Electrospun sorbents for solid phase extraction (SPE) and colorimetric detection of pesticides
- Authors: Gulamussen, Noor Jehan
- Date: 2014
- Subjects: Sorbents , Electrospinning , Extraction (Chemistry) , Colorimetry , Pesticides , Water -- Pesticide content -- Research
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:4501 , http://hdl.handle.net/10962/d1013241
- Description: The thesis presents the evaluation of polysulfone sorbents for solid phase extraction (SPE) and the development of colorimetric probes for pesticides analysis in water. Through electrospraying and electrospinning techniques, different morphologies of sorbents (particles, beaded fibers and bead-free fibers) were fabricated. The sorbents were morphologically characterized by scanning electron microscopy. Adsorption capacities of sorbents were evaluated by conducting recoveries studies for model pesticides; atrazine, chlorpyrifos and DDT using batch and column SPE modes. Better recovery results were achieved by employing the batch mode of fibers, as values ranged from 98 to 105percent. Further sorbent evaluation was conducted using breakthrough experiments and static experiments. The breakthrough studies indicated that 1700 μL was the sample volume that could be percolated with no breakthrough of the analyte that correspond to a concentration of 150 mg/g of sorbent that can be extracted without any loss of analyte. From static studies, quantities of each model compound adsorbed into the fiber at the equilibrium time were evaluated. The adsorbed atrazine was 65, chlorpyrifos 250 and DDT 400 mg/g of sorbent. Kinetic studies suggested retention mechanism following pseudo first and second order model observed by high correlation coefficients (> 0. 96), demonstrating the fiber affinity to retain both polar and non-polar compounds opening a possibility to be used as sorbent for sample preparation of different classes of pesticides in water. For the second part of the study simple strategies for colorimetric sensing based on silver nanoparticles and polivinylpyrrolidone capped nanoparticles were developed, respectively for atrazine and chlorpyrifos detection. The limits of detection of the methods were 3.32 and 0.88 mg/L for atrazine and chlorpyrifos respectively. The applicability of the probe in real samples was demonstrated by the recoveries studies of tap water varying from 94 to 104 percent. The versatility of the probe was demonstrated by affording a simple, rapid and selective detection of atrazine and chlorpyrifos in the presence of other pesticides by direct analysis without employing any sample handling steps. Attempt to incorporate the probes in a solid support was achieved by using nylon 6 as solid support polymer proving to be fast and useful for on-site detection.
- Full Text:
- Authors: Gulamussen, Noor Jehan
- Date: 2014
- Subjects: Sorbents , Electrospinning , Extraction (Chemistry) , Colorimetry , Pesticides , Water -- Pesticide content -- Research
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:4501 , http://hdl.handle.net/10962/d1013241
- Description: The thesis presents the evaluation of polysulfone sorbents for solid phase extraction (SPE) and the development of colorimetric probes for pesticides analysis in water. Through electrospraying and electrospinning techniques, different morphologies of sorbents (particles, beaded fibers and bead-free fibers) were fabricated. The sorbents were morphologically characterized by scanning electron microscopy. Adsorption capacities of sorbents were evaluated by conducting recoveries studies for model pesticides; atrazine, chlorpyrifos and DDT using batch and column SPE modes. Better recovery results were achieved by employing the batch mode of fibers, as values ranged from 98 to 105percent. Further sorbent evaluation was conducted using breakthrough experiments and static experiments. The breakthrough studies indicated that 1700 μL was the sample volume that could be percolated with no breakthrough of the analyte that correspond to a concentration of 150 mg/g of sorbent that can be extracted without any loss of analyte. From static studies, quantities of each model compound adsorbed into the fiber at the equilibrium time were evaluated. The adsorbed atrazine was 65, chlorpyrifos 250 and DDT 400 mg/g of sorbent. Kinetic studies suggested retention mechanism following pseudo first and second order model observed by high correlation coefficients (> 0. 96), demonstrating the fiber affinity to retain both polar and non-polar compounds opening a possibility to be used as sorbent for sample preparation of different classes of pesticides in water. For the second part of the study simple strategies for colorimetric sensing based on silver nanoparticles and polivinylpyrrolidone capped nanoparticles were developed, respectively for atrazine and chlorpyrifos detection. The limits of detection of the methods were 3.32 and 0.88 mg/L for atrazine and chlorpyrifos respectively. The applicability of the probe in real samples was demonstrated by the recoveries studies of tap water varying from 94 to 104 percent. The versatility of the probe was demonstrated by affording a simple, rapid and selective detection of atrazine and chlorpyrifos in the presence of other pesticides by direct analysis without employing any sample handling steps. Attempt to incorporate the probes in a solid support was achieved by using nylon 6 as solid support polymer proving to be fast and useful for on-site detection.
