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Marija Kaštelan-macan - One of the best experts on this subject based on the ideXlab platform.
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Determination of multi-class pharmaceuticals in wastewater by liquid chromatography–tandem mass spectrometry (LC–MS–MS)
Analytical and Bioanalytical Chemistry, 2010Co-Authors: Sandra Babić, Danijela Ašperger, Alka J.m. Horvat, Dragana Mutavdžić Pavlović, Martina Periša, Mirta Zrnčić, Marija Kaštelan-macanAbstract:An analytical method for multi-class pharmaceuticals determination in wastewater has been developed and validated. Target compounds were: sulfonamides (sulfadiazine, Sulfaguanidine, sulfamethazine, sulfamethoxazole), fluoroquinolones (ciprofloxacin, enrofloxacin, norfloxacin), diaminopyrimidine (trimethoprim), anaesthetic (procaine), anthelmintic (praziquantel and febantel), and macrolide (roxithromycin). The method involves pre-concentration and clean-up by solid-phase extraction (SPE) using Strata-X extraction cartridges at pH 4.0. Target analytes were identified and quantitatively determined by liquid chromatography–tandem mass spectrometry using multiple reaction monitoring (MRM). Recoveries were higher than 50% with relative standard deviation (RSD) below 18.3% for three concentrations. Only for Sulfaguanidine was low recovery obtained. Matrix effect was evaluated using matrix-matched standards. The method detection limit (MDL) was between 0.5 and 5 ng L^−1 in spiked water samples. The precision of the method, calculated as relative standard deviation, ranged from 0.5 to 2.0% and from 1.4 to 8.3 for intra-day and inter-day analysis, respectively. The described analytical method was used for determination of pharmaceuticals in effluent wastewaters from the pharmaceutical industry.
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Preparation of Sulfaguanidine-Imprinted Polymers for the Selective Extraction from Waters
2010Co-Authors: Dragana Mutavdžić Pavlović, Sandra Babić, Sara Livazović, Ivan Brnardić, Marija Kaštelan-macanAbstract:Molecularly imprinted polymers (MIPs) are an artificially macromolecular material, which has prearrangement of structure and specific molecular recognition ability [1] because MIPs are synthesised in the presence of target molecules named templates. After removing the template, complementary binding sites are revealed, which exhibit a template-selective binding capacity. [2] In the last few years, MIPs were widely used for the selective enrichment and pretreatment of target compounds existing in complex matrix and molecular imprinting technology has been expanded to the field of environmental analysis. Sulfaguanidine belong to sulfonamide group of antibiotic which are widely used in medicine, animal husbandry and veterinary practice. Because of Sulfaguanidine physicochemical properties and great production and consumption in Croatia, especially in veterinary practice, preparation of molecularly imprinted polymers with Sulfaguanidine as a template molecule is a big challenge. In this study the preparation of molecularly imprinted (MIP) and non-imprinted polymers (NIP) for solid-phase extraction (SPE) of Sulfaguanidine from water samples (pH value 4.00) was presented. For that purpose we used different functional monomers (methacrylic acid, 2-hydroxyethyl methacrylate and 4-vinyl-pyridine), cross-linker (ethylene-glycol-dimethacrylate) and initiator (2, 2’- azobis isobutyronitrile). Retained Sulfaguanidine was eluted from the sorbent with adequate volumes of MeOH:HAc (9:1) and later with pure methanol. Efficiency of Sulfaguanidine elution was checked by 3-aminophenol reagent. The solid-phase extraction efficiency and efficiency of prepared MIP sorbents were determined by thin-layer chromatography. It has been determined that the highest extraction efficiency of Sulfaguanidine was realised with molecularly imprinted polymer based on methacrylic acid. References [1] X. Jiang, W. Tian, C. Zhao, H. Zhang, M. Liu, Talanta 2007, 72, 119–125. [2] N. Zheng, Q. Fu, Y.-Z Li, W-B Chang, Z.-M. Wang, T.-J. Li, Microchemical Journal 2001, 69, 153-158.
