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Pulicharla R.,University of Québec | Brar S.K.,University of Québec | Rouissi T.,University of Québec | Auger S.,Phytronix Technologies | And 3 more authors.
Ultrasonics Sonochemistry | Year: 2017

Residual emerging contaminants in wastewater sludge remain an obstacle for its wide and safe applications such as landfilling and bio-fertilizer. In this study, the feasibility of individual ultrasonication (UlS) and Fenton oxidation (FO) and combined, Ferro-sonication processes (FO) on the degradation of chlortetracycline (CTC) in wastewater sludge was investigated. UlS parameters such as amplitude and sonication time were optimized by response surface methodology (RSM) for further optimization of FS process. Generation of highly reactive hydroxyl radicals in FO and FS processes were compared to evaluate the degradation efficiency of CTC. Increasing in the ratio of hydrogen peroxide and iron concentration showed increased CTC degradation in FO process; whereas in FS, an increase in iron concentration did not show any significant effect (p > 0.05) on CTC degradation in sludge. The estimated iron concentration in sludge (115 mg/kg) was enough to degrade CTC without the addition of external iron. The only adjustment of sludge pH to 3 was enough to generate in-situ hydroxyl radicals by utilizing iron which is already present in the sludge. This observation was further supported by hydroxyl radical estimation with adjustment of water pH to 3 and with and without the addition of iron. The optimum operating UlS conditions were found to be 60% amplitude for 106 min by using RSM. Compared to standalone UlS and FO at 1:1 ratio, FS showed 15% and 8% increased CTC degradation respectively. In addition, UlS of sludge increased estrogenic activity 1.5 times higher compared to FO. FS treated samples did not show any estrogenic activity. © 2016 Elsevier B.V. All rights reserved.

Jourdil J.-F.,Grenoble University Hospital Center | Picard P.,Phytronix Technologies | Meunier C.,Grenoble University Hospital Center | Auger S.,Phytronix Technologies | And 3 more authors.
Analytica Chimica Acta | Year: 2013

In the last decade the quantitation of immunosuppressive drugs has seen vast improvements in analytical methods, optimizing time, accuracy of analysis and cost. Laser Diode Thermal Desorption (LDTD) coupled to Atmospheric Pressure Chemical ionization-tandem mass spectrometry (APCI-MS/MS) represents a technological breakthrough that removes the chromatographic separation step and thereby significantly increases the analytical throughput for the quantitation of cyclosporin A (CsA) in whole blood for therapeutic drug monitoring (TDM).A simple protein precipitation step was used prior to depositing 5. μL of the extract on a 96-well LazWell™ plate and CsA was quantified by LDTD-APCI-MS/MS.The laser pattern was set to ramp from 0 to 45% laser power within 2s. The APCI parameters were set to negative needle voltage (-2μA), carrier gas temperature (30°C) and air flow rate (3Lmin-1). The negative ion single reaction monitoring transitions for CsA and its internal standard cyclosporin D (CsD) were respectively m/z 1201.1/1088.9 and m/z 1214.8/1102.8; obtained with a collision energy of -40V.The analysis was achieved within 9. s from sample to sample.The extraction procedure yielded high recovery (92%; RSD=9.4%, n=6). The lower limit of quantitation was fixed at the first level of calibration: 23.5ngmL-1 (accuracy=112.3%; RSD=9.6%; n=6) and a blank+6 point linear regression up to 965ngmL-1 was used. Using 4 levels of quality control (QC), intra-day assays (n=6) ranged from 93.5 to 95.7% (bias) and from 3.4 to 13.1% (RSD) while inter-day assays (n=6) ranged from 92.9 to 105.3% (bias) and from 4.9 to 7.5% (RSD). An inter-sample contamination of CsA of 2.3% was calculated that was considered negligible with respect to the range of CsA concentrations. Whole blood samples (120) from patients under CsA treatment were analyzed by LDTD-APCI-MS/MS and HPLC-ESI-MS/MS, the gold standard reference method for CsA quantification. Both methods agreed (P≥0.99), with a coefficient of correlation of 0.99 (95% confidence interval 0.982-0.991). The Passing-Bablok regression revealed no significant deviation from linearity (Cusum test, P=0.11). This method seems suitable for use in TDM of CsA. © 2013.