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Assessment of organochlorine pesticide residues in fish samples from the Okavango Delta, Botswana
- Authors: Mpofu, Christopher
- Date: 2011 , 2011-02-28
- Subjects: Pesticides , Organochlorine compounds , Freshwater fishes -- Effect of pesticides on -- Botswana -- Okavango River Delta , Water -- Pesticide content -- Botswana -- Okavango River Delta , Catfishes -- Botswana -- Okavango River Delta , Tigerfish -- Botswana -- Okavango River Delta , Redbreast tilapia -- Botswana -- Okavango River Delta
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:4404 , http://hdl.handle.net/10962/d1006707 , Pesticides , Organochlorine compounds , Freshwater fishes -- Effect of pesticides on -- Botswana -- Okavango River Delta , Water -- Pesticide content -- Botswana -- Okavango River Delta , Catfishes -- Botswana -- Okavango River Delta , Tigerfish -- Botswana -- Okavango River Delta , Redbreast tilapia -- Botswana -- Okavango River Delta
- Description: This thesis presents an evaluation of the dispersive solid-phase extraction (d-SPE) method referred to as the quick, easy, cheap, effective, rugged and safe (QuEChERS) method for the determination of four organochlorine pesticide residues in fish samples. The pesticides investigated in this study were o, p′-DDT, p, p′-DDE, aldrin and dieldrin. The combined use of Gas Chromatography with an Electron Capture Detector (GC-ECD) and sensitive Time of Flight (TOF) mass detector facilitated the identification of the target analytes. In the absence of certified reference material, the overall analytical procedure was validated by systematic recovery experiments on spiked samples at three levels of 2, 5 and 10 ng/g. The targeted compounds were successfully extracted and their recovery ranged from 76 to 96% with relative standard deviations of less than 13%. The optimum QuEChERS conditions were 2g of fish powder, 10 ml acetonitrile and 1 min shaking time. The optimal conditions were applied to assess the levels of chlorinated pesticides in blunt-tooth catfish (Clarias ngamensis), tigerfish (Hydrocynus vittatus), Oreochromis andersonii and red-breasted tilapia (Tilapia rendalli) from the Okavango Delta, Botswana. Dieldrin, p, p′-DDE and aldrin were detected in all the analysed samples with a concentration range of 0.04 – 0.29, 0.07 – 0.33, 0.04 – 0.28 and 0.03 – 0.24 ng/g per dry weight in O. andersonii, C. ngamensis, T. rendalli and H. vittatus respectively. These concentrations were below the US-EPA 0.1 μg/g allowable limit in edible fish and the Australian Maximum Residue Limit (MRL) of 50 - 1000 ng/g in fresh fish. DDT was not detected in all the fish species investigated. The mean lipid content recorded in the fish samples were 1.24, 2.16, 2.18 and 4.21% for H. vittatus, T. rendalli, O. andersonni and C. ngamensis respectively. No systematic trend was observed between fish age and pesticide levels in fish. Acetylcholinesterase (AChE) activity assays were performed to assess the effects of organochlorine pesticides in Clarias ngamensis. The enzyme activity recorded in Clarias ngamensis from the Okavango Delta and the reference site was 12.31 μmol of acetylcholine iodide hydrolysed/min/g brain tissue. The enzyme activity remained the same indicating no enzyme inhibition. The conclusions drawn from this study are that the QuEChERS method is applicable for the determination of organochlorine pesticide residues in fish matrices. The fish from the Okavango Delta are safe for human consumption.