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Determination of Veterinary Pharmaceuticals in Production Wastewater by HPTLC-Videodensitometry
Chromatographia, 2007Co-Authors: S. Babić, Danijela Ašperger, Dragana Mutavdžić, A. J. M. Horvat, Marija Kaštelan-macanAbstract:An SPE-HPTLC method for simultaneous identification and quantification of seven pharmaceuticals in production wastewater was optimized and validated. The studied compounds were enrofloxacine, oxytetracycline, trimethoprim, sulfamethazine, sulfadiazine, Sulfaguanidine and penicillin G/procaine. The method involves solid-phase extraction on hydrophilic-lipophilic balance cartridges with methanol and HPTLC analysis of extracts on CN modified chromatographic plates followed by videodensitometry at 254 and 366 nm. Optimization of chromatographic separation was performed by systematic variation of the mobile phase composition using genetic algorithm approach and the optimum mobile phase composition for TLC separation was 0.05 M H_2C_2O_4:methanol = 0.81:0.19 ( v / v ). Linearity of the method was demonstrated in the ranges from 1.5 to 15.0 µg L^−1 for enrofloxacine, 100–500 µg L^−1 for oxytetracycline, 150–600 µg L^−1 for trimethoprim, 300–1100 µg L^−1 for Sulfaguanidine and 100–400 µg L^−1 for sulfamethazine, sulfadiazine and penicillin G/procaine with coefficients of determination higher than 0.991. Mean recoveries ranged from 74.6 to 117.1% and 55.1 to 108.0% for wellspring water and production wastewater, respectively. Only Sulfaguanidine showed lower results. The described method has been applied to the determination of pharmaceuticals in wastewater samples from pharmaceutical industry.
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Solid phase extraction and HPLC determination of veterinary pharmaceuticals in wastewater
Talanta, 2006Co-Authors: Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka J.m. Horvat, Marija Kaštelan-macanAbstract:This work focuses on the application of SPE-HPLC analysis of important veterinary pharmaceuticals from different classes in highly complex wastewater matrix. The pharmaceutical investigated included three sulfonamides (sulfamethazine, sulfadiazine and Sulfaguanidine), a sulfonamide synergist (trimethoprim), a tetracycline (oxytetracycline), a fluoroquinolone (enrofloxacine) and a beta-lactame (penicillin G/procaine). The method involves pre-concentration and clean-up by solid phase extraction (SPE) using Oasis HLB extraction catridges. Final analysis of the selected pharmaceutical compounds was carried out by high-performance liquid chromatography (HPLC) coupled with diode array detector (DAD). Recoveries were ranged from 68.3 to 97.9% with relative standard deviation below 8.4%. Only for Sulfaguanidine low recovery was obtained. Limits of quantification were in the range 1.5-100mug/L depending on pharmaceutical. The described method was applied to the determination of pharmaceuticals in wastewater samples from pharmaceutical industry.
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Determination of Sulfonamides and Trimethoprim in Spiked Water Samples by Solid-Phase Extraction and Thin-Layer Chromatography
JPC – Journal of Planar Chromatography – Modern TLC, 2005Co-Authors: Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka J.m. Horvat, Marija Kaštelan-macanAbstract:This paper describes a method for separation and quantification of a mixture of antibiotics extracted from spiked water samples. The method involves SPE of the analytes from water then analysis of the extract by TLC. Excellent separation of sulfadimidine, sulfadiazine, Sulfaguanidine, and trimethoprim (TMP) was achieved by HPTLC on silica gel F_254 plates with chloroform-methanol, 89 + 11, as mobile phase. Videodensitometric quantification was validated for linearity, precision, limit of detection, and limit of quantification. Limit of detection (LOD) was 0.05 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.1 µg per spot for TMP. Limit of quantification (LOQ) was 0.1 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.2 µg per spot for TMP. The TLC method was tested on extracts obtained, by use of solid-phase extraction, from spiked water samples. The best recovery of these antibiotics was achieved by use of HLB cartridges and elution with acetonitrile. Apparent recoveries were 87.1 ± 8.4 for sulfadiazine, 93.1 ± 6.4 for sulfadimidine, 16.1 ± 7.2 for Sulfaguanidine, and 108.7 ± 23.7 for trimethoprim.
Sandra Babić - One of the best experts on this subject based on the ideXlab platform.
