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1.
J Pharm Sci ; 2024 Jul 04.
Article in English | MEDLINE | ID: mdl-38971409

ABSTRACT

A new regression model is presented which offers flexibility, freedom from subjective determinations of linear range, and very wide applicability to measurement systems of industrial importance. This "progressive decay" model starts as a deceptively simple ordinary differential equation. We show here that its solution faithfully describes real but seemingly unconnected data from a plate-based assay for quantitation of RNA with RiboGreen® and dissolution data for a triple fixed-dose combination solid oral dosage form.

2.
Int J Mol Sci ; 25(11)2024 May 28.
Article in English | MEDLINE | ID: mdl-38892094

ABSTRACT

Alzheimer's Disease (AD), a prevalent neurodegenerative disorder, is the primary cause of dementia. Despite significant advancements in neuroscience, a definitive cure or treatment for this debilitating disease remains elusive. A notable characteristic of AD is oxidative stress, which has been identified as a potential therapeutic target. Polyphenols, secondary metabolites of plant origin, have attracted attention due to their potent antioxidant properties. Epidemiological studies suggest a correlation between the consumption of polyphenol-rich foods and the prevention of chronic diseases, including neurodegenerative disorders, which underscores the potential of polyphenols as a therapeutic strategy in AD management. Hence, this comprehensive review focuses on the diverse roles of polyphenols in AD, with a particular emphasis on neuroprotective potential. Scopus, ScienceDirect, and Google Scholar were used as leading databases for study selection, from 2018 to late March 2024. Analytical chemistry serves as a crucial tool for characterizing polyphenols, with a nuanced exploration of their extraction methods from various sources, often employing chemometric techniques for a holistic interpretation of the advances in this field. Moreover, this review examines current in vitro and in vivo research, aiming to enhance the understanding of polyphenols' role in AD, and providing valuable insights for forthcoming approaches in this context.


Subject(s)
Alzheimer Disease , Neuroprotective Agents , Polyphenols , Alzheimer Disease/metabolism , Alzheimer Disease/drug therapy , Polyphenols/therapeutic use , Polyphenols/chemistry , Polyphenols/pharmacology , Humans , Neuroprotective Agents/therapeutic use , Neuroprotective Agents/pharmacology , Animals , Oxidative Stress/drug effects , Antioxidants/therapeutic use , Antioxidants/pharmacology , Neuroprotection/drug effects
3.
BMC Chem ; 18(1): 118, 2024 Jun 26.
Article in English | MEDLINE | ID: mdl-38926795

ABSTRACT

Mathematical manipulation technique has proven to be a very powerful tool for efficient processing and handling of highly overlapped spectra. This work introduced two green and sustainable approaches for the successful recovery of the ternary mixture, Tylosin tartarate (TYL), Sulfadimdine (SLD), and Trimethoprim (TRI). The approaches were constructed using three different methods, derivative ratio spectrum zero-crossing method (DRSZ), double divisor ratio spectra derivative method (DDRD), and factorized derivative ratio method coupled with spectrum subtraction (FDRM-SS). The two approaches succeeded in recovering the three drugs (Linearity range achieved were 0.5-5 µg/mL for TYL, 0.3-1.3 µg/mL for SLD, and 0.3-5 µg/mL for TRI), giving convenient standard deviations and satisfactory recovery percentages. The recommended methods have been verified in accordance with (ICH) guidelines. When the results were statistically compared to the official methods, no significant difference was found. Both AGREE-Analytical GREEnness Metric Approach and Software, and White Analytical Chemistry (WAC) RGB model gave scores of 0.93 and 97.2%, respectively, which proved that the approaches were eco-friendly and abiding by the sustainability principles.

