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1.
Ecotoxicol Environ Saf ; 208: 111603, 2021 Jan 15.
Article in English | MEDLINE | ID: mdl-33396123

ABSTRACT

Chlorothalonil (CLT) is a broad spectrum, and non-systemic fungicide applied in foliar structures to prevent and treat pathogens. This compound reaches to aquatic environments and affects the biota. In this context, the main goal of this study was to assess the effects of CLT at biochemical, tissular, and individual levels of biological organization using the invasive bivalve Corbicula largillierti as a bioindicator species. Clams were exposed to different sublethal concentrations (0, 10, 20 and 50 µg. L-1 CLT) for 96 h. At biochemical level, the enzymatic activity (Glutathione-s-Transferase, Catalase, Acetyl-, Butiryl- and Carboxyl-esterases) and lipid peroxidation were measured in gills and the visceral mass. Also, the digestive gland morphometry through quantitative histological indexes was registered at the tissular level. Finally, filtering activity and burial behavior at the individual level were measured. At the highest CLT concentration, the most significant changes were observed in enzymatic activity (except for butyrylcholinesterase), lipid peroxidation and in digestive gland morphometry. It was also registered increases of the filtering activity and the latency time to burial. Most of the biomarkers assessed showed significant responses under CLT exposure. Therefore, taking into account that C. largillierti was affected by CLT, it can be expected that other species could be in a potential risk if this fungicide is present in freshwater systems.


Subject(s)
Corbicula/drug effects , Environmental Monitoring/methods , Fresh Water/chemistry , Fungicides, Industrial/toxicity , Nitriles/toxicity , Water Pollutants, Chemical/toxicity , Animals , Biomarkers/metabolism , Catalase/metabolism , Corbicula/enzymology , Dose-Response Relationship, Drug , Fungicides, Industrial/analysis , Gills/drug effects , Gills/enzymology , Glutathione Transferase/metabolism , Lipid Peroxidation/drug effects , Nitriles/analysis , Water Pollutants, Chemical/analysis
2.
Food Chem ; 311: 126014, 2020 May 01.
Article in English | MEDLINE | ID: mdl-31864181

ABSTRACT

A method for the simultaneous determination of three commonly used coccidiostats in chicken liver was developed, comprising a multi-residue QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction step, and a liquid chromatography-ultra violet-fluorescence (HPLC-UV/FL) analysis. The QuEChERS extraction was optimized using an experimental design approach that includes a screening step to obtain the critical variables, an optimization step using multiple response surface analysis and the calculation of a desirability parameter. The optimized method was validated with fortified samples, reaching an average recovery of 91% and an overall precision of 5.5% (mean of three analytes at three levels). Limits of detection calculated on fortified samples were 20 µg kg-1 for lasalocid, 15 µg kg-1 for nicarbazin and 120 µg kg-1 for diclazuril. These values resulted at least one order of magnitude lower than the maximum allowed residue limit (MRL) of the studied coccidiostats for chicken liver.


Subject(s)
Chickens , Coccidiostats/analysis , Lasalocid/analysis , Nicarbazin/analysis , Nitriles/analysis , Triazines/analysis , Animals , Chromatography, High Pressure Liquid/methods , Coccidiostats/isolation & purification , Feasibility Studies , Food Safety , Lasalocid/isolation & purification , Liquid-Liquid Extraction , Liver/chemistry , Nicarbazin/isolation & purification , Nitriles/isolation & purification , Poultry , Research Design , Time Factors , Triazines/isolation & purification
3.
Food Res Int ; 125: 108626, 2019 11.
Article in English | MEDLINE | ID: mdl-31554076

ABSTRACT

The efficiencies of two conventional domestic procedures (immersion in pure water and detergent solution at 0.25 and 1%) and two treatments using ozone (immersion in water with bubbling O3 and immersion in ozonated water, both at 1 and 3 mg L-1) were evaluated for the removal of residues of the fungicides azoxystrobin, chlorothalonil and difenoconazole in tomatoes. The fungicides were sprayed on the fruits at the recommended concentration for the crop. The residues in the tomatoes and in the washing solutions were determined by extraction with low-temperature partition techniques and analysis by gas chromatography. More concentrated solutions were more effective in removing pesticide residues. The water bubbled with ozone at 3 mg L-1 was the most efficient treatment for the removal of fungicides, reaching a reduction of 70-90% of the residues. However, the treatments with the lowest concentration of ozone had lower loss of fruit mass during storage.