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Determination of multi-class pharmaceuticals in wastewater by liquid chromatography–tandem mass spectrometry (LC–MS–MS)
Analytical and Bioanalytical Chemistry, 2010Co-Authors: Sandra Babić, Danijela Ašperger, Alka J.m. Horvat, Dragana Mutavdžić Pavlović, Martina Periša, Mirta Zrnčić, Marija Kaštelan-macanAbstract:An analytical method for multi-class pharmaceuticals determination in wastewater has been developed and validated. Target compounds were: sulfonamides (sulfadiazine, Sulfaguanidine, sulfamethazine, sulfamethoxazole), fluoroquinolones (ciprofloxacin, enrofloxacin, norfloxacin), diaminopyrimidine (trimethoprim), anaesthetic (procaine), anthelmintic (praziquantel and febantel), and macrolide (roxithromycin). The method involves pre-concentration and clean-up by solid-phase extraction (SPE) using Strata-X extraction cartridges at pH 4.0. Target analytes were identified and quantitatively determined by liquid chromatography–tandem mass spectrometry using multiple reaction monitoring (MRM). Recoveries were higher than 50% with relative standard deviation (RSD) below 18.3% for three concentrations. Only for Sulfaguanidine was low recovery obtained. Matrix effect was evaluated using matrix-matched standards. The method detection limit (MDL) was between 0.5 and 5 ng L^−1 in spiked water samples. The precision of the method, calculated as relative standard deviation, ranged from 0.5 to 2.0% and from 1.4 to 8.3 for intra-day and inter-day analysis, respectively. The described analytical method was used for determination of pharmaceuticals in effluent wastewaters from the pharmaceutical industry.
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Preparation of Sulfaguanidine-Imprinted Polymers for the Selective Extraction from Waters
2010Co-Authors: Dragana Mutavdžić Pavlović, Sandra Babić, Sara Livazović, Ivan Brnardić, Marija Kaštelan-macanAbstract:Molecularly imprinted polymers (MIPs) are an artificially macromolecular material, which has prearrangement of structure and specific molecular recognition ability [1] because MIPs are synthesised in the presence of target molecules named templates. After removing the template, complementary binding sites are revealed, which exhibit a template-selective binding capacity. [2] In the last few years, MIPs were widely used for the selective enrichment and pretreatment of target compounds existing in complex matrix and molecular imprinting technology has been expanded to the field of environmental analysis. Sulfaguanidine belong to sulfonamide group of antibiotic which are widely used in medicine, animal husbandry and veterinary practice. Because of Sulfaguanidine physicochemical properties and great production and consumption in Croatia, especially in veterinary practice, preparation of molecularly imprinted polymers with Sulfaguanidine as a template molecule is a big challenge. In this study the preparation of molecularly imprinted (MIP) and non-imprinted polymers (NIP) for solid-phase extraction (SPE) of Sulfaguanidine from water samples (pH value 4.00) was presented. For that purpose we used different functional monomers (methacrylic acid, 2-hydroxyethyl methacrylate and 4-vinyl-pyridine), cross-linker (ethylene-glycol-dimethacrylate) and initiator (2, 2’- azobis isobutyronitrile). Retained Sulfaguanidine was eluted from the sorbent with adequate volumes of MeOH:HAc (9:1) and later with pure methanol. Efficiency of Sulfaguanidine elution was checked by 3-aminophenol reagent. The solid-phase extraction efficiency and efficiency of prepared MIP sorbents were determined by thin-layer chromatography. It has been determined that the highest extraction efficiency of Sulfaguanidine was realised with molecularly imprinted polymer based on methacrylic acid. References [1] X. Jiang, W. Tian, C. Zhao, H. Zhang, M. Liu, Talanta 2007, 72, 119–125. [2] N. Zheng, Q. Fu, Y.-Z Li, W-B Chang, Z.-M. Wang, T.-J. Li, Microchemical Journal 2001, 69, 153-158.
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Solid phase extraction and HPLC determination of veterinary pharmaceuticals in wastewater
Talanta, 2006Co-Authors: Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka J.m. Horvat, Marija Kaštelan-macanAbstract:This work focuses on the application of SPE-HPLC analysis of important veterinary pharmaceuticals from different classes in highly complex wastewater matrix. The pharmaceutical investigated included three sulfonamides (sulfamethazine, sulfadiazine and Sulfaguanidine), a sulfonamide synergist (trimethoprim), a tetracycline (oxytetracycline), a fluoroquinolone (enrofloxacine) and a beta-lactame (penicillin G/procaine). The method involves pre-concentration and clean-up by solid phase extraction (SPE) using Oasis HLB extraction catridges. Final analysis of the selected pharmaceutical compounds was carried out by high-performance liquid chromatography (HPLC) coupled with diode array detector (DAD). Recoveries were ranged from 68.3 to 97.9% with relative standard deviation below 8.4%. Only for Sulfaguanidine low recovery was obtained. Limits of quantification were in the range 1.5-100mug/L depending on pharmaceutical. The described method was applied to the determination of pharmaceuticals in wastewater samples from pharmaceutical industry.