4.
J Mass Spectrom ; 59(7): e5064, 2024 Jul.
Article in English | MEDLINE | ID: mdl-38873895

ABSTRACT

Mass spectrometry-based approaches to assess protein conformation have become widely utilized due to their sensitivity, low sample requirements, and broad applicability to proteins regardless of size and environment. Their wide applicability and sensitivity also make these techniques suitable for the analysis of complex mixtures of proteins, and thus, they have been applied at the cell and even the simple organism levels. These works are impressive, but they predominately employ "bottom-up" workflows and require proteolytic digestion prior to analysis. Once digested, it is not possible to distinguish the proteoform from which any single peptide is derived and therefore, one cannot associate distal-in primary structure-concurrent post-translational modifications (PTMs) or covalent labels, as they would be found on separate peptides. Thus, analyses via bottom-up proteomics report the average PTM status and higher-order structure (HOS) of all existing proteoforms. Second, these works predominately employ promiscuous reagents to probe protein HOS. While this does lead to improved conformational resolution, the formation of many products can divide the signal associated with low-copy number proteins below signal-to-noise thresholds and complicate the bioinformatic analysis of these already challenging systems. In this perspective, I further detail these limitations and discuss the positives and negatives of top-down proteomics as an alternative.


Subject(s)
Mass Spectrometry , Protein Conformation , Protein Footprinting , Protein Processing, Post-Translational , Proteins , Proteomics , Mass Spectrometry/methods , Protein Footprinting/methods , Proteins/chemistry , Proteins/analysis , Proteomics/methods
5.
J Environ Sci Health B ; : 1-14, 2024 Jun 10.
Article in English | MEDLINE | ID: mdl-38853697

ABSTRACT

Selected wild-growing edible fungi (Boletus edulis, Neoboletus luridiformis, Cantharellus cibarius, Macrolepiota procera, Amanita rubescens, Russula virescens, Lycoperdon perlatum, and Flammulina velutipes) along with the poisonous medicinal species Amanita muscaria were collected from five sites in the Bohemian Forest, the Czech Republic and analyzed regarding the contents of 19 elements (Ag, Al, As, Be, Ca, Cd, Co, Cr, Cu, Fe, Li, Mg, Mn, Ni, Pb, Rb, Se, Tl, and Zn) in their fruiting bodies. The contents of the elements as well as bioconcentration factors (ratios of the element content in dry matter of the mushroom to the content in the soil; BCF) were significantly species dependent. In general, the analysis revealed the most intensive accumulation of Cd, Rb, Ag, Cu, Se, and Zn in the studied mushrooms. B. edulis accumulated Ag, Se, Cd, Rb, Cu, and Zn with average BCF of 31, 25, 18, 13, 3.9, and 2.6, respectively. On the other hand, A. rubescens accumulated Cd, Rb, Ag, Cu, Zn, and As (BCF of 41, 27, 4.8, 3.3, 2.1, and 1.4). The data concerning the detrimental elements in sporocarps of edible mushrooms indicate no negative effect on human health if the fungi are consumed occasionally or as a delicacy.

6.
Biomed Chromatogr ; 38(8): e5928, 2024 Aug.
Article in English | MEDLINE | ID: mdl-38924173

ABSTRACT

The literature reveals gaps in the availability of green analytical methods for assessing products containing gatifloxacin (GFX), a fluoroquinolone. Presently, method development is supported by tools such as the National Environmental Methods Index (NEMI) and Eco-Scale Assessment (ESA), which offer objective insights into the environmental friendliness of analytical procedures. The objective of this work was to develop and validate a green method by the NEMI and ESA to quantify GFX in eye drops using HPLC. The method utilized a C8 column (4.6 × 150 mm, 5 µm), with a mobile phase of purified water containing 2% acetic acid and ethanol (70:30, v/v). The injection volume was 10 µL and the flow rate was 0.7 mL/min in isocratic mode at 25°C, with detection performed at 292 nm. The method demonstrated linearity in the range of 2-20 µg/mL, and precision at intra-day (relative standard deviation [RSD] 1.44%), inter-day (RSD 3.45%), and inter-analyst (RSD 2.04%) levels. It was selective regarding the adjuvants of the final product (eye drops) and under forced degradation conditions. The method was accurate (recovery 101.07%) and robust. The retention time for GFX was approximately 3.5 min. The greenness of the method, as evaluated by the NEMI, showed four green quadrants, and by ESA, it achieved a score of 88.