Mohapatra D.P.,University of Québec | Brar S.K.,University of Québec | Tyagi R.D.,University of Québec | Picard P.,Phytronix Technologies | Surampalli R.Y.,U.S. Environmental Protection Agency
Talanta | Year: 2012

In this study, the distribution of the anti-epileptic drug carbamazepine (CBZ) in wastewater (WW) and aqueous and solid phases of wastewater sludge (WWS) was carried out. A rapid and reliable method enabling high-throughput sample analysis for quicker data generation, detection, and monitoring of CBZ in WW and WWS was developed and validated. The ultrafast method (15 s per sample) is based on the laser diode thermal desorption-atmospheric pressure chemical ionization (LDTD-APCI) coupled to tandem mass spectrometry (MS/MS). The optimization of instrumental parameters and method application for environmental analysis are presented. The performance of the novel method was evaluated by estimation of extraction recovery, linearity, precision and detection limit. The method detection limits was 12 ng L-1 in WW and 3.4 ng g -1 in WWS. The intra- and inter-day precisions were 8% and 11% in WW and 6% and 9% in WWS, respectively. Furthermore, three extraction methods, ultrasonic extraction (USE), microwave-assisted extraction (MAE) and accelerated solvent extraction (ASE) with three different solvent condition such as methanol, acetone and acetonitrile:ethyle acetate (5:1, v/v) were compared on the basis of procedural blank and method recovery. Overall, ASE showed the best extraction efficiency with methanol as compared to USE and MAE. Furthermore, the quantification of CBZ in WW and WWS samples showed the presence of contaminant in all stages of the treatment plant. © 2012 Elsevier B.V.

Lemoine P.,University of Montréal | Roy-Lachapelle A.,University of Montréal | Prevost M.,Ecole Polytechnique de Montréal | Tremblay P.,Phytronix Technologies | And 2 more authors.
Toxicon | Year: 2013

A novel approach for the analysis of the cyanobacterial toxin, anatoxin-a (ANA-a), in an environmentally relevant matrix, using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry (LDTD-APCI-MS/MS) is presented. The ultra-fast analysis time (15 s/sample) provided by the LDTD-APCI interface is strengthened by its ability to remove interference from phenylalanine (PHE), an isobaric interference in ANA-a analysis by MS/MS. Thus the LDTD-APCI interface avoids the time consuming steps of derivatization, chromatographic separation or solid-phase extraction prior to analysis. Method development and instrumental parameter optimizations were focused toward signal enhancement of ANA-a, and signal removal of a PHE interference as high as 500 μg/L. External calibration in a complex matrix gave detection and quantification limit values of 1 and 3 μg/L respectively, as well as good linearity (R2 > 0.999) over nearly two orders of magnitude. Internal calibration with clomiphene (CLO) is possible and method performance was similar to that obtained by external calibration. This work demonstrated the utility of the LDTD-APCI source for ultra-fast detection and quantification of ANA-a in environmental aqueous matrices, and confirmed its ability to suppress the interference of PHE without sample preparation or chromatographic separation. © 2012 Elsevier Ltd.

Mohapatra D.P.,University of Québec | Brar S.K.,University of Québec | Tyagi R.D.,University of Québec | Picard P.,Phytronix Technologies | Surampalli R.Y.,U.S. Environmental Protection Agency
Science of the Total Environment | Year: 2013

A comparative study of ultrasonication (US), Fenton's oxidation (FO) and ferro-sonication (FS) (combination of ultrasonication and Fenton's oxidation) advanced oxidation processes (AOPs) for degradation of carbamazepine (CBZ) from wastewater (WW) is reported for the first time. CBZ is a worldwide used antiepileptic drug, found as a persistent emerging contaminant in many wastewater treatment plants (WWTPs) effluents and other aquatic environments. The oxidation treatments of WW caused an effective removal of the drug. Among the various US, FO and FS pre-treatments carried out, higher soluble chemical oxygen demand (SCOD) and soluble organic carbon (SOC) increment (63 to 86% and 21 to 34%, respectively) was observed during FO pre-treatment process, resulting in higher removal of CBZ (84 to 100%) from WW. Furthermore, analysis of by-products formed during US, FO and FS pre-treatment in WW was carried out by using laser diode thermal desorption-atmospheric pressure chemical ionization (LDTD-APCI) coupled to tandem mass spectrometry (MS/MS). LDTD-APCI-MS/MS analysis indicated formation of two by-products, such as epoxycarbamazepine and hydroxycarbamazepine due to the reaction of hydroxyl radicals (OH) with CBZ during the three types of pre-treatment processes. In addition, the estrogenic activity of US, FO and FS pre-treated sample with CBZ and its by-products was carried out by Yeast Estrogen Screen (YES) assay method. Based upon the YES test results, none of the pre-treated samples showed estrogenic activity. © 2012 Elsevier B.V..