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Determination of Sulfonamides and Trimethoprim in Spiked Water Samples by Solid-Phase Extraction and Thin-Layer Chromatography
JPC – Journal of Planar Chromatography – Modern TLC, 2005Co-Authors: Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka J.m. Horvat, Marija Kaštelan-macanAbstract:This paper describes a method for separation and quantification of a mixture of antibiotics extracted from spiked water samples. The method involves SPE of the analytes from water then analysis of the extract by TLC. Excellent separation of sulfadimidine, sulfadiazine, Sulfaguanidine, and trimethoprim (TMP) was achieved by HPTLC on silica gel F_254 plates with chloroform-methanol, 89 + 11, as mobile phase. Videodensitometric quantification was validated for linearity, precision, limit of detection, and limit of quantification. Limit of detection (LOD) was 0.05 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.1 µg per spot for TMP. Limit of quantification (LOQ) was 0.1 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.2 µg per spot for TMP. The TLC method was tested on extracts obtained, by use of solid-phase extraction, from spiked water samples. The best recovery of these antibiotics was achieved by use of HLB cartridges and elution with acetonitrile. Apparent recoveries were 87.1 ± 8.4 for sulfadiazine, 93.1 ± 6.4 for sulfadimidine, 16.1 ± 7.2 for Sulfaguanidine, and 108.7 ± 23.7 for trimethoprim.
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Determination of sulfonamides and trimethoprim in spiked water samples by solid-phase extraction and thin-layer chromatography
Journal of Planar Chromatography – Modern TLC, 2005Co-Authors: Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka J.m. Horvat, Marija Kaštelan-macanAbstract:This paper describes a method for separation and quantification of a mixture of antibiotics extracted from spiked water samples. The method involves SPE of the analytes from water then analysis of the extract by TLC. Excellent separation of sulfadimidine, sulfadiazine, Sulfaguanidine, and trimethoprim (TMP) was achieved by HPTLC on silica gel F 254 plates with chloroform-methanol, 89 + 11, as mobile phase. Videodensitometric quantification was validated for linearity, precision, limit of detection, and limit of quantification. Limit of detection ( LOD ) was 0.05 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.1 µg per spot for TMP. Limit of quantification ( LOQ ) was 0.1 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.2 µg per spot for TMP. The TLC method was tested on extracts obtained, by use of solid-phase extraction, from spiked water samples. The best recovery of these antibiotics was achieved by use of HLB cartridges and elution with acetonitrile. Appare...
Rafael Luque - One of the best experts on this subject based on the ideXlab platform.
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Catalytic Versatility of Novel Sulfonamide Functionalized Magnetic Composites
ACS Sustainable Chemistry & Engineering, 2018Co-Authors: Somayeh Ostovar, Pepijn Prinsen, Alfonso Yepez, Hamid Reza Shaterian, Rafael LuqueAbstract:The present work describes two novel magnetic composite catalysts, synthesized by functionalizing the silica/iron oxide composite surface with Sulfaguanidine and sulfadiazine. The Sulfaguanidine functionalized catalyst was found to be very efficient for multicomponent coupling reactions of phenylacetylene with various aldehydes and amines. The sulfadiazine functionalized catalyst was successfully applied in the synthesis of various 1,8-dioxo-octahydroxanthenes in water. Both the Sulfaguanidine and sulfadiazine functionalized catalysts were very active and selective in the alkylation of toluene with benzyl chloride.