Subject(s)
Gatifloxacin , Green Chemistry Technology , Limit of Detection , Ophthalmic Solutions , Gatifloxacin/analysis , Gatifloxacin/chemistry , Chromatography, High Pressure Liquid/methods , Reproducibility of Results , Green Chemistry Technology/methods , Linear Models , Ophthalmic Solutions/chemistry , Ophthalmic Solutions/analysis , Fluoroquinolones/analysis , Fluoroquinolones/chemistry
7.
J Biol Chem ; 300(7): 107458, 2024 Jun 08.
Article in English | MEDLINE | ID: mdl-38857862

ABSTRACT

The function of endogenous cell-cell signaling peptides relies on their interactions with cognate receptors, which in turn are influenced by the peptides' structures, necessitating a comprehensive understanding of the suite of post-translational modifications of the peptide. Herein, we report the initial characterization of putative peptide isomerase enzymes extracted from R. norvegicus, A. californica, and B. taurus tissues. These enzymes are both tissue and substrate-specific across all three organisms. Notably, the lungs of the mammalian species, and the central nervous system of the mollusk displayed the highest isomerase activity among the examined tissues. In vitro enzymatic conversion was observed for several endogenous peptides, such as the tetrapeptide GFFD in A. californica, and mammalian neuropeptide FF in R. norvegicus and B. taurus. To understand their mode of action, we explored the effects of several inhibitors on these enzymes, which suggest common active site residues. While further characterization of these enzymes is required, the investigations emphasize a widespread and overlooked enzyme activity related to the creation of bioactive peptides.

8.
J Pharm Biomed Anal ; 248: 116317, 2024 Jun 19.
Article in English | MEDLINE | ID: mdl-38936170

ABSTRACT

An instrumental-free, high-throughput assay has been developed for the quantification of thiocyanate in human saliva. The proposed green method is based on the rapid reaction of the analyte with Fe(III) under acidic pH in a microplates format to form a colored complex that is captured as an image by an overhead book scanner. Optimization included the effects of the amount concentration of Fe(III), acidity and reaction time / complex stability using a total volume of 300 µL per well. Validation towards the matrix effect was focused on the specific application and was performed using both artificial and human saliva. The linearity of the developed assay was up to 500 µM thiocyanate offering a lower limit of quantification (LLOQ) of 30 µM. The green potentials were evaluated by both the Green Analytical Procedure (GAPI) and Blue Applicability Grade (BAGI) indexes. The thiocyanate content in the saliva of non-smoking volunteers ranged between 750 and 1350 µΜ, while elevated concentrations were verified in smoking individuals (1860-3080 µΜ). Statistical agreement with a corroborative method was assessed using the Bland-Altman plot.

9.
J Chem Educ ; 101(2): 675-681, 2024 Feb 13.
Article in English | MEDLINE | ID: mdl-38939529

ABSTRACT

Artificial intelligence (AI) is rapidly transforming our world, making it imperative to educate the next generation about both the potential benefits and challenges associated with AI. This study presents a cross-disciplinary curriculum that connects AI and chemistry disciplines in the high school classroom. Particularly, we leverage machine learning (ML), an important and simple application of AI to instruct students to build an ML-based virtual pH meter for high-precision pH read-outs. We used a "codeless" and free ML neural network building software - Orange, along with a simple chemical topic of pH to show the connection between AI and chemistry for high-schoolers who might have rudimentary backgrounds in both disciplines. The goal of this curriculum is to promote student interest and drive in the analytical chemistry domain and offer insights into how the interconnection between chemistry and ML can benefit high-school students in science learning. The activity involves students using pH strips to measure the pH of various solutions with local relevancy and then building an ML neural network model to predict the pH value based on color changes of pH strips. The integrated curriculum increased student interest in chemistry and ML and demonstrated the relevance of science to their daily lives and global issues. This approach is transformative in developing a broad spectrum of integration topics between chemistry and ML and understanding their global impacts.