Mohapatra D.P.,University of Québec | Brar S.K.,University of Québec | Tyagi R.D.,University of Québec | Picard P.,Phytronix Technologies | Surampalli R.Y.,U.S. Environmental Protection Agency
Science of the Total Environment | Year: 2014

Pharmaceutically active compounds (PhACs) are considered as emerging environmental problem due to their continuous input and persistence to the aquatic ecosystem even at low concentrations. Among them, carbamazepine (CBZ) has been detected at the highest frequency, which ends up in aquatic systems via wastewater treatment plants (WWTPs) among other sources. The identification and quantification of CBZ in wastewater (WW) and wastewater sludge (WWS) is of major interest to assess the toxicity of treated effluent discharged into the environment. Furthermore, WWS has been subjected for re-use either in agricultural application or for the production of value-added products through the route of bioconversion. However, this field application is disputable due to the presence of these organic compounds and in order to protect the ecosystem or end users, data concerning the concentration, fate, behavior as well as the perspective of simultaneous degradation of these compounds is urgently necessary. Many treatment technologies, including advanced oxidation processes (AOPs) have been developed in order to degrade CBZ in WW and WWS. AOPs are technologies based on the intermediacy of hydroxyl and other radicals to oxidize recalcitrant, toxic and non-biodegradable compounds to various by-products and eventually to inert end products. The purpose of this review is to provide information on persistent pharmaceutical compound, carbamazepine, its ecological effects and removal during various AOPs of WW and WWS. This review also reports the different analytical methods available for quantification of CBZ in different contaminated media including WW and WWS. © 2013 Elsevier B.V.

Mohapatra D.P.,University of Québec | Brar S.K.,University of Québec | Picard P.,Phytronix Technologies | Tyagi R.D.,University of Québec
Science of Advanced Materials | Year: 2013

Degradation of bisphenol A (BPA), an endocrine disruptor from water has recently attracted great interest. The primary objective of this work was to prepare ZnO nanoparticles and to study the effect of these nanoparticles on changing the viscosity and zeta potential value of water and simultaneous degradation of BPA. Whey material was used as a dispersant for the preparation of nanoparticles. Analysis of BPA in water was carried out using the ultrafast method (15 s per sample) based on the Laser Diode Thermal Desorption/Atmospheric Pressure Chemical Ionization (LDTD/APCI) coupled to tandem Mass Spectrometry (MS/MS). The whey stabilized nanoparticles displayed lower agglomeration with higher BPA degradation power than those prepared without a stabilizer. The sample with whey stabilized nanoparticle showed lower viscosity and higher zeta potential value in the medium leading to higher degradation of BPA as compared to non-stabilized one. The whey stabilized ZnO nanoparticles were able to degrade 100% BPA from the medium as compared to 60% with the nonstabilized one. The application of a stabilizer for ZnO nanoparticles may substantially enhance the performance of nanoparticles for environmental applications. © 2013 by American Scientific Publishers.

Puicharla R.,University of Québec | Mohapatra D.P.,University of Québec | Brar S.K.,University of Québec | Drogui P.,University of Québec | And 2 more authors.
Journal of Environmental Chemical Engineering | Year: 2014

The addition of high concentration of chlortetracycline (CTC) antibiotic to livestock feed and its resistance toward degradation results in accumulation of CTC in the environment. The strong chelation activity of CTC with metal ions has impact on numerous factors, such as solubility, stability, degradation, and antibacterial activity of CTC in wastewater treatment plant (WWTP). Further, no studies have been carried out on the chelation behavior of CTC with metal ions and its effect on removal efficiency from WWTP. This study attempts to provide the information about CTC distribution in wastewater (WW) and wastewater sludge (WWS) and the role of CTC-metals complexation on this behavior. The analytical method developed in this study combines an existing pre-treatment technique of solid-phase extraction (SPE) with laser diode thermal desorption (LDTD) coupled with tandem mass spectrometry (MS/MS). LDTD-MS/MS analysis has been recently developed to enhance the high throughput capacity in MS by reducing LC-MS/MS runs of 5-30 min to 10-30 s in LDTD-MS/MS run. This study considered the most common, polluting and efficient metal ions (Al(III), Ca(II), Co(II), Cu(II), Fe(III), Mg(II), Ni(II) and Zn(II)) which have a tendency to complex with CTC in WW. Chlortetracycline-metal complex and its mobility in WWTP were well-correlated which showed that CTC concentration in WWS was higher than the WW. These results showed that the water soluble CTC became insoluble and/or relatively less soluble after chelation with metal ions. Furthermore, the results signify the importance of chelation property of CTC and serve as a tool in determining the wastewater treatment plant matrix to be treated and also the type of treatment method to be used. © 2014 Elsevier Ltd.

