The method limits of detection (MLOD) of the validated approach were between 4 and 150 pg/L.
This method enabled the analysis of cylindrospermopsin, anatoxin-a, nodularin and seven microcystins (MC-LR, MC-RR, MC-YR, MC-LA, MC-LY, MC-LW, MC-LF).
This work describes the development of a fast, sensitive and robust analytical method for multiclass cyanotoxins determination based on dual solid-phase extraction (SPE) procedure using a polymeric cartridge first Oasis HLB (Waters Corporation, USA), and second, a graphitized non-porous carbon cartridge, SupelcleanTM ENVI-CarbTM (Sigma-Aldrich, USA), followed by ultra-high performance liquid chromatography high-resolution mass spectrometry (SPE-UHPLC-HRMS). For this reason, efficient multiclass analytical methods are needed to assess the level of cyanotoxins in water reservoirs and tackle these problems. The main human hazard may arise from drinking water supply and recreational water use. The increasing frequency of episodes of harmful algal blooms of cyanobacterial origin is a risk for ecosystems and human health.
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Results of analysis of surface water samples demonstrated the ability of the proposed method to analyze ultra-trace levels of antibiotics, without the need for complex manual pretreatment. The precision of the method, as indicated by the relative standard deviation, was 2.4–7.9%. The detection limit for all test compounds by this method was in the range of 0.2–1.5 ng/L, with recoveries of 76.6–118%. The optimization of the analytical methods was discussed, which included optimization of pH of the sample, filtration membrane, Na2EDTA, chromatographic column, formic acid and aqueous ammonia in mobile phase. The analyte was eluted by the mobile phase during on-line SPE and separated on an Acquity BEH130 column, detected by tandem mass spectrometry, and quantified using an external standard method. Aliquots of the water samples (5 mL) were filtered through a membrane and enriched on an on-line polymeric column with hydrophilic–lipophilic balance (HLB). The enrichment and analysis conditions were optimized for the determination of trace concentrations (nanogram per liter). Samples demonstrated that the proposed method has theĪbility to determine microcystins and nodularin without theĪ method was developed for the determination of 33 antibiotics belonging to 4 different antibiotic groups, including sulfonamides (16), fluoroquinolones (12), macrolides (1), and tetracyclines (4) in water samples using on-line solid-phase extraction-ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (on-line SPE-UPLC-MS/MS). The results of the analysis of surface water Of the method, indicated by the relative standard deviation,
Under the optimized conditions, the methodĭetection limits for all of the targets ranged from 1.4 toģ.3 ng/L with the recoveries from 85.5 to 121%. Using tandem mass spectrometry, and quantified by external Were separated by Acquity BEH130 column, detected (HLB) polymeric column and eluted by mobile phase. The water sample wasĮnriched and purified by a hydrophilic–liphophilic balance Aliquots ofĥmL water sample were directly injected into on-line SPE after Mass spectrometry (on-line SPE-UPLC-MS/MS). Liquid chromatography – electrospray ionization tandem In surface water at nanogram per liter concentrations wasĭeveloped based on on-line solid-phase extraction ultra-performance A method for determining seven microcystins and nodularin
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