10.
Molecules ; 29(12)2024 Jun 16.
Article in English | MEDLINE | ID: mdl-38930935

ABSTRACT

Antimony (Sb) contamination poses significant environmental and health concerns due to its toxic nature and widespread presence, largely from anthropogenic activities. This study addresses the urgent need for an accurate speciation analysis of Sb, particularly in water sources, emphasizing its migration from polyethylene terephthalate (PET) plastic materials. Current methodologies primarily focus on total Sb content, leaving a critical knowledge gap for its speciation. Here, we present a novel analytical approach utilizing frontal chromatography coupled with inductively coupled plasma mass spectrometry (FC-ICP-MS) for the rapid speciation analysis of Sb(III) and Sb(V) in water. Systematic optimization of the FC-ICP-MS method was achieved through multivariate data analysis, resulting in a remarkably short analysis time of 150 s with a limit of detection below 1 ng kg-1. The optimized method was then applied to characterize PET leaching, revealing a marked effect of the plastic aging and manufacturing process not only on the total amount of Sb released but also on the nature of leached Sb species. This evidence demonstrates the effectiveness of the FC-ICP-MS approach in addressing such an environmental concern, benchmarking a new standard for Sb speciation analysis in consideration of its simplicity, cost effectiveness, greenness, and broad applicability in environmental and health monitoring.


Subject(s)
Antimony , Mass Spectrometry , Polyethylene Terephthalates , Antimony/analysis , Antimony/chemistry , Polyethylene Terephthalates/chemistry , Mass Spectrometry/methods , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/chemistry , Environmental Monitoring/methods
11.
J Pharm Biomed Anal ; 248: 116270, 2024 May 31.
Article in English | MEDLINE | ID: mdl-38870836

ABSTRACT

The misuse of pregabalin has become a significant issue over the last decade. Consequently, there is a growing demand for a sensitive and selective method for its determination. In this study, an eco-friendly cobalt-doped carbon quantum dots (CQDs) have been fabricated and applied as nanoprobes for the fluorometric determination of pregabalin. The CQDs were synthesized through mixed doping with non-metallic atoms such as nitrogen and sulfur, and a metal ion, cobaltous ion, via a microwave-assisted method in just 1.5 min. The synthesized Co-NS-CQDs exhibited advantageous characteristics, including rapid response times, compatibility with various pH levels, exceptional detection limits, high sensitivity, and excellent selectivity. The Co-NS-CQDs exhibited a high quantum yield (55 %) relative to NS-CQDs (38 %), with blue emissive light at 438 nm. The assessment of pregabalin was based on its enhancement effect on the native fluorescence intensity of CQDs. The proposed method had a good linearity over the range of 25-250 µg/mL, with a limit of detection of 4.17 µg/mL and a limit of quantitation of 12.63 µg/mL, respectively. The prepared NS-CQDs have been successfully applied for the pregabalin determination in pharmaceutical capsules, with excellent % recovery (98-102 %). The greenness of the developed method has been investigated using different greenness metrics, in comparison with the reported RP HPLC method. The greenness characteristics of the method originated from the synthesis of CQDs, utilizing sustainable, readily available, and cost-effective starting materials.