Mohapatra D.P.,University of Québec | Brar S.K.,University of Québec | Tyagi R.D.,University of Québec | Picard P.,Phytronix Technologies | Surampalli R.Y.,U.S. Environmental Protection Agency
Chemical Engineering Science | Year: 2012

The effect of physico-chemical pre-treatment processes, including ferro-sonication (FS) and partial ozonation (OZ) on the rheology of wastewater sludge (WWS) was investigated. The ferro-sonication and partial ozonation pre-treatment was carried out at optimum conditions: 163min ultrasonication time, 2.71mgL -1 FeSO 47H 2O with pH 2.81 and 26.16mgg -1 SS ozone dose, 16.47min ozonation time at pH 6.23, respectively. Raw and pre-treated sludge depicted non-Newtonian and pseudoplastic behavior with 85%-97% confidence of fit into Bingham, Casson, Power and IPC paste models for solids concentration ranging from 15gL -1 to 35gL -1. Among all the rheological models studied, the power law was more prominent (confidence of fit 90% to 97%) in describing the rheology of the raw and pre-treated sludge. Pre-treatment of WWS led to decrease in pseudoplasticity due to decrease in consistency index K and increase in flow behavior index n. Further, the effects of FS and OZ pre-treatment of WWS on particle size change and on the degradation of bisphenol A (BPA), an endocrine disruptor were also investigated. The results showed a decrease in viscosity and particle size together with a higher degradation of BPA from WWS. BPA degradation by laccases produced by Sinorhizobium meliloti in raw and pre-treated sludge was also determined. Higher activity of laccase (366 UL -1) was observed in partially ozonated sludge, resulting in higher removal of BPA (0.16μgg -1) from WWS. The findings presented in this manuscript are potentially interesting to researcher studying the behavior of sewage sludge in wastewater treatment and removal of trace organic contaminants. © 2012 Elsevier Ltd.

Mohapatra D.P.,University of Québec | Brar S.K.,University of Québec | Daghrir R.,University of Québec | Tyagi R.D.,University of Québec | And 3 more authors.
Science of the Total Environment | Year: 2014

Nanoscale photocatalysts have attracted much attention due to their high surface area to volume ratios. However, due to extremely high reactivity, TiO2 and ZnO nanoparticles prepared using different methods tend to either react with surrounding media or agglomerate, resulting in the formation of much larger flocs and significant loss in reactivity. This work investigates the photocatalytic degradation of carbamazepine (CBZ), a persistent pharmaceutical compound from wastewater (WW) using TiO2 and ZnO nanoparticles prepared in the presence of a water-soluble whey powder as stabilizer. The TiO2 and ZnO nanoparticles prepared in the presence of whey stabilizer displayed much less agglomeration and greater degradation power than those prepared without a stabilizer. Higher photocatalytic degradation of carbamazepine was observed (100%) by using whey stabilized TiO2 nanoparticles with 55min irradiation time as compared to ZnO nanoparticles (92%). The higher degradation of CBZ in wastewater by using TiO2 nanoparticles as compared to ZnO nanoparticles was due to formation of higher photo-generated holes with high oxidizing power of TiO2. The photocatalytic capacity of ZnO anticipated as similar to that of TiO2 as it has the same band gap energy (3.2eV) as TiO2. However, in the case of ZnO, photocorrosion frequently occurs with the illumination of UV light and this phenomenon is considered as one of the main reasons for the decrease of ZnO photocatalytic activity in aqueous solutions. Further, the estrogenic activity of photocatalyzed WW sample with CBZ and its by-products was carried out by yeast estrogen screen (YES) assay method. Based upon the YES test results, none of the samples showed estrogenic activity. © 2014 Elsevier B.V.

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