scholarly journals Multi-Spheres Adsorptive Microextraction (MSAμE)—Application of a Novel Analytical Approach for Monitoring Chemical Anthropogenic Markers in Environmental Water Matrices

Molecules ◽  
2019 ◽  
Vol 24 (5) ◽  
pp. 931 ◽  
Author(s):  
Ana Silva ◽  
Nuno Neng ◽  
José Nogueira

Multi-spheres adsorptive microextraction using powdered activated carbons (ACs) was studied as a novel enrichment approach, followed by liquid desorption and high-performance liquid chromatography with diode array detection (MSAµE(AC)-LD/HPLC-DAD) to monitor caffeine (CAF) and acetaminophen (ACF) traces in environmental matrices. In this study, commercial activated carbons (N, NOX, and R) were tested, with the latter showing a much better performance for the analysis of both anthropogenic drugs. The main parameters affecting the efficiency of the proposed methodology are fully discussed using commercial AC(R). Textural and surface chemistry properties of the ACs sample were correlated with the analytical results. Assays performed on 30 mL of water samples spiked at 10 µg L−1 under optimized experimental conditions, yielding recoveries of 75.3% for ACF and 82.6% for CAF. The methodology also showed excellent linear dynamic ranges for both drugs with determination coefficients higher than 0.9976, limits of detection and quantification of 0.8–1.2 µg L−1 and 2.8–4.0 µg L−1, respectively, and suitable precision (RSD < 13.8%). By using the standard addition method, the application of the present method to environmental matrices, including superficial, sea, and wastewater samples, allowed very good performance at the trace level. The proposed methodology proved to be a feasible alternative for polar compound analysis, showing to be easy to implement, reliable, and sensitive, with the possibility to reuse and store the analytical devices loaded with the target compounds for later analysis.

Molecules ◽  
2020 ◽  
Vol 25 (9) ◽  
pp. 2133
Author(s):  
Samir M. Ahmad ◽  
Bruno B.C. Calado ◽  
Mariana N. Oliveira ◽  
Nuno R. Neng ◽  
J.M.F. Nogueira

In the present work we propose, for the first time, bar adsorptive microextraction coated with carbon-based phase mixtures, followed by microliquid desorption and high performance liquid chromatography-diode array detection (BAμE-μLD/HPLC-DAD) analysis, to enhance the performance of the determination of traces of benzotriazoles (BTRs), benzothiazoles (BTs), and benzenesulfonamide derivatives (BSDs) in environmental water matrices. Assessing six carbon-based sorbents (CA1, CN1, B test EUR, SX PLUS, SX 1, and R) with different selectivity properties allowed us to tailor the best phase mixture (R, 12.5%/CN1, 87.5%) that has convenient porosity, texture, and surface chemistry (pHPZC,mix ~6.5) for trace analysis of benzenesulfonamide, 1-hydroxybenzotriazole, 1H-benzotriazole, 5-methyl-1H-benzotriazole, benzothiazole, and 1,3-benzothiazol-2-ol chemicals in aqueous media. Optimized experimental conditions provided average recoveries ranging from 37.9% to 59.2%, appropriate linear dynamic ranges (5.0 to 120.0 µg L−1; r2 ≥ 0.9964), limits of detection between 1.0 and 1.4 μg L−1, and good precisions (relative standard deviation (RSD) ≤ 9.3%). The proposed methodology (BAμE(R, 12.5%/CN1, 87.5%)-μLD/HPLC-DAD) also proved to be a suitable sorption-based static microextraction alternative to monitor traces of BTRs, BTs, and BSDs in rain, waste, tap, and estuarine water samples. From the data obtained, the proposed approach showed that the BAμE technique with the addition of lab-made devices allows users to adapt the technique to use sorbents or mixtures of sorbents with the best selectivity characteristics whenever distinct classes of target analytes occur simultaneously in the same application.


2021 ◽  
Vol 40 (1) ◽  
pp. 187-203
Author(s):  
Shirley Kholofelo Selahle ◽  
Anele Mpupa ◽  
Philiswa Nosizo Nomngongo

Abstract Neonicotinoid insecticides are widely used to kill and prevent unwanted insects from attacking growing crops. Extensive use of insecticides in various compartments of the environment has led to adverse effect on the health of living organisms. Several analytical methodologies have been reported for extraction and quantification of neonicotinoid insecticides in various matrices. The analytical detection techniques range from traditional to modern or state of the art quantification methods. The traditional analytical techniques include gas chromatography and high-performance liquid chromatography. These methods require extensive sample pretreatment before identification, separation, and quantification of target analytes. Advanced detection techniques refer to the sensor technologies based on optical, biorecognition, molecular imprinted polymers chemical, and piezoelectric. In this review, a summary and explanation of the various traditional analytical and advanced methodologies for extraction, separation, detection, and quantification of neonicotinoid insecticides residue in water samples have been discussed.


2014 ◽  
Vol 4 (1) ◽  
Author(s):  
Bhupander Kumar ◽  
Virendra Kumar Verma ◽  
Chandra Shekhar Sharma ◽  
Avinash B. Akolkar

Phenols and phenolic compounds are ubiquitous contaminants in the environment. Due to toxic potential, some phenolic compounds mainly chlorophenols and nitrophenols have been classified as priority pollutants. They enter into the environment through various sources such as industrial, domestic and vehicular emissions. For compliance of national and international regulations, various analytical methods have been developed for assessment in the environmental matrices. This paper presents quick, easy and reliable method for simultaneous determination of eleven priority phenolic compounds in wastewater using reversed-phase high-performance liquid chromatography and diode array detector. Liquid-liquid extraction technique with dichloromethane in acidic condition was used for the extraction, and chromatographic separation of compounds was carried out on a C18 column with water and methanol as the mobile phase. The following parameters like selectivity/ specificity, linearity (<em>R</em><sup>2</sup>), range, limit of detection (LOD) and quantification (LOQ), precision (repeatability) and accuracy (recovery) were validated for consistent and reliable results. Calibration curves for all compounds were linear (<em>R</em><sup>2</sup>, 0.998-0.999) within the concentration range of 5-125 (μg/mL). The LOD and LOQ of the method ranged between 0.11- 0.61 μg/L and 0.37-2.04 μg/L, respectively. This method was applied to quantify phenolic compounds in wastewater samples from urban drain with good separated peaks, precision and accuracy.