12.
Spectrochim Acta A Mol Biomol Spectrosc ; 319: 124521, 2024 Oct 15.
Article in English | MEDLINE | ID: mdl-38830329

ABSTRACT

The USFDA recently approved mirabegron, a novel once-daily ß-3 adrenoceptor agonist for oral administration, as a transformative treatment for overactive bladder. Despite the existence of numerous analytical methods for the assay and bioanalysis of mirabegron, it's perplexing that none have explored the domain of microwave-assisted sensitive spectrofluorimetric method for mirabegron estimation, even after extensive literature review. Adding to the enigma is the insistence of current analytical methods on using expensive and harmful organic solvents, posing a threat to marine life and the broader environment. Recently, the white analytical chemistry approach has been introduced to develop analytical methods that are cost-effective, environmentally friendly, and user-friendly. Consequently, a white analytical chemistry-based, sensitive, and eco-friendly spectrofluorimetric estimation of mirabegron has been initiated, using 4-Chloro-7-nitrobenzofurazan as a fluorescent biosensing probe. The development of this robust method involved a series of experiments designed to minimize solvent and time wastage. Through a combination of fractional factorial and Box-Behnken designs, researchers identified the critical variables and optimized the method to perfection. This method was validated according to the stringent ICH Q2 (R2) and USFDA guidelines, ensuring its reliability and accuracy. Once approved, this sensitive spectrofluorimetric method was tested, accurately estimating mirabegron levels in commercial formulations and rat plasma samples. To further enrich the study, a comprehensive evaluation of existing analytical methods was conducted alongside the proposed spectrofluorimetric method, using advanced tools like the AGREE calculator, GAPI software, and RGB model to assess their eco-friendliness and effectiveness in mirabegron estimation.


Subject(s)
Acetanilides , Fluorescent Dyes , Microwaves , Spectrometry, Fluorescence , Thiazoles , Thiazoles/chemistry , Thiazoles/blood , Thiazoles/analysis , Acetanilides/analysis , Acetanilides/blood , Acetanilides/chemistry , Animals , Fluorescent Dyes/chemistry , Spectrometry, Fluorescence/methods , Biosensing Techniques/methods , Green Chemistry Technology/methods , Reproducibility of Results , Rats , Limit of Detection , Male
13.
Talanta ; 277: 126418, 2024 Jun 13.
Article in English | MEDLINE | ID: mdl-38879948

ABSTRACT

Polycyclic aromatic compounds (PACs) encompass a wide variety of organic analytes that have mutagenic and carcinogenic potentials for human health and are recalcitrant in the environment. Evaluating PACs levels in fuel (e.g., gasoline and diesel), food (e.g., grilled meat, fish, powdered milk, fruits, honey, and coffee) and environmental (e.g., industrial effluents, water, wastewater and marine organisms) samples are critical to determine the risk that these chemicals pose. Deep eutectic solvents (DES) have garnered significant attention in recent years as a green alternative to traditional organic solvents employed in sample preparation. DES are biodegradable, have low toxicities, ease of synthesis, low cost, and a remarkable ability to extract PACs. However, no comprehensive assessment of the use of DESs for extracting PACs from fuel, food and environmental samples has been performed. This review focused on research involving the utilization of DESs to extract PACs in matrices such as PAHs in environmental samples, NSO-HET in fuels, and bisphenols in foods. Chromatographic methods, such as gas chromatography (GC) and high-performance liquid chromatography (HPLC), were also revised, considering the sensibility to quantify these compound types. In addition, the characteristics of DES and advantages and limitations for PACs in the context of green analytical chemistry principles (GAC) and green profile based on metrics provide perspective and directions for future development.

14.
J Chromatogr A ; 1729: 465055, 2024 Aug 16.
Article in English | MEDLINE | ID: mdl-38852265

ABSTRACT

Universal microchip isotachophoresis (µITP) methods were developed for the determination of cationic and anionic macrocomponents (active pharmaceutical ingredients and counterions) in cardiovascular drugs marketed in salt form, amlodipine besylate and perindopril erbumine. The developed methods are characterized by low reagent and sample consumption, waste production and energy consumption, require only minimal sample preparation and provide fast analysis. The greenness of the proposed methods was assessed using AGREE. An internal standard addition was used to improve the quantitative parameters of µITP. The proposed methods were validated according to the ICH guideline. Linearity, precision, accuracy and specificity were evaluated for each of the studied analytes and all set validation criteria were met. Good linearity was observed in the presence of matrix and in the absence of matrix, with a correlation coefficient of at least 0.9993. The developed methods allowed precise and accurate determination of the studied analytes, the RSD of the quantitative and qualitative parameters were less than 1.5% and the recoveries ranged from 98 to 102%. The developed µITP methods were successfully applied to the determination of cationic and anionic macrocomponents in six commercially available pharmaceutical formulations.