- Full Text:
- Authors: Mpofu, Christopher
- Date: 2011 , 2011-02-28
- Subjects: Pesticides , Organochlorine compounds , Freshwater fishes -- Effect of pesticides on -- Botswana -- Okavango River Delta , Water -- Pesticide content -- Botswana -- Okavango River Delta , Catfishes -- Botswana -- Okavango River Delta , Tigerfish -- Botswana -- Okavango River Delta , Redbreast tilapia -- Botswana -- Okavango River Delta
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:4404 , http://hdl.handle.net/10962/d1006707 , Pesticides , Organochlorine compounds , Freshwater fishes -- Effect of pesticides on -- Botswana -- Okavango River Delta , Water -- Pesticide content -- Botswana -- Okavango River Delta , Catfishes -- Botswana -- Okavango River Delta , Tigerfish -- Botswana -- Okavango River Delta , Redbreast tilapia -- Botswana -- Okavango River Delta
- Description: This thesis presents an evaluation of the dispersive solid-phase extraction (d-SPE) method referred to as the quick, easy, cheap, effective, rugged and safe (QuEChERS) method for the determination of four organochlorine pesticide residues in fish samples. The pesticides investigated in this study were o, p′-DDT, p, p′-DDE, aldrin and dieldrin. The combined use of Gas Chromatography with an Electron Capture Detector (GC-ECD) and sensitive Time of Flight (TOF) mass detector facilitated the identification of the target analytes. In the absence of certified reference material, the overall analytical procedure was validated by systematic recovery experiments on spiked samples at three levels of 2, 5 and 10 ng/g. The targeted compounds were successfully extracted and their recovery ranged from 76 to 96% with relative standard deviations of less than 13%. The optimum QuEChERS conditions were 2g of fish powder, 10 ml acetonitrile and 1 min shaking time. The optimal conditions were applied to assess the levels of chlorinated pesticides in blunt-tooth catfish (Clarias ngamensis), tigerfish (Hydrocynus vittatus), Oreochromis andersonii and red-breasted tilapia (Tilapia rendalli) from the Okavango Delta, Botswana. Dieldrin, p, p′-DDE and aldrin were detected in all the analysed samples with a concentration range of 0.04 – 0.29, 0.07 – 0.33, 0.04 – 0.28 and 0.03 – 0.24 ng/g per dry weight in O. andersonii, C. ngamensis, T. rendalli and H. vittatus respectively. These concentrations were below the US-EPA 0.1 μg/g allowable limit in edible fish and the Australian Maximum Residue Limit (MRL) of 50 - 1000 ng/g in fresh fish. DDT was not detected in all the fish species investigated. The mean lipid content recorded in the fish samples were 1.24, 2.16, 2.18 and 4.21% for H. vittatus, T. rendalli, O. andersonni and C. ngamensis respectively. No systematic trend was observed between fish age and pesticide levels in fish. Acetylcholinesterase (AChE) activity assays were performed to assess the effects of organochlorine pesticides in Clarias ngamensis. The enzyme activity recorded in Clarias ngamensis from the Okavango Delta and the reference site was 12.31 μmol of acetylcholine iodide hydrolysed/min/g brain tissue. The enzyme activity remained the same indicating no enzyme inhibition. The conclusions drawn from this study are that the QuEChERS method is applicable for the determination of organochlorine pesticide residues in fish matrices. The fish from the Okavango Delta are safe for human consumption.
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The effect of the pesticide, endosulfan, on hepatic cytochrome P-450, liver and gill ultrastructure, and selected haematological parameters of Oreochromis Mossambicus (Peters, 1852) (Pisces : Cichlidae)
- Authors: Quick, Arthur Joseph Rex
- Date: 1986
- Subjects: Pesticides , Mozambique tilapia , Cichlids
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:5195 , http://hdl.handle.net/10962/d1001971 , Pesticides , Mozambique tilapia , Cichlids
- Description: Two possible ways in which fish may acclimate to prolonged exposure· to sublethal levels of endosulfan were investigated: induction of the hepatic monooxygenase system and changes in haematology. These studies also involved an examination of the ultrastructure of liver and gill tissue. Endosulfan caused none of the characteristic phenobarbital-type inductive effects on the liver of Oreochromis mossambicus. There was no increase in cytochrome P-450 levels, microsomal protein or hepatosomatic index. The reasons for the lack of induction are discussed. The effect of endosulfan on the following haematological parameters was determined: haemoglobin, erythrocyte count, microhaematocrit, mean erythrocyte volume and mean erythrocyte haemoglobin concentration. The only effect was an increase in erythrocyte count. The value of changes in haematological parameters as indicators of pollutioninduced anemia in the field is discussed. No changes in gill ultrastructure were noted although electron micrographs of liver tissue showed lesions in hepatocytes. The diagnostic value of pollution-induced pathological changes on cell ultrastructure are discussed. Recommendations are made with regard to future large scale application of pesticides on or near large water bodies
- Full Text:
- Authors: Quick, Arthur Joseph Rex
- Date: 1986
- Subjects: Pesticides , Mozambique tilapia , Cichlids
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:5195 , http://hdl.handle.net/10962/d1001971 , Pesticides , Mozambique tilapia , Cichlids
