatory drugs (NSAIDs) understudy in San Luis Potosí, México, wastewater, finding concentrations of 0.642, 0.985, and 0.403 mg L-1 for DCF, NPX, and IBP, respectively.


Subject(s)
Molecular Imprinting , Adsorption , Anti-Inflammatory Agents, Non-Steroidal/analysis , Diclofenac/analysis , Emulsions , Ibuprofen , Molecular Imprinting/methods , Molecularly Imprinted Polymers , Naproxen/analysis , Wastewater/analysis
12.
Chemosphere ; 291(Pt 1): 132822, 2022 Mar.
Article in English | MEDLINE | ID: mdl-34767851

ABSTRACT

Nonsteroidal anti-inflammatory drugs (NSAIDs), including naproxen (NP), diclofenac, ibuprofen, etc., are widely used for fever and pain relief. NP is one of the most widely consumed drugs in the world, because it is available over the counter in many countries. Many studies have proven that NP is not eliminated in conventional water treatment processes and its biodegradation in the environment is also difficult compared to other drugs. Along these lines, we are aware that both the original compound and its metabolites can be found in different destinations in the environment. To assess the environmental exposure and the risks associated with NP, it is important to understand better the environment where they finally reach, the behavior of its original compounds, its metabolites, and its transformation products. In this sense, the purpose of this review is to summarize the current state of knowledge about the introduction and behavior of NP in the environments they reach and highlight research needs and gaps. Likewise, we present the sources, environmental destinations, toxicology, environmental effects, and quantification methodologies.


Subject(s)
Environmental Pollutants , Pharmaceutical Preparations , Water Pollutants, Chemical , Anti-Inflammatory Agents, Non-Steroidal , Diclofenac , Ibuprofen , Naproxen/analysis , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/toxicity
13.
J Environ Manage ; 300: 113694, 2021 Dec 15.
Article in English | MEDLINE | ID: mdl-34537557

ABSTRACT

In recent years, Non-Steroidal Anti-Inflammatory Drugs (NSAIDs) have surfaced as a novel class of pollutants due to their incomplete degradation in wastewater treatment plants and their inherent ability to promote physiological predicaments in humans even at low doses. The occurrence of the most common NSAIDs (diclofenac, ibuprofen, naproxen, and ketoprofen) in river water, groundwater, finished water samples, WWTPs, and hospital wastewater effluents along with their toxicity effects were reviewed. The typical concentrations of NSAIDs in natural waters were mostly below 1 µg/L, the rivers receiving untreated wastewater discharge have often showed higher concentrations, highlighting the importance of effective wastewater treatment. The critical analysis of potential, pathways and mechanisms of microbial degradation of NSAIDs were also done. Although studies on algal and fungal strains were limited, several bacterial strains were known to degrade NSAIDs. This microbial ability is attributed to hydroxylation by cytochrome P450 because of the decrease in drug concentrations in fungal cultures of Phanerochaete sordida YK-624 on incubation with 1-aminobenzotriazole. Moreover, processes like decarboxylation, dehydrogenation, dechlorination, subsequent oxidation, demethylation, etc. also constitute the degradation pathways. A wide array of enzymes like dehydrogenase, oxidoreductase, dioxygenase, monooxygenase, decarboxylase, and many more are upregulated during the degradation process, which indicates the possibility of their involvement in microbial degradation. Specific hindrances in upscaling the process along with analytical research needs were also identified, and novel investigative approaches for future monitoring studies are proposed.


Subject(s)
Pharmaceutical Preparations , Water Pollutants, Chemical , Anti-Inflammatory Agents, Non-Steroidal , Humans , Ibuprofen , Naproxen/analysis , Phanerochaete , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/toxicity
14.
Chemosphere ; 280: 130688, 2021 Oct.
Article in English | MEDLINE | ID: mdl-33962297

ABSTRACT

Non-steroidal anti-inflammatory drugs (NSAIDs) are medications used individually or as mixtures with other pharmaceuticals for the treatment of various illnesses. Their easy accessibility and high human consumption have resulted to their detection at high concentrations in South African water resources. In the present work, an extensive review of the occurrence and ecotoxicological risk assessment of NSAIDs in South African aquatic environment is provided. Reviewed literature suggested ibuprofen, naproxen, diclofenac, ketoprofen and fenoprofen as the most prominent NSAIDs in the South African aquatic environment. Among these NSAIDs, higher concentrations of ibuprofen are common in South African waters. As a result, this drug was found to pose high ecotoxicological risks towards the aquatic organisms with the highest risk quotients of 14.9 and 11.9 found for algae in surface water and wastewater, respectively. Like in other parts of the world, NSAIDs are not completely removed in wastewater treatment plants. Removal efficiencies below 0% due to higher concentrations of NSAIDs in wastewater effluents rather than influents were observed in certain instances. The detection of NSAIDs in sediments and aquatic plants could serve as the important starting step to investigate other means of NSAIDs removal from water. In conclusion, recommendations regarding future studies that could paint a clearer picture regarding the occurrence and ecotoxicological risks posed by NSAIDs in South African aquatic environment are provided.


