Screening of sulfonamides in waters based on miniaturized solid phase extraction and microplate spectrophotometric detection

Peixoto, Patrícia S.; Tóth, Ildikó V.; Machado, Sandia; Barreiros, Luísa; Machado, Ana Isabel; Bordalo, Adriano A.; Lima, José L.F.C.; Segundo, Marcela A.

doi:10.1039/c7ay02624b

Cited by 10 publications

(8 citation statements)

References 38 publications

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“…Thus, the disk conditioning with organic solvents (acetone, isopropanol and methanol) allows the reduction of surface tension and the solvation of the hydrocarbon chains. On the other hand, the colored product of the SMZ and DMACA reaction was visualized on the surface of the Empore™ disks even without conditioning, as demonstrated in previous research [43]. Despite the general composition of the AttractSPE™ and Empore™ disks being the same (sulfonated styrene divinylbenzene entrapped in a matrix of inert PTFE), the fabrication of the AttractSPE™ and the Empore™ membranes differ, in the latter leading to a lower surface tension and higher availability of the hydrocarbon chains even without conditioning.…”

Section: Solid Phase Extraction Supportsupporting

confidence: 79%

“…If the surface of the disk became dry before the sample was added, these two steps of the conditioning procedure were repeated. For Empore™ disks, no conditioning was required [43].…”

Section: Methodsmentioning

confidence: 99%

“…The colorimetric reaction between DMACA and aromatic amines, including sulfonamides, is based on the condensation between the formyl group of DMACA and the amino group of sulfonamides, which results in a violet-red, stable-colored product corresponding to a Schiff base (Figure 2) [43,[46][47][48]. Several working parameters related to DMACA and SMZ reactions were evaluated previously [43], where it was found that the color intensity of the reaction product was proportional to the concentration of sulfonamides, as depicted in the spectrum shown in Figure 2. In the present work, this relation was evaluated upon probing at the disk surface, where the reaction product was immobilized and concentrated.…”

Section: Reaction Conditionsmentioning

confidence: 99%

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Development of a Screening Method for Sulfamethoxazole in Environmental Water by Digital Colorimetry Using a Mobile Device

et al. 2022

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Antibiotic resistance is a major health concern of the 21st century. The misuse of antibiotics over the years has led to their increasing presence in the environment, particularly in water resources, which can exacerbate the transmission of resistance genes and facilitate the emergence of resistant microorganisms. The objective of the present work is to develop a chemosensor for screening of sulfonamides in environmental waters, targeting sulfamethoxazole as the model analyte. The methodology was based on the retention of sulfamethoxazole in disks containing polystyrene divinylbenzene sulfonated sorbent particles and reaction with p-dimethylaminocinnamaldehyde, followed by colorimetric detection using a computer-vision algorithm. Several color spaces (RGB, HSV and CIELAB) were evaluated, with the coordinate a_star, from the CIELAB color space, providing the highest sensitivity. Moreover, in order to avoid possible errors due to variations in illumination, a color palette is included in the picture of the analytical disk, and a correction using the a_star value from one of the color patches is proposed. The methodology presented recoveries of 82–101% at 0.1 µg and 0.5 µg of sulfamethoxazole (25 mL), providing a detection limit of 0.08 µg and a quantification limit of 0.26 µg. As a proof of concept, application to in-field analysis was successfully implemented.

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Section: Solid Phase Extraction Supportsupporting

confidence: 79%

“…If the surface of the disk became dry before the sample was added, these two steps of the conditioning procedure were repeated. For Empore™ disks, no conditioning was required [43].…”

Section: Methodsmentioning

confidence: 99%

Section: Reaction Conditionsmentioning

confidence: 99%

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Development of a Screening Method for Sulfamethoxazole in Environmental Water by Digital Colorimetry Using a Mobile Device

et al. 2022

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“…Considering the reproducible conditions attained in flow-based SPE extractions [29,37] using dedicated devices for supporting the disk membrane, commercially available holders aimed for filtration of small volumes were selected, and connected to a multi-channel pump for simultaneous processing of several samples. In this way, sample loading volume and flow rate would be precisely controlled through pump operation [38]. Moreover, removal of water residue can also be performed using the same apparatus by pumping air after sample loading.…”