- Description: Two possible ways in which fish may acclimate to prolonged exposure· to sublethal levels of endosulfan were investigated: induction of the hepatic monooxygenase system and changes in haematology. These studies also involved an examination of the ultrastructure of liver and gill tissue. Endosulfan caused none of the characteristic phenobarbital-type inductive effects on the liver of Oreochromis mossambicus. There was no increase in cytochrome P-450 levels, microsomal protein or hepatosomatic index. The reasons for the lack of induction are discussed. The effect of endosulfan on the following haematological parameters was determined: haemoglobin, erythrocyte count, microhaematocrit, mean erythrocyte volume and mean erythrocyte haemoglobin concentration. The only effect was an increase in erythrocyte count. The value of changes in haematological parameters as indicators of pollutioninduced anemia in the field is discussed. No changes in gill ultrastructure were noted although electron micrographs of liver tissue showed lesions in hepatocytes. The diagnostic value of pollution-induced pathological changes on cell ultrastructure are discussed. Recommendations are made with regard to future large scale application of pesticides on or near large water bodies
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The mode of action of the acyl-diethylamide molluscicides
- Authors: Solomon, Keith Ross
- Date: 1971
- Subjects: Pesticides , Molluscicides
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:5821 , http://hdl.handle.net/10962/d1007406
- Description: From Introduction: That bilharziasis an important public health, social and economic problem in the tropical and subtropical countries of the world is well appreciated. (WHO, 1965) Bilharsiasis is the disease caused by parasitic worms of the genus Schistosoma having certain fresh water snails as the intermediate host. In South Africa the more important snails are Bulinus africanus and B. globosus, the secondary hosts of Schistosom haematobium. (WHO, 1965) One method of controling the disease is to reduce the numbers of the intermediate host snails to such a low level that transmission cannot occur (WHO, 1965 and Macdonald, 1965) This has led to a strong interest in those substances that kill snails. The first recorded use of a molluscicide, copper sulphate, was during the first world War in Egypt. (De Villiers, 1965) More recently, the more or less random testing of large numbers of compounds led to the discovery of a large number of molluscicides. These were the heavy metal compounds such as the salts of mercury and arsenic, the substituted phenols such as pentachlorophenol (PCP) and the 2-substituted 4:6-dinitrophenols. (De Villiers, 1965) These compounds are good molluscicides but suffer from a number of disadvantages. The use of copper compounds in hard waters is impractical as the copper precipitates out as the less effective carbonate. The heavy metal salts are expensive and biocidal thus making the treated water unsuitable for human or agricultural use. The phenolic compounds are unpleasant and dangerous to handle and the hydrolysis of PCP is catalysed by sunlight in clear waters. High concentrations of these compounds are required, thus increasing transport and handling costs, particularly in inaccessible areas.
- Full Text:
- Authors: Solomon, Keith Ross
- Date: 1971
- Subjects: Pesticides , Molluscicides
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:5821 , http://hdl.handle.net/10962/d1007406
- Description: From Introduction: That bilharziasis an important public health, social and economic problem in the tropical and subtropical countries of the world is well appreciated. (WHO, 1965) Bilharsiasis is the disease caused by parasitic worms of the genus Schistosoma having certain fresh water snails as the intermediate host. In South Africa the more important snails are Bulinus africanus and B. globosus, the secondary hosts of Schistosom haematobium. (WHO, 1965) One method of controling the disease is to reduce the numbers of the intermediate host snails to such a low level that transmission cannot occur (WHO, 1965 and Macdonald, 1965) This has led to a strong interest in those substances that kill snails. The first recorded use of a molluscicide, copper sulphate, was during the first world War in Egypt. (De Villiers, 1965) More recently, the more or less random testing of large numbers of compounds led to the discovery of a large number of molluscicides. These were the heavy metal compounds such as the salts of mercury and arsenic, the substituted phenols such as pentachlorophenol (PCP) and the 2-substituted 4:6-dinitrophenols. (De Villiers, 1965) These compounds are good molluscicides but suffer from a number of disadvantages. The use of copper compounds in hard waters is impractical as the copper precipitates out as the less effective carbonate. The heavy metal salts are expensive and biocidal thus making the treated water unsuitable for human or agricultural use. The phenolic compounds are unpleasant and dangerous to handle and the hydrolysis of PCP is catalysed by sunlight in clear waters. High concentrations of these compounds are required, thus increasing transport and handling costs, particularly in inaccessible areas.
- Full Text:
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