Subject(s)
Pharmaceutical Preparations , Water Pollutants, Chemical , Anti-Inflammatory Agents, Non-Steroidal/analysis , Anti-Inflammatory Agents, Non-Steroidal/toxicity , Environmental Monitoring , Humans , Ibuprofen/toxicity , Naproxen/analysis , Naproxen/toxicity , Risk Assessment , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/toxicity
15.
Mikrochim Acta ; 188(5): 179, 2021 04 29.
Article in English | MEDLINE | ID: mdl-33914148

ABSTRACT

A core-shell material (UiO@TapbTp) has been developed as an adsorbent and matrix to detect nonsteroidal anti-inflammatory drugs (NSAIDS) by matrix laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) in complex samples. The hybrid material is prepared by growing covalent organic framework (COF, TapbTp) layers in situ on an amino-modified metal-organic framework (MOF, UiO-66-NH2). The combination of the MOF and COF overcomes their individual shortcomings and integrates both of their advantages. Compared with the bare COF and MOF, the core-shell composite exhibits improved enrichment ability and matrix performance. With the help of pre-enrichment under optimized conditions, the limits of detection (LODs) for ketoprofen, naproxen, and aspirin are reduced by nearly 1000 times, with values of 0.001 mg L-1, 0.010 mg L-1, and 0.001 mg L-1, respectively, and the relative standard deviations (RSDs) are all below 12.35%. The good recoveries (84.8-118%) in (spiked) saliva and environmental water sample further verify the applicability of the method in complex samples.


Subject(s)
Anti-Inflammatory Agents, Non-Steroidal/analysis , Aspirin/analysis , Ketoprofen/analysis , Metal-Organic Frameworks/chemistry , Naproxen/analysis , Adsorption , Anti-Inflammatory Agents, Non-Steroidal/chemistry , Aspirin/chemistry , Drinking Water/analysis , Ketoprofen/chemistry , Lakes/analysis , Limit of Detection , Naproxen/chemistry , Saliva/chemistry , Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization/methods , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/chemistry
16.
Anal Bioanal Chem ; 413(7): 1851-1859, 2021 Mar.
Article in English | MEDLINE | ID: mdl-33469709

ABSTRACT

In this work, a liquid-liquid microextraction methodology using solidified floating organic drop (SFODME) was combined with liquid chromatography and UV/Vis detection to determine non-steroidal anti-inflammatory drugs (NSAIDs) naproxen (NPX), diclofenac (DCF), and mefenamic acid (MFN) in tap water, surface water, and seawater samples. Parameters that can influence the efficiency of the process were evaluated, such as the type and volume of the extractor and dispersive solvents, effect of pH, agitation type, and ionic strength. The optimized method showed low detection limits (0.09 to 0.25 µg L-1), satisfactory recovery rates (90 to 116%), and enrichment factors in the range between 149 and 199. SFODME showed simplicity, low cost, speed, and high concentration capacity of the analytes under study. Its use in real samples did not demonstrate a matrix effect that would compromise the effectiveness of the method, being possible to apply it successfully in water samples with different characteristics.


Subject(s)
Anti-Inflammatory Agents, Non-Steroidal/analysis , Chromatography, High Pressure Liquid/methods , Liquid Phase Microextraction/methods , Chemistry, Organic/methods , Diclofenac/analysis , Dodecanol/analysis , Hydrogen-Ion Concentration , Ions , Limit of Detection , Linear Models , Mefenamic Acid/analysis , Methanol , Naproxen/analysis , Osmolar Concentration , Pharmaceutical Preparations/analysis , Reproducibility of Results , Seawater , Solvents , Temperature , Water/analysis , Water Pollutants, Chemical/analysis
18.
Eur J Mass Spectrom (Chichester) ; 26(6): 400-408, 2020 Dec.
Article in English | MEDLINE | ID: mdl-33175578

ABSTRACT

The UV-visible photodegradation of Naproxen (6-methoxy-α-methyl-2-naphthaleneacetic acid, CAS: 22204-53-1), one of the most used and detected non-steroidal anti-inflammatory drugs (NSAIDs) in the world, and its ecotoxicological consequences were investigated in an aqueous medium. The photo-transformation products were analyzed and the structures of photoproducts were elucidated using gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) and high-performance liquid chromatography coupled with ultrahigh-resolution Fourier transform ion cyclotron resonance mass spectrometry (LC-FTICR-MS). Seven photoproducts were detected and characterized, photo-transformation mechanisms have been postulated to rationalize their formation under irradiation. In silico Q.S.A.R. (Quantitative Structure-Activity Relationship) toxicity predictions were performed with the Toxicity Estimation Software Tool (T.E.S.T.) and in vitro assays were carried out on Vibrio fischeri bacteria. Some of the obtained photoproducts exhibit higher potential toxicity than Naproxen itself but the whole toxicity of the irradiated solution is not of major concern.