2011 ◽  
Vol 8 (4) ◽  
pp. 419 ◽  
Author(s):  
Janne Rubarth ◽  
Annekatrin Dreyer ◽  
Nils Guse ◽  
Jürgen W. Einax ◽  
Ralf Ebinghaus

Environmental contextPerfluorinated compounds are commonly used chemicals that are detected globally in all environmental matrices. We investigated the extent of contamination by perfluorinated compounds in the red-throated diver, a marine predatory bird, and observed an unusual distribution of perfluorinated compounds in tissues. The data help us to better understand the behaviour of these contaminants in organisms. AbstractTwenty poly- and perfluorinated compounds (PFCs) were investigated in four red-throated divers (Gavia stellata) from the German Baltic Sea sampled in 2005. Concentrations of perfluoroalkyl sulfonates (PFSAs), perfluoroalkyl carboxylates (PFCAs), alkylated perfluoroalkyl sulfonamides, alkylated perfluoroalkyl sulfonamidoethanols and perfluorooctane sulfonamides were determined in blood, brain, fatty tissue, gall bladder, heart, kidney, liver, lung, muscle and spleen by high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). For quantification standard addition was applied. Twelve compounds were detected with average total PFC concentrations ranging from 42 ng g–1 in muscle to 220 ng g–1 in liver samples. Perfluorooctane sulfonate (PFOS) was the major compound in each of the 40 tissue samples. Except for brain, perfluoroundecanoate was the dominant PFCA. In brain samples preferential enrichment of long-chain PFSAs and PFCAs was observed. The total PFC body burden was estimated to 100 ± 39 µg. Multivariate statistical analyses supported the identification of the preferred accumulation ‘location’ of individual PFCs in the birds’ body.


2017 ◽  
pp. 96-103 ◽  
Author(s):  
Gillian Eggleston ◽  
Isabel Lima ◽  
Emmanuel Sarir ◽  
Jack Thompson ◽  
John Zatlokovicz ◽  
...  

In recent years, there has been increased world-wide concern over residual (carry-over) activity of mostly high temperature (HT) and very high temperature (VHT) stable amylases in white, refined sugars from refineries to various food and end-user industries. HT and VHT stable amylases were developed for much larger markets than the sugar industry with harsher processing conditions. There is an urgent need in the sugar industry to be able to remove or inactivate residual, active amylases either in factory or refinery streams or both. A survey of refineries that used amylase and had activated carbon systems for decolorizing, revealed they did not have any customer complaints for residual amylase. The use of high performance activated carbons to remove residual amylase activity was investigated using a Phadebas® method created for the sugar industry to measure residual amylase in syrups. Ability to remove residual amylase protein was dependent on the surface area of the powdered activated carbons as well as mixing (retention) time. The activated carbon also had the additional benefit of removing color and insoluble starch.


2019 ◽  
Vol 15 (6) ◽  
pp. 607-615 ◽  
Author(s):  
Shirley K. Selahle ◽  
Philiswa N. Nomngongo

Background and Objective: A rapid, simple and environmental friendly supramolecular solvent (SUPRAS) based liquid-liquid microextraction method for preconcentration of ciprofloxacin (CIPRO), danofloxacin (DANO) and enrofloxacin (ENRO) from wastewater was developed. Methods: This microextraction technique was coupled with high-performance liquid chromatography equipped with a diode array detector (HPLC-PDA) for detection and separation of the antibiotics. The SUPRAS composed of decanoic acid and tricaprylymethylammonium chloride. Optimum conditions for the extraction and preconcentration of all the antibiotics were obtained using surface response methodology (RSM) based on Box-Behnken design. Results: Under optimum conditions, the limits of detection (LOD) and limit of quantification (LOQ) ranged from 0.06-0.14 µg L−1 and 0.22-0.47 μg L−1, respectively with the preconcentration factors ranging from 153-241. The linear dynamic ranges were between LOQ and 850 µg L−1 with correlation coefficients ranging from 0.9928 to 0.9999. The intra-day (n = 15) and inter-day (n = 5) precisions (expressed in terms of %RSD) for 50 µg L−1 of CIPRO, DANO and ENRO were in the range of 3.3–4% and 4.1–5.8%, respectively. Conclusion: Lastly, the developed method was used for the extraction, preconcentration and quantification of selected CIPRO, DANO and ENRO in influent and effluent wastewater samples.


2002 ◽  
Vol 67 (11) ◽  
pp. 1596-1608 ◽  
Author(s):  
Josef Janča

The effect of miniaturization of the separation channel on the performance of thermal field-flow fractionation (TFFF) is substantiated theoretically. The experiments carried out under carefully chosen experimental conditions proved the high performance of the separation of polymers within an extended range of molar masses from relatively low up to ultrahigh-molar-mass (UHMM) samples. The new micro-TFFF allows to achieve high resolution when applying constant field force operation, it makes easy the programming of the temperature drop which is an advantageous operational mode from the point of view of the time of analysis, and it extends considerably the range of perfectly controlled temperature of the cold wall due to a substantial decrease in the heat energy flux compared with standard size channels.


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