Subject(s)
Detergents , Food Handling/methods , Fruit/chemistry , Ozone , Pesticide Residues/analysis , Solanum lycopersicum , Dioxolanes/analysis , Food Contamination/prevention & control , Food Handling/instrumentation , Food Quality , Food Storage/methods , Fungicides, Industrial/analysis , Nitriles/analysis , Pyrimidines/analysis , Solutions , Strobilurins/analysis , Triazoles/analysis , Water
4.
Article in English | MEDLINE | ID: mdl-31443140

ABSTRACT

The dissipation of three field-applied pesticides (chlorothalonil, chlorpyrifos, and malathion), on cultivated prickly pear (Opuntia ficus-indica (L.) Mill.) pads was studied. The extraction of pesticides was carried out using the European quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction technique and detection was carried out using tandem liquid chromatography with mass spectrometry. At harvest, 15 days after application, pesticide dissipation was below the level of detectability. Dissipation curves for prickly pear pads fit to a first-order kinetic equation. Two initial concentration levels were used for each pesticide. The approximate dissipation time for all pesticides studied was similar (10 days) and the half-life time was around six days. Final concentrations for the three pesticides were below the reference maximum residue level (MRL) (0.01 mg/kg), which suggests that these products can be applied safely in the commercial production of prickly pear pads at the established concentrations.


Subject(s)
Chlorpyrifos/analysis , Environmental Monitoring/methods , Malathion/analysis , Nitriles/analysis , Opuntia/chemistry , Pesticide Residues/analysis , Chromatography, Liquid , Mass Spectrometry , Mexico
5.
Bull Environ Contam Toxicol ; 100(3): 384-388, 2018 Mar.
Article in English | MEDLINE | ID: mdl-29307113

ABSTRACT

Surface sediments from Reloncaví Fjord and the Chiloé inner sea in Chilean Patagonia were extracted and analyzed to estimate deltamethrin and diflubenzuron levels. These antiparasitary pesticides have been used for decades in the salmon industry. Relationships were determined between pesticide concentrations and organic carbon percent in sediments. Deltamethrin (0.39-1.05 µg g-1 dw) was found at all sampling sites but diflubenzuron (0.06-0.09 µg g-1 dw) at only five. Diflubenzuron levels were similar for sediments from other fjord areas. However, deltamethrin concentration was 2-3 fold higher than other studies on this area. The organic carbon percent was correlated positively and significantly with diflubenzuron, but not with deltamethrin. Our results suggest that the high deltamethrin concentrations in sediments are due to the increased use of pyrethroids around salmon farming areas. But, the diflubenzuron levels can be explained by degradation processes.


Subject(s)
Diflubenzuron/analysis , Environmental Monitoring/methods , Geologic Sediments/chemistry , Nitriles/analysis , Pesticides/analysis , Pyrethrins/analysis , Animals , Chile , Estuaries , Fisheries , Oceans and Seas , Salmon
6.
Biomedica ; 37(0): 180-186, 2017 Mar 29.
Article in English | MEDLINE | ID: mdl-29161489

ABSTRACT

INTRODUCTION: The use of long lasting insecticidal materials has shown promising results in the control of Aedes aegypti. OBJECTIVE: To evaluate the efficacy of long-lasting insecticidal nets (PermaNet®) for Aedes aegypti control after three washing treatments in the city of Girardot, Colombia. MATERIALS AND METHODS: Standard bioassays were conducted with the nets following the World Health Organization protocols using wild A. aegypti after three washing treatments: (1) Detergent powder, (2) detergent powder and bleach, and (3) bar soap, until completing 20 washes. RESULTS: The type and number of wash treatments had a significant effect on net efficacy. Greater effects in the insecticide bioavailability were seen for the bar soap treatment. After six washes, mortality decreased by 50% (25/50), vs 66% (33/50) for the detergent powder and 84% (42/50) for the detergent powder and bleach treatments. Regarding the number of washes, the bar soap treatment reduced the efficacy to 68% after only three washes. CONCLUSION: The effectiveness of long-lasting insecticidal nets (PermaNet 2.0) for A. aegypti control varied in relation to the treatment and number of washes. The bar soap treatment resulted in the greatest reduction of mortality. Further studies on insecticidal reductions are needed under local conditions.