Section: Implementation Of Disk-based Spe Proceduresmentioning

confidence: 99%

Screening of fluoroquinolones in environmental waters using disk-based solid-phase extraction combined to microplate fluorimetric determination and LC-MS/MS

Peixoto

Tóth

Barreiros

et al. 2019

International Journal of Environmental Analytical Chemistry

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Fluoroquinolones are in the order of the day concerning environmental contamination through anthropogenic activities, resulting in increased risk for antibiotic resistance dissemination. In this context, accessible, low-cost analytical methods are required for implementation of comprehensive surveillance and screening schemes. In this work, we propose a down-scaled disk-based solidphase extraction system from which the eluate can be first screened by miniaturized fluorimetric reading, followed by individual determination of target fluoroquinolones (ciprofloxacin, norfloxacin, and enrofloxacin) by liquid chromatography combined to tandem mass spectrometry. The fluorimetric measurement is based on the intrinsic fluorescence of fluoroquinolones. Diskbased retention was performed after sample acidification (pH 4.0) by mixed-mode cation exchange using polystyrene divinylbenzene sulphonated sorbent. Sample loading was precisely controlled in a dedicated flow system operating at 4.0 mL min −1. Different eluent compositions were tested, with elution performed by 1.00 mL of methanol-ammonium hydroxide (98:2, v/v), with subsequent reading of eluate in both detectors. Quantification was attained for 2-25 µg L −1 range, with LOD values at 1 µg L −1. The proposed approach was successfully applied to estuarine waters from the Douro River, with comparable results to a conventional SPE-LC-MS/MS procedure.

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“…In this context, miniaturization of (bio)chemical reactions and analytical methods is a current trend, using either microchips [ 19 , 20 ] or downscaling under microplate format [ 21 , 22 ], fostering greener methodologies that originate less effluent, consume fewer reagents, and have a lower environmental footprint. Taking into account the need to develop a simple, fast, sensitive, and precise methodology for zinc determination to support pet food formulation using different sources of bioavailable zinc, the objective of this work is to implement a fluorimetric methodology based on FluoZin-1, aiming for the determination of zinc in pet food samples after acid digestion.…”

Section: Introductionmentioning

confidence: 99%

Miniaturized Fluorimetric Method for Quantification of Zinc in Dry Dog Food

Martins

Pereira

Matos³

et al. 2020

Journal of Analytical Methods in Chemistry

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Zinc is an essential trace element for animals in several biological processes, particularly in energy production, and it is acquired from food ingestion. In this context, a microplate-based fluorimetric assay was developed for simple, fast, and low-cost determination of zinc in pet food using 2,2′-((4-(2,7-difluoro-3,6-dihydroxy-4aH-xanthen-9-yl)-3-methoxyphenyl)azanediyl)diacetic acid (FluoZin-1) as fluorescent probe. Several aspects were studied, namely, the stability of the fluorescent product over time, the FluoZin-1 concentration, and the pH of reaction media. The developed methodology provided a limit of detection of 1 μg L−1 in sample acid digests, with a working range of 10 to 200 μg L−1, corresponding to 100–2000 mg of Zn per kg of dry dog food samples. Intraday repeatability and interday repeatability were assessed, with relative standard deviation values < 3.4% (100 μg L−1) and <11.7% (10 μg L−1). Sample analysis indicated that the proposed fluorimetric assay provided results consistent with ICP-MS analysis. These results demonstrated that the developed assay can be used for rapid determination of zinc in dry dog food.

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Screening of sulfonamides in waters based on miniaturized solid phase extraction and microplate spectrophotometric detection

Abstract: A simple and cost-effective screening method for determination of sulfonamides in water is proposed.

Cited by 10 publications

References 38 publications

Development of a Screening Method for Sulfamethoxazole in Environmental Water by Digital Colorimetry Using a Mobile Device

Development of a Screening Method for Sulfamethoxazole in Environmental Water by Digital Colorimetry Using a Mobile Device

Screening of fluoroquinolones in environmental waters using disk-based solid-phase extraction combined to microplate fluorimetric determination and LC-MS/MS

Miniaturized Fluorimetric Method for Quantification of Zinc in Dry Dog Food

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