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Catalytic Versatility of Novel Sulfonamide Functionalized Magnetic Composites
2018Co-Authors: Somayeh Ostovar, Pepijn Prinsen, Alfonso Yepez, Hamid Reza Shaterian, Rafael LuqueAbstract:The present work describes two novel magnetic composite catalysts, synthesized by functionalizing the silica/iron oxide composite surface with Sulfaguanidine and sulfadiazine. The Sulfaguanidine functionalized catalyst was found to be very efficient for multicomponent coupling reactions of phenylacetylene with various aldehydes and amines. The sulfadiazine functionalized catalyst was successfully applied in the synthesis of various 1,8-dioxo-octahydroxanthenes in water. Both the Sulfaguanidine and sulfadiazine functionalized catalysts were very active and selective in the alkylation of toluene with benzyl chloride
Danijela Ašperger - One of the best experts on this subject based on the ideXlab platform.
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Determination of multi-class pharmaceuticals in wastewater by liquid chromatography–tandem mass spectrometry (LC–MS–MS)
Analytical and Bioanalytical Chemistry, 2010Co-Authors: Sandra Babić, Danijela Ašperger, Alka J.m. Horvat, Dragana Mutavdžić Pavlović, Martina Periša, Mirta Zrnčić, Marija Kaštelan-macanAbstract:An analytical method for multi-class pharmaceuticals determination in wastewater has been developed and validated. Target compounds were: sulfonamides (sulfadiazine, Sulfaguanidine, sulfamethazine, sulfamethoxazole), fluoroquinolones (ciprofloxacin, enrofloxacin, norfloxacin), diaminopyrimidine (trimethoprim), anaesthetic (procaine), anthelmintic (praziquantel and febantel), and macrolide (roxithromycin). The method involves pre-concentration and clean-up by solid-phase extraction (SPE) using Strata-X extraction cartridges at pH 4.0. Target analytes were identified and quantitatively determined by liquid chromatography–tandem mass spectrometry using multiple reaction monitoring (MRM). Recoveries were higher than 50% with relative standard deviation (RSD) below 18.3% for three concentrations. Only for Sulfaguanidine was low recovery obtained. Matrix effect was evaluated using matrix-matched standards. The method detection limit (MDL) was between 0.5 and 5 ng L^−1 in spiked water samples. The precision of the method, calculated as relative standard deviation, ranged from 0.5 to 2.0% and from 1.4 to 8.3 for intra-day and inter-day analysis, respectively. The described analytical method was used for determination of pharmaceuticals in effluent wastewaters from the pharmaceutical industry.
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Determination of Veterinary Pharmaceuticals in Production Wastewater by HPTLC-Videodensitometry
Chromatographia, 2007Co-Authors: S. Babić, Danijela Ašperger, Dragana Mutavdžić, A. J. M. Horvat, Marija Kaštelan-macanAbstract:An SPE-HPTLC method for simultaneous identification and quantification of seven pharmaceuticals in production wastewater was optimized and validated. The studied compounds were enrofloxacine, oxytetracycline, trimethoprim, sulfamethazine, sulfadiazine, Sulfaguanidine and penicillin G/procaine. The method involves solid-phase extraction on hydrophilic-lipophilic balance cartridges with methanol and HPTLC analysis of extracts on CN modified chromatographic plates followed by videodensitometry at 254 and 366 nm. Optimization of chromatographic separation was performed by systematic variation of the mobile phase composition using genetic algorithm approach and the optimum mobile phase composition for TLC separation was 0.05 M H_2C_2O_4:methanol = 0.81:0.19 ( v / v ). Linearity of the method was demonstrated in the ranges from 1.5 to 15.0 µg L^−1 for enrofloxacine, 100–500 µg L^−1 for oxytetracycline, 150–600 µg L^−1 for trimethoprim, 300–1100 µg L^−1 for Sulfaguanidine and 100–400 µg L^−1 for sulfamethazine, sulfadiazine and penicillin G/procaine with coefficients of determination higher than 0.991. Mean recoveries ranged from 74.6 to 117.1% and 55.1 to 108.0% for wellspring water and production wastewater, respectively. Only Sulfaguanidine showed lower results. The described method has been applied to the determination of pharmaceuticals in wastewater samples from pharmaceutical industry.