Subject(s)
Naproxen , Aliivibrio fischeri/drug effects , Gas Chromatography-Mass Spectrometry , Naproxen/analysis , Naproxen/chemistry , Naproxen/radiation effects , Naproxen/toxicity , Photolysis , Quantitative Structure-Activity Relationship , Tandem Mass Spectrometry , Ultraviolet Rays , Water
19.
Environ Monit Assess ; 192(8): 557, 2020 Aug 01.
Article in English | MEDLINE | ID: mdl-32740832

ABSTRACT

Human consumption of non-steroidal anti-inflammatory drugs (NSAIDs) is increasing, which poses a great risk of pollution by these pharmaceuticals on the aquatic environment. Therefore, this study reports the optimization of microwave-assisted extraction using water as a green solvent and hollow fiber liquid-phase microextraction (HF-LPME) methods followed by high-performance liquid chromatography-high resolution mass spectrometry analysis of NSAIDs in wastewater and aquatic plant, Eichhornia crassipes. The optimized MAE resulted in efficient transfer of selected NSAIDs from plant samples into the aqueous phase yielding the recoveries ranging from 91 to115%. A multivariate approach based on half fractional factorial and central composite design was used during the optimization of HF-LPME. Under the optimized conditions, the maximum enrichment factors for naproxen, fenoprofen, diclofenac, and ibuprofen were 49, 126, 93 and 156, respectively. The overall analytical method recoveries ranged from 86 to 116% while the limits of quantitation for wastewater and plant samples ranged from 0.09 to 0.59 µg L-1 and from 0.11 to 0.59 µg kg-1, respectively. The precision of the proposed analytical method which was measured in terms of RSD values did not exceed 5%. Naproxen was the most abundant compound in both wastewater and the Eichhornia crassipes plant samples with concentrations of up to 3.30 µg L-1 and 10.97 µg kg-1, respectively. The detection of NSAIDs in Eichhornia crassipes means this plant has the ability to bioaccumulate pharmaceutical load in surface water.


Subject(s)
Liquid Phase Microextraction , Microwaves , Anti-Inflammatory Agents, Non-Steroidal/analysis , Environmental Monitoring , Humans , Naproxen/analysis
20.
Aquat Toxicol ; 224: 105499, 2020 Jul.
Article in English | MEDLINE | ID: mdl-32416570

ABSTRACT

Pharmaceutical substances are ubiquitous in the aquatic environment and their concentration levels typically range from ng/L up to several µg/L. Furthermore, as those compounds are designed to be highly biologically active, assessing their impacts on non-target organisms is important. Here, we conducted a mesocosm experiment testing a mixture of five pharmaceuticals (diclofenac, carbamazepine, irbesartan, acetaminophen and naproxen) on fish, three-spined stickleback (Gasterosteus aculeatus). The mixture concentration levels were chosen on the basis of the contamination of the Meuse river in Belgium which had been measured previously during a monitoring campaign undertaken in 2015 and 2016. Three nominal mixture concentration levels were tested: the lowest concentration level mixture was composed by environmentally-relevant concentrations that approximate average realistic values for each pharmaceuticals (Mx1); the two other levels were 10 and 100 times these concentrations. Although no impact on stickleback prey was observed, the mixture significantly impaired the survival of female fish introduced in the mesocosms at the highest treatment level without causing other major differences on fish population structure. Impacts on condition factors of adults and juveniles were also observed at both individual and population levels. Using a modelling approach with an individual-based model coupled to a bioenergetic model (DEB-IBM), we concluded that chronic exposure to environmentally-relevant concentrations of five pharmaceuticals often detected in the rivers did not appear to strongly affect the three-spined stickleback populations. Mechanisms of population regulation may have counteracted the mixture impacts in the mesocosms.


Subject(s)
Pharmaceutical Preparations/analysis , Rivers/chemistry , Smegmamorpha/growth & development , Water Pollutants, Chemical/toxicity , Acetaminophen/analysis , Acetaminophen/toxicity , Animals , Belgium , Carbamazepine/analysis , Carbamazepine/toxicity , Diclofenac/analysis , Diclofenac/toxicity , Female , Models, Theoretical , Naproxen/analysis , Naproxen/toxicity , Population Dynamics , Smegmamorpha/physiology , Water Pollutants, Chemical/analysis
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