Development of a multiresidue quantitative screening method based on pulsed amperometric detection at a glassy carbon electrode for sulfonamides monitoring in foodstuffs of animal origin

Article

Author: Croce, Lucia ; Palermo, Carmen ; Centonze, Diego

A new effective quantitative screening method was developed to detect sulfonamides (SAs) in foodstuffs of animal origin. The method was based on pulsed amperometric detection (PAD) at a glassy carbon electrode (GCE) coupled with a reversed-phase high performance liquid chromatographic separation (RP-HPLC). First, SAs electrochemical behaviour at GCE was investigated by cyclic voltammetry (CV) experiments. In the light of the CV results, a new three-step waveform for pulsed amperometric detection of SAs was designed and optimized by performing flow injection analysis (FIA) of SAs standard solutions. The optimized PAD waveform ensured an excellent response stability and sensitivity with respect to the direct current detection at constant potential. PAD was then applied to detect SAs after RP-HPLC in gradient mode by using a typical organic mobile phase containing acetate buffer, acetonitrile and methanol. The developed method showed, for all the SAs investigated, very low limits of detection and quantification, in the range 2.1-2.7 μg L^-1 and 6.9-9.0 μg L^-1, respectively, and a wide linear range (up to 0.5 mg L^-1). Method selectivity was tested by comparing the chromatograms of SAs mix standard solutions, blank purified milk samples (without SAs) and spiked purified milk samples. Excellent values of precision under repeatability (1.0-5.0 %, n = 6) and within-laboratory reproducibility (11.2-18.6 %, n = 18) conditions, and recoveries (94-105 %) were obtained.

01 Jul 2025·Separation and Purification Technology

Hydroquinone enhanced Cu(II)/peroxymonosulfate for the degradation of sulfonamide antibiotics under acidic pH conditions

Author: Lv, Xiaoli ; Huang, Xianfeng ; Xiao, Jibo ; Cai, Anhong ; Wang, Tianhong ; Zhao, Min ; Zhang, Hui

The Cu(II)-mediated activation of peroxymonosulfate (PMS) has been studied for the degradation of contaminants due to its ability to produce reactive species.However, the yield of reactive species generated from Cu(II)/PMS is relatively low under acidic conditions due to the slow conversion rate of metal valence states, which limits its application prospects.Herein, we found that the introduction of hydroquinone (HQ) in the Cu(II)/PMS system can accelerate the activation of PMS by promoting the redox cycling of Cu(II)/Cu(I), thereby achieving efficient destruct of sulfonamide antibiotics.The degradation rate constants of six sulfonamide antibiotics by HQ/Cu(II)/PMS system was 5-8 times of that by Cu(II)/PMS system under pH 3.0.Both hydroxyl radical (HO.) and singlet oxygen (1O₂) participated in the degradation of sulfamethoxazole (SMX, a representative sulfonamide antibiotic), and the former played the most important role.HQ improved the reduction of Cu(II) to Cu(I) due to the electron-donating capacity of hydroxyl in HQ, thereby promoting PMS decomposition to produce more HO. under acidic conditions.The presence of humic acid (HA) and low concentration of Cl^- presented the inhibitory effect on SMX degradation, while the degradation of SMX was promoted in the presence of high concentration of Cl^-.The addition of NO₃^- and SO₄^2- has almost no effect on the removal of SMX.The degradation pathways of SMX by HQ/Cu(II)/PMS system mainly involved in the S-N cleavage and amino oxidationThe significant enhancement effects were still observed in actual wastewater treatment by Cu(II)/PMS system after introduction of HQ.

01 Jun 2025·Talanta

Improving detection sensitivity of SALDI-MS by constructing patterned composite hierarchical structures

Article

Author: Zhao, Hongkun ; Lu, Nan ; Wang, Yalei ; Zhai, Jingtong ; Dou, Shuzhen ; Lu, Jiaxin ; Chen, Chunning

Surface-Assisted Laser Desorption/Ionization Mass Spectrometry (SALDI-MS) is a prominent tool for detecting small molecules; however, enhancing its detection sensitivity remains a significant challenge. Two strategies are commonly employed to enhance detection sensitivity: enriching analytes through substrate modification and improving the laser desorption/ionization efficiency of the substrate. In this study, we developed a patterned composite hierarchical structure as a SALDI-MS substrate to improve detection sensitivity. The substrate consists of Si nanopillars and Au nanoparticles, and is patterned with hydrophilic spots and hydrophobic surrounding area. The signal intensity of tetrabutylammonium iodide and sulfacetamide is enhanced by 100-fold and 60-fold, respectively, compared to testing on the Si nanopillars array. The sensitivity enhancement on this substrate is primarily attributed to two factors: first, the analytes are enriched on the hydrophilic spots; and second, the laser desorption/ionization efficiency is improved by the introduction of Schottky barriers through the deposition of Au nanoparticles on Si nanopillars, which extends the lifetime of electron-holes. This design offers high sensitivity, with the lowest detection concentrations for dyes, amino acids and sulfonamides reaching the attomole level. Patterned modifications overcome common issues with super-hydrophobic substrate, such as difficult analyte addition and droplet slippage. The pattern also ensures excellent detection reproducibility, with relative standard deviations (RSD) of 2.4 % across different areas of the same substrate and 6.36 % across different substrates. The substrate is suitable for detecting trace levels of dyes and sulfonamides in river water and seafood extract, demonstrating its potential for analyzing real samples.

100 Deals associated with Sulfamonomethoxine

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KEGG	Wiki	ATC	Drug Bank
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Gastroenteritis	China	-	-
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