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Solid phase extraction and HPLC determination of veterinary pharmaceuticals in wastewater
Talanta, 2006Co-Authors: Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka J.m. Horvat, Marija Kaštelan-macanAbstract:This work focuses on the application of SPE-HPLC analysis of important veterinary pharmaceuticals from different classes in highly complex wastewater matrix. The pharmaceutical investigated included three sulfonamides (sulfamethazine, sulfadiazine and Sulfaguanidine), a sulfonamide synergist (trimethoprim), a tetracycline (oxytetracycline), a fluoroquinolone (enrofloxacine) and a beta-lactame (penicillin G/procaine). The method involves pre-concentration and clean-up by solid phase extraction (SPE) using Oasis HLB extraction catridges. Final analysis of the selected pharmaceutical compounds was carried out by high-performance liquid chromatography (HPLC) coupled with diode array detector (DAD). Recoveries were ranged from 68.3 to 97.9% with relative standard deviation below 8.4%. Only for Sulfaguanidine low recovery was obtained. Limits of quantification were in the range 1.5-100mug/L depending on pharmaceutical. The described method was applied to the determination of pharmaceuticals in wastewater samples from pharmaceutical industry.
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Determination of Sulfonamides and Trimethoprim in Spiked Water Samples by Solid-Phase Extraction and Thin-Layer Chromatography
JPC – Journal of Planar Chromatography – Modern TLC, 2005Co-Authors: Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka J.m. Horvat, Marija Kaštelan-macanAbstract:This paper describes a method for separation and quantification of a mixture of antibiotics extracted from spiked water samples. The method involves SPE of the analytes from water then analysis of the extract by TLC. Excellent separation of sulfadimidine, sulfadiazine, Sulfaguanidine, and trimethoprim (TMP) was achieved by HPTLC on silica gel F_254 plates with chloroform-methanol, 89 + 11, as mobile phase. Videodensitometric quantification was validated for linearity, precision, limit of detection, and limit of quantification. Limit of detection (LOD) was 0.05 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.1 µg per spot for TMP. Limit of quantification (LOQ) was 0.1 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.2 µg per spot for TMP. The TLC method was tested on extracts obtained, by use of solid-phase extraction, from spiked water samples. The best recovery of these antibiotics was achieved by use of HLB cartridges and elution with acetonitrile. Apparent recoveries were 87.1 ± 8.4 for sulfadiazine, 93.1 ± 6.4 for sulfadimidine, 16.1 ± 7.2 for Sulfaguanidine, and 108.7 ± 23.7 for trimethoprim.
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Determination of sulfonamides and trimethoprim in spiked water samples by solid-phase extraction and thin-layer chromatography
Journal of Planar Chromatography – Modern TLC, 2005Co-Authors: Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka J.m. Horvat, Marija Kaštelan-macanAbstract:This paper describes a method for separation and quantification of a mixture of antibiotics extracted from spiked water samples. The method involves SPE of the analytes from water then analysis of the extract by TLC. Excellent separation of sulfadimidine, sulfadiazine, Sulfaguanidine, and trimethoprim (TMP) was achieved by HPTLC on silica gel F 254 plates with chloroform-methanol, 89 + 11, as mobile phase. Videodensitometric quantification was validated for linearity, precision, limit of detection, and limit of quantification. Limit of detection ( LOD ) was 0.05 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.1 µg per spot for TMP. Limit of quantification ( LOQ ) was 0.1 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.2 µg per spot for TMP. The TLC method was tested on extracts obtained, by use of solid-phase extraction, from spiked water samples. The best recovery of these antibiotics was achieved by use of HLB cartridges and elution with acetonitrile. Appare...
Alka J.m. Horvat - One of the best experts on this subject based on the ideXlab platform.
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Determination of multi-class pharmaceuticals in wastewater by liquid chromatography–tandem mass spectrometry (LC–MS–MS)
Analytical and Bioanalytical Chemistry, 2010Co-Authors: Sandra Babić, Danijela Ašperger, Alka J.m. Horvat, Dragana Mutavdžić Pavlović, Martina Periša, Mirta Zrnčić, Marija Kaštelan-macanAbstract:An analytical method for multi-class pharmaceuticals determination in wastewater has been developed and validated. Target compounds were: sulfonamides (sulfadiazine, Sulfaguanidine, sulfamethazine, sulfamethoxazole), fluoroquinolones (ciprofloxacin, enrofloxacin, norfloxacin), diaminopyrimidine (trimethoprim), anaesthetic (procaine), anthelmintic (praziquantel and febantel), and macrolide (roxithromycin). The method involves pre-concentration and clean-up by solid-phase extraction (SPE) using Strata-X extraction cartridges at pH 4.0. Target analytes were identified and quantitatively determined by liquid chromatography–tandem mass spectrometry using multiple reaction monitoring (MRM). Recoveries were higher than 50% with relative standard deviation (RSD) below 18.3% for three concentrations. Only for Sulfaguanidine was low recovery obtained. Matrix effect was evaluated using matrix-matched standards. The method detection limit (MDL) was between 0.5 and 5 ng L^−1 in spiked water samples. The precision of the method, calculated as relative standard deviation, ranged from 0.5 to 2.0% and from 1.4 to 8.3 for intra-day and inter-day analysis, respectively. The described analytical method was used for determination of pharmaceuticals in effluent wastewaters from the pharmaceutical industry.