Subject(s)
Aedes , Insecticide-Treated Bednets , Insecticides , Laundering , Mosquito Control/instrumentation , Mosquito Vectors , Nitriles , Pyrethrins , Animals , Bleaching Agents/pharmacology , Colombia , Detergents/pharmacology , Female , Insecticides/analysis , Insecticides/chemistry , Nitriles/analysis , Nitriles/chemistry , Powders , Pyrethrins/analysis , Pyrethrins/chemistry , Soaps/pharmacology , Solubility
7.
Biomédica (Bogotá) ; Biomédica (Bogotá);37(supl.2): 180-186, jul.-set. 2017. tab, graf
Article in Spanish | LILACS | ID: biblio-888536

ABSTRACT

Resumen Introducción. El uso de mosquiteros tratados con insecticida en fórmulas de larga duración ha demostrado resultados prometedores en el control de Aedes aegypti. Objetivo. Evaluar la eficacia de mosquiteros impregnados con deltametrina en una fórmula de larga duración para el control de A. aegypti en Girardot, Colombia, después de tres lavados. Materiales y métodos. Se hicieron bioensayos de eficacia de los mosquiteros contra A. aegypti silvestres después de utilizar los siguientes tres productos de lavado, siguiendo la metodología de la Organización Mundial de la Salud: detergente en polvo, detergente en polvo y blanqueador, y jabón de barra, todos utilizados hasta en 20 lavados. Resultados. El tipo de producto de lavado y el número de lavados afectaron significativamente la eficacia de los mosquiteros impregnados con deltametrina. El lavado con jabón de barra presentó el mayor efecto, pues en tan solo seis lavados la mortalidad bajó a 50 % (25/50), en contraste con 66 % (33/50 de mortalidad después del lavado con detergente en polvo y de 84 % (42/50) después del lavado con detergente y blanqueador. En cuanto al número de lavados, el jabón en barra también causó una mayor reducción de la eficacia: a 68 % con solo tres lavados. Conclusión. La eficacia de los mosquiteros impregnados con deltametrina de larga duración en el control de A. aegypti varió con el tipo de producto de lavado y el número de lavados, siendo el jabón en barra el que redujo su eficacia en mayor medida. Se requieren nuevos estudios para establecer la disminución en la concentración del insecticida entre lavados.


Abstract Introduction: The use of long lasting insecticidal materials has shown promising results in the control of Aedes aegypti. Objective: To evaluate the efficacy of long-lasting insecticidal nets (PermaNet®) for Aedes aegypti control after three washing treatments in the city of Girardot, Colombia. Materials and methods: Standard bioassays were conducted with the nets following the World Health Organization protocols using wild A. aegypti after three washing treatments: (1) Detergent powder, (2)detergent powder and bleach, and (3) bar soap, until completing 20 washes. Results: The type and number of wash treatments had a significant effect on net efficacy. Greater effects in the insecticide bioavailability were seen for the bar soap treatment. After six washes, mortality decreased by 50% (25/50), vs 66% (33/50) for the detergent powder and 84% (42/50) for the detergent powder and bleach treatments. Regarding the number of washes, the bar soap treatment reduced the efficacy to 68% after only three washes. Conclusion: The effectiveness of long-lasting insecticidal nets (PermaNet 2.0) for A. aegypti control varied in relation to the treatment and number of washes. The bar soap treatment resulted in the greatest reduction of mortality. Further studies on insecticidal reductions are needed under local conditions.


Subject(s)
Animals , Female , Pyrethrins , Mosquito Control/instrumentation , Aedes , Insecticide-Treated Bednets , Mosquito Vectors , Insecticides , Laundering , Nitriles , Powders , Pyrethrins/analysis , Pyrethrins/chemistry , Soaps/pharmacology , Solubility , Colombia , Detergents/pharmacology , Bleaching Agents/pharmacology , Insecticides/analysis , Insecticides/chemistry , Nitriles/analysis , Nitriles/chemistry
8.
Environ Monit Assess ; 189(6): 303, 2017 Jun.
Article in English | MEDLINE | ID: mdl-28567597

ABSTRACT

Agricultural pesticides are widely used in Suriname, an upper middle-income Caribbean country located in South America. Suriname imported 1.8 million kg of agricultural pesticides in 2015. So far, however, national monitoring of pesticides in crops is absent. Reports from the Netherlands on imported Surinamese produce from 2010 to 2015 consistently showed that samples exceeded plant-specific pesticide maximum residue limits (MRLs) of the European Union (EU). Consumption of produce containing unsafe levels of pesticide residues can cause neurological disorders, and particularly, pregnant women and children may be vulnerable. This pilot study assessed the presence of pesticide residues in commonly consumed produce items cultivated in Suriname. Thirty-two insecticides (organophosphates, organochlorines, carbamates, and pyrethroids) and 12 fungicides were evaluated for their levels in nine types of produce. Pesticide residue levels exceeding MRLs in this study regarded cypermethrin (0.32 µg/g) in tomatoes (USA MRL 0.20 µg/g), lambda-cyhalothrin (1.08 µg/g) in Chinese cabbage (USA MRL 0.40 µg/g), endosulfan (0.07 µg/g) in tannia (EU MRL 0.05 µg/g), and lindane (0.02 and 0.03 µg/g, respectively) in tannia (EU MRL 0.01 µg/g). While only a few pesticide residues were detected in this small pilot study, these residues included two widely banned pesticides (endosulfan and lindane). There is a need to address environmental policy gaps. A more comprehensive sampling and analysis of produce from Suriname is warranted to better understand the scope of the problem. Preliminary assessments, using intake rate, hazard quotient, and level of concern showed that it is unlikely that daily consumption of tannia leads to adverse health effects.


Subject(s)
Environmental Monitoring , Pesticide Residues/analysis , Vegetables/chemistry , Agriculture , Carbamates/analysis , Crops, Agricultural/chemistry , Endosulfan/analysis , Food Contamination/analysis , Food Contamination/statistics & numerical data , Fungicides, Industrial/analysis , Hexachlorocyclohexane/analysis , Humans , Hydrocarbons, Chlorinated/analysis , Insecticides/analysis , Nitriles/analysis , Pesticides/analysis , Pilot Projects , Pyrethrins/analysis , Suriname
9.
Environ Toxicol Chem ; 36(11): 2895-2898, 2017 11.
Article in English | MEDLINE | ID: mdl-28640485

ABSTRACT

Residential indoor environments are potential sources of exposure to pyrethroids, which have low acute toxicity to humans but are allergenic and suspected endocrine disruptors. The present study evaluated the persistence of the pyrethroids cypermethrin and beta-cyfluthrin on indoor surfaces and in house dust. Cypermethrin and beta-cyfluthrin were applied and maintained on aluminum foils and in dust samples for 112 d under controlled conditions and for 12 mo in a test house; periodically, they were quantified by high-performance liquid chromatography. Cypermethrin and beta-cyfluthrin concentrations showed decreases of 10.1% and 7.7% on aluminum foils, and 12.7% and 16.4% in dust, respectively, at 112 d under controlled conditions. In the test house, cypermethrin and beta-cyfluthrin concentrations decreased by 40.3% and 60.2% on aluminum foils, and 29.6% and 56.2% in dust at the end of the study. The results show the considerable persistence of cypermethrin and beta-cyfluthrin indoors and indicate the risk of exposure to these products. Environ Toxicol Chem 2017;36:2895-2898. © 2017 SETAC.


Subject(s)
Air Pollution, Indoor/analysis , Insecticides/analysis , Pyrethrins/analysis , Aluminum/chemistry , Chromatography, High Pressure Liquid , Dust/analysis , Endocrine Disruptors/analysis , Humans , Nitriles/analysis , Time Factors
10.
Chemosphere ; 177: 77-83, 2017 Jun.
Article in English | MEDLINE | ID: mdl-28284118

ABSTRACT

Over the last decade, Uruguay has expanded and intensified its rainfed crop production. This process has affected beekeeping in several ways: for example, by reducing the space available. This has increased the density of apiaries, the risk of varroosis and acaricide use. Additionally, the dominance of no-tillage crops has increased the frequencies of application and of loads of pesticides in regions where such crops share the land with beekeeping and honey production. Therefore, the exposure of bees to xenobiotics (agricultural pesticides and veterinary products) has increased in line with pollution of hives and their products. To document pollution from hive exposure to pesticides, we surveyed the presence of 30 xenobiotics normally used in Uruguay, in recycled beeswax (RB) and in honey cappings (HC) from the main Uruguayan beekeeping regions. There was contamination of all the analyzed samples (RB and HC) with the herbicide atrazine at a range of 1-2 ng g-1. At least three or four additional xenobiotics were detected: insecticides (chlorpyrifos-ethyl and thiacloprid); fungicides (azoxystrobin and tebuconazole); and veterinary products (coumaphos, ethion, and tau-fluvalinate). The frequency of detection of chlorpyrifos-ethyl and coumaphos in RB samples was higher than in those of HC. Moreover, the concentrations of azoxystrobin, coumaphos, and tebuconazole in RB samples were higher than in HC samples. Therefore, we suggest the use of HC to produce recycled printed beeswax films for use in hives to minimize pollution transfer.


Subject(s)
Agriculture , Pesticides/analysis , Waxes/chemistry , Xenobiotics/analysis , Acaricides/analysis , Animals , Beekeeping , Bees , Fungicides, Industrial/analysis , Gas Chromatography-Mass Spectrometry , Geography , Herbicides/analysis , Honey/analysis , Insecticides/analysis , Nitriles/analysis , Pyrethrins/analysis , Risk Assessment , Uruguay
11.
Sci Total Environ ; 586: 1254-1262, 2017 May 15.
Article in English | MEDLINE | ID: mdl-28237465

ABSTRACT

The objective of this study was to measure the impact of the mechanized chlorpyrifos, copper oxychloride and myclobutanil application in a small peach orchard, on humans (operators, bystanders and residents) and on the productive soil. The mean Potential Dermal Exposure (PDE) of the workers (tractor drivers) was 30.8mL·h-1±16.4mL·h-1, with no specific pesticide distribution on the laborers body. Although the Margin of Safety (MOS) factor for the application stage were above 1 (safe condition) for myclobutanil and cooper oxycloride it was below 1 for chlorpyrifos. The mix and load stage remained as the riskier operation. Pesticide found on the orchard soil ranged from 5.5% to 14.8% of the total chlorpyrifos, copper oxychloride and myclobutanil applied. Pesticide drift was experimentally measured, finding values in the range of 2.4% to 11.2% of the total pesticide applied. Using experimental drift values, bystander (for one application), resident (for 20 applications) and earthworm (for one application) risk indicators (RIs) were calculated for the chlorpyrifos plus copper oxychloride and for myclobutanil treatments for different distances to the orchard border. Earthworm RI was correlated with experimental Eisenia andrei ecotoxicological assays (enzymatic activities: cholinesterases, carboxylesterases and glutathione S-transferases; behavioral: avoidance and bait-lamina tests) with good correlation.


Subject(s)
Agriculture , Chlorpyrifos/analysis , Copper/analysis , Nitriles/analysis , Occupational Exposure/analysis , Pesticides/analysis , Triazoles/analysis , Animals , Argentina , Environmental Monitoring , Humans , Oligochaeta , Prunus persica , Soil , Soil Pollutants/analysis
12.
J Environ Sci Health B ; 52(4): 274-281, 2017 Apr 03.
Article in English | MEDLINE | ID: mdl-28085564

ABSTRACT

The most efficient system of horizontal subsurface flow constructed wetlands (HSSFCW) for removing dissolved organic carbon (DOC) in the presence of chlorothalonil pesticide (CLT) present in synthetic domestic wastewater was determined using the macrophyte Phragmites australis. Two concentrations of CLT (85 and 385 µg L-1) and one concentration of glucose (20 mg L-1) were evaluated in four pilot scale horizontal surface flow constructed wetlands coupled with two sizes of silica gravel, igneous gravel, fine chalky gravel (3.18-6.35 mm), coarse gravel (12.70-25.40 mm) and two water surface heights (20 and 40 cm). For a month, wetlands were acclimated with domestic wastewater. Some groups of bacteria were also identified in the biofilm attached to the gravel. In each treatment periodic samplings were conducted in the influent and effluent. Chlorothalonil was quantified by gas chromatography (GC-ECD m), DOC by an organic carbon analyzer and bacterial groups using conventional microbiology in accordance with Standard Methods. The largest removals of DOC (85.82%-85.31%) were found when using fine gravel (3.18-6.35 mm) and the lower layer of water (20 cm). The bacterial groups quantified in the biofilm were total heterotrophic, revivable heterotrophic, Pseudomonas and total coliforms. The results of this study indicate that fine grain gravel (3.18-6.35 mm) and both water levels (20 to 40 cm) can be used in the removal of organic matter and for the treatment of agricultural effluents contaminated with organo-chloride pesticides like CLT in HSSFCW.


Subject(s)
Carbon , Nitriles , Waste Disposal, Fluid/methods , Wetlands , Ammonia/metabolism , Biofilms , Carbon/chemistry , Chromatography, Gas , Microbial Consortia , Nitriles/analysis , Phosphates/metabolism , Poaceae , Wastewater/chemistry , Water Purification/methods
13.
Food Chem ; 181: 64-71, 2015 Aug 15.
Article in English | MEDLINE | ID: mdl-25794722

ABSTRACT

This work describes the optimization and validation of a method employing solid-liquid extraction with low temperature partitioning (SLE/LTP) together with analysis by gas chromatography with electron capture detection (GC/ECD) for the determination of nine pesticides (chlorothalonil, methyl parathion, procymidone, endosulfan, iprodione, λ-cyhalothrin, permethrin, cypermethrin, and deltamethrin) in lettuce. The method was found to be selective, accurate, and precise, with means recovery values in the range of 72.3-103.2%, coefficients of variation ⩽ 12%, and detection limits in the range 0.4-37 µg kg(-1). The matrix components significantly influence the chromatographic response of the analytes (above 10%). The optimized and validated method was applied to determine the residual concentrations of the fungicides iprodione and procymidone that had been applied to field crops of lettuce. The maximum residual concentrations of the pesticides in the lettuce samples were 13.6 ± 0.4 mg kg(-1) (iprodione) and 1.00 ± 0.01 mg kg(-1) (procymidone), on the day after application of the products.


Subject(s)
Chromatography, Gas/methods , Lactuca/chemistry , Pesticide Residues/isolation & purification , Solid Phase Extraction/methods , Food Contamination/analysis , Methyl Parathion/analysis , Methyl Parathion/isolation & purification , Nitriles/analysis , Nitriles/isolation & purification , Pesticide Residues/analysis , Pyrethrins/analysis , Pyrethrins/isolation & purification , Temperature
14.
Forensic Sci Int ; 243: 95-8, 2014 Oct.
Article in English | MEDLINE | ID: mdl-24887446

ABSTRACT

Cocaine represents a serious problem to society. Smoked cocaine is very addictive and it is frequently associated with violence and health issues. Knowledge of the purity and adulterants present in seized cocaine, as well as variations in drug characteristics are useful to identify drug source and estimate health impact. No data are available regarding smoked cocaine composition in most countries, and the smoked form is increasing in the Brazilian market. The purpose of the present study is to contribute to the current knowledge on the status of crack cocaine seized samples on the illicit market by the police of São Paulo. Thus, 404 samples obtained from street seizures conducted by the police were examined. The specimens were macroscopically characterized by color, form, odor, purity, and adulterant type, as well as smoke composition. Samples were screened for cocaine using modified Scott test and thin-layer chromatographic (TLC) technique. Analyses of purity and adulterants were performed with gas chromatography equipped with flame ionization detector (GC-FID). Additionally, smoke composition