Subject(s)
Amlodipine , Isotachophoresis , Isotachophoresis/methods , Amlodipine/analysis , Reproducibility of Results , Green Chemistry Technology/methods , Quality Control , Pharmaceutical Preparations/analysis , Pharmaceutical Preparations/chemistry , Perindopril/analysis , Limit of Detection , Electrophoresis, Microchip/methods , Cardiovascular Agents/analysis
15.
Environ Toxicol Chem ; 43(7): 1468-1484, 2024 Jul.
Article in English | MEDLINE | ID: mdl-38726957

ABSTRACT

The primary goal of our review was to systematically explore and compare the state-of-the-art methodologies employed in the detection of pesticides, a critical component of global food safety initiatives. New approach methods in the fields of luminescent nanosensors, chromatography, terahertz spectroscopy, and Raman spectroscopy are discussed as precise, rapid, and versatile strategies for pesticide detection in food items and agroecological samples. Luminescent nanosensors emerge as powerful tools, noted for their portability and unparalleled sensitivity and real-time monitoring capabilities. Liquid and gas chromatography coupled to spectroscopic detectors, stalwarts in the analytical chemistry field, are lauded for their precision, wide applicability, and validation in diverse regulatory environments. Terahertz spectroscopy offers unique advantages such as noninvasive testing, profound penetration depth, and bulk sample handling. Meanwhile, Raman spectroscopy stands out with its nondestructive nature, its ability to detect even trace amounts of pesticides, and its minimal requirement for sample preparation. While acknowledging the maturity and robustness of these techniques, our review underscores the importance of persistent innovation. These methodologies' significance extends beyond their present functions, highlighting their adaptability to meet ever-evolving challenges. Environ Toxicol Chem 2024;43:1468-1484. © 2024 The Authors. Environmental Toxicology and Chemistry published by Wiley Periodicals LLC on behalf of SETAC.


Subject(s)
Pesticides , Spectrum Analysis, Raman , Pesticides/analysis , Environmental Monitoring/methods , Food Contamination/analysis
16.
Spectrochim Acta A Mol Biomol Spectrosc ; 318: 124467, 2024 Oct 05.
Article in English | MEDLINE | ID: mdl-38796892

ABSTRACT

The study aimed to determine the potential of the infrared (IR) spectrophotometric technique for measuring the content of sulphanilamide with the sulfonamide group. The study aimed to obtain the IR spectra of sulfanilamide and use the -SO2 band at 1114.37 for the quantitative assay, determining its area under the curve (AUC). The study gives an alternative approach to existing analytical techniques that require vast amounts of organic solvents, which are costly and can be toxic, thus impacting the environment and increasing the analysis cost. The study evaluated the method's whiteness and greenness by utilizing the Complex green analytical procedure index, analytical GREEness calculator and Red Green Blue algorithm tool. The linierity was found to be 5 to 30 µg/ml. The present study has developed an infrared (IR) spectroscopic method that employs a straightforward sample preparation technique in methanol. The IR spectroscopic method's linearity range was determined to be 5-30 µg/ml. The p-value was 0.001 at 95 % confidence level assuring better recovery. This method is evaluated according to the Q2R1 ICH guideline. It is applicable to routine quality control analysis without pre-extraction using green IR spectroscopy. In conclusion, the study demonstrated that IR spectrophotometric techniques can quantify sulfanilamide while reducing the use of organic solvents, contributing to the green-and-white analytical chemistry approach. The developed methods are reliable, accurate, and cost-effective and have the potential to be implemented in routine analysis of sulfanilamide.