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Solid phase extraction and HPLC determination of veterinary pharmaceuticals in wastewater
Talanta, 2006Co-Authors: Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka J.m. Horvat, Marija Kaštelan-macanAbstract:This work focuses on the application of SPE-HPLC analysis of important veterinary pharmaceuticals from different classes in highly complex wastewater matrix. The pharmaceutical investigated included three sulfonamides (sulfamethazine, sulfadiazine and Sulfaguanidine), a sulfonamide synergist (trimethoprim), a tetracycline (oxytetracycline), a fluoroquinolone (enrofloxacine) and a beta-lactame (penicillin G/procaine). The method involves pre-concentration and clean-up by solid phase extraction (SPE) using Oasis HLB extraction catridges. Final analysis of the selected pharmaceutical compounds was carried out by high-performance liquid chromatography (HPLC) coupled with diode array detector (DAD). Recoveries were ranged from 68.3 to 97.9% with relative standard deviation below 8.4%. Only for Sulfaguanidine low recovery was obtained. Limits of quantification were in the range 1.5-100mug/L depending on pharmaceutical. The described method was applied to the determination of pharmaceuticals in wastewater samples from pharmaceutical industry.
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Determination of Sulfonamides and Trimethoprim in Spiked Water Samples by Solid-Phase Extraction and Thin-Layer Chromatography
JPC – Journal of Planar Chromatography – Modern TLC, 2005Co-Authors: Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka J.m. Horvat, Marija Kaštelan-macanAbstract:This paper describes a method for separation and quantification of a mixture of antibiotics extracted from spiked water samples. The method involves SPE of the analytes from water then analysis of the extract by TLC. Excellent separation of sulfadimidine, sulfadiazine, Sulfaguanidine, and trimethoprim (TMP) was achieved by HPTLC on silica gel F_254 plates with chloroform-methanol, 89 + 11, as mobile phase. Videodensitometric quantification was validated for linearity, precision, limit of detection, and limit of quantification. Limit of detection (LOD) was 0.05 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.1 µg per spot for TMP. Limit of quantification (LOQ) was 0.1 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.2 µg per spot for TMP. The TLC method was tested on extracts obtained, by use of solid-phase extraction, from spiked water samples. The best recovery of these antibiotics was achieved by use of HLB cartridges and elution with acetonitrile. Apparent recoveries were 87.1 ± 8.4 for sulfadiazine, 93.1 ± 6.4 for sulfadimidine, 16.1 ± 7.2 for Sulfaguanidine, and 108.7 ± 23.7 for trimethoprim.
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Determination of sulfonamides and trimethoprim in spiked water samples by solid-phase extraction and thin-layer chromatography
Journal of Planar Chromatography – Modern TLC, 2005Co-Authors: Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka J.m. Horvat, Marija Kaštelan-macanAbstract:This paper describes a method for separation and quantification of a mixture of antibiotics extracted from spiked water samples. The method involves SPE of the analytes from water then analysis of the extract by TLC. Excellent separation of sulfadimidine, sulfadiazine, Sulfaguanidine, and trimethoprim (TMP) was achieved by HPTLC on silica gel F 254 plates with chloroform-methanol, 89 + 11, as mobile phase. Videodensitometric quantification was validated for linearity, precision, limit of detection, and limit of quantification. Limit of detection ( LOD ) was 0.05 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.1 µg per spot for TMP. Limit of quantification ( LOQ ) was 0.1 µg per spot for sulfadimidine, sulfadiazine, and Sulfaguanidine, and 0.2 µg per spot for TMP. The TLC method was tested on extracts obtained, by use of solid-phase extraction, from spiked water samples. The best recovery of these antibiotics was achieved by use of HLB cartridges and elution with acetonitrile. Appare...