Subject(s)
Spectrophotometry, Infrared , Sulfanilamide , Sulfanilamide/analysis , Sulfanilamide/chemistry , Spectrophotometry, Infrared/methods , Sulfanilamides/analysis , Sulfanilamides/chemistry , Algorithms , Reproducibility of Results
17.
Food Res Int ; 183: 114240, 2024 May.
Article in English | MEDLINE | ID: mdl-38760119

ABSTRACT

Polycyclic aromatic hydrocarbons (PAHs) are carcinogenic organic pollutants found in various environments, notably aquatic ecosystems and the food chain, posing significant health risks. Traditional methods for detecting PAHs in food involve complex processes and considerable reagent usage, raising environmental concerns. This study explores eco-friendly approaches suing solid phases derived from natural sources in matrix solid phase dispersion. We aimed to develop, optimize, and validate a sample preparation technique for seafood, employing natural materials for PAH analysis. Ten natural phases were compared with a commercial reference phase. The methodology involved matrix solid phase dispersion and pressurized liquid extraction, followed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Three solid phases (perlite, sweet manioc starch, and barley) showed superior performance in LC-MS/MS and were further evaluated with gas chromatography-tandem mass spectrometry (GC-MS/MS), confirming perlite as the most effective phase. Validation followed Brazilian regulatory guidelines and European Community Regulation 2021/808/EC. The resulting method offered advantages in cost-effectiveness, reduced environmental impact, cleaner extracts, and enhanced analytical performance compared to the reference solid phase and LC-MS/MS. Proficiency analysis confirmed method reliability, with over 50% alignment with green analytical chemistry principles. In conclusion, this study developed an environmentally sustainable sample preparation technique for seafood analysis using natural solid phases, particularly perlite, for PAH determination.


Subject(s)
Food Contamination , Gas Chromatography-Mass Spectrometry , Polycyclic Aromatic Hydrocarbons , Seafood , Tandem Mass Spectrometry , Polycyclic Aromatic Hydrocarbons/analysis , Seafood/analysis , Tandem Mass Spectrometry/methods , Gas Chromatography-Mass Spectrometry/methods , Chromatography, Liquid/methods , Food Contamination/analysis , Solid Phase Extraction/methods , Reproducibility of Results , Brazil , Green Chemistry Technology/methods
18.
J Hazard Mater ; 472: 134609, 2024 Jul 05.
Article in English | MEDLINE | ID: mdl-38759280

ABSTRACT

Simultaneous rapid screening of multiple drugs of abuse in environmental water facilitates effective monitoring and trend assessments. Herein, a novel porphyrin-based metal organic frameworks modified Ti3C2Tx nanosheets (Cu-TCPP/Ti3C2Tx) composite was prepared and utilized as solid-phase microextraction (SPME) coating for the simultaneous analysis of 21 drugs from water samples. The composite was embedded with matrix-compatible polyacrylonitrile binder to prepare a coated blade with thin and uniform coating layer. Ambient mass spectrometry (MS) technique was used to create a coated blade spray-MS (CBS-MS) method for the quantitative determination of drugs in water samples. High throughput and automated sample preparation were achieved with the use of a Concept 96-well plate system, enabling analysis of 21 drugs of abuse within 1 min per sample, while using only 8 µL of organic solvent for desorption and CBS-MS detection. The developed method showed favorable linearity (R2 ≥ 0.9983) in the range of 0.05 to 10 ng mL-1, low limits of detection (1.5-9.0 ng L-1), sufficient recovery (67.6-133.2%), as well as satisfactory precision (RSDs≤13.5%). This study not only delivers a novel and efficient SPME coating composite, but also demonstrates the excellent performance of a high-throughput, efficient, and green analytical method for determination of drugs in environmental water.


Subject(s)
Mass Spectrometry , Metal-Organic Frameworks , Solid Phase Microextraction , Water Pollutants, Chemical , Water Pollutants, Chemical/analysis , Solid Phase Microextraction/methods , Metal-Organic Frameworks/chemistry , Mass Spectrometry/methods , Titanium/chemistry , Limit of Detection , Illicit Drugs/analysis , Environmental Monitoring/methods , Pharmaceutical Preparations/analysis , Pharmaceutical Preparations/chemistry
19.
Anal Chim Acta ; 1311: 342725, 2024 Jul 04.
Article in English | MEDLINE | ID: mdl-38816162

ABSTRACT

BACKGROUND: The introduction of white analytical chemistry encourages the development of methods characterized by a balance among greenness, productivity/feasibility and analytical performances. In the environmental analysis of emerging contaminants (ECs), for which high sensitivity and specificity are mandatory, the use of green and sustainable sample preparation needs to be coupled to a reliable analytical determination. Herein, an extraction method based on the use of a biodegradable polymeric film (Mater-Bi) and coupled to LC-MS/MS analysis was developed for the sensitive determination of ECs in wastewater. RESULTS: The interaction among a range of ECs and the Mater-Bi film (a commercially available patented blend of polybutylene-terephthalate, starch and fatty acids) was investigated by two sequential experimental designs, to simultaneously study several factors and optimize extraction efficiency. The final method, resembling a fabric phase sorptive extraction, involved pH and ionic strength modification of the sample, 1h extraction and desorption in ethanol. Satisfactory recoveries from real wastewater were obtained for sixteen analytes (56-116 %), as well as excellent precision (inter-day relative standard deviations below 10 % for most compounds). Matrix effect was in the range 88-116 % at the lower pre-concentration factor, but also acceptable in most cases at the higher pre-concentration factor. LODs in matrix, from 0.004 to 0.159 µg L-1, were lower than or comparable to those from recent studies employing green extraction procedures. The method demonstrated its applicability to samples from wastewater treatment plants, allowing quantification of pharmaceuticals and UV filters at the µg L-1 and ng L-1 levels, respectively. SIGNIFICANCE: For the first time, the synthetic biopolymer Mater-Bi, so far unexplored for the use in analytical chemistry, was exploited for a green, simple and extremely cheap extraction protocol. The optimized method is suitable for several ECs, guaranteeing very good accuracy, precision and specificity, also thanks to the LC-MS/MS analysis. The evaluation by green and white analytical chemistry metrics highlighted its superiority to conventional extraction methods.


Subject(s)
Polymers , Tandem Mass Spectrometry , Wastewater , Water Pollutants, Chemical , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/isolation & purification , Polymers/chemistry , Tandem Mass Spectrometry/methods , Wastewater/analysis , Wastewater/chemistry , Chromatography, Liquid/methods
20.
Crit Rev Anal Chem ; : 1-26, 2024 May 16.
Article in English | MEDLINE | ID: mdl-38753210

ABSTRACT

Cyclodextrins belong to a class of cyclic oligosaccharides composing of α-(1,4) linked glucopyranose subunits having a torus-like macro ring shape. Cyclodextrins based materials find a wide range of applications in separation technology due to their unique property to differentiate between enantiomers, positional isomers and functional groups. Conversely, ionic liquids are the non-molecular compounds composed of different anion and cations with low melting point making them a designer and greener solvents. Because of their fascinating properties, the combined effect of cyclodextrin and ionic liquids as cyclodextrin functionalized ionic liquids (CDILs) have nowadays led to an excellent development for their utilization in the area of analytical chemistry. This review focuses mainly on the synthesis of cyclodextrin functionalized ionic liquids and their application in separation techniques like capillary electrophoresis (CE), high-performance liquid chromatography (HPLC) and gas chromatography (GC). The nature of the interactions between CDILs and analytes have also been highlighted in this review.


Synthesis of cyclodextrin functionalized ionic liquids.Separation of model analytes using cyclodextrin functionalized ionic liquids as promising materials.Analytical techniques are basic tools in separation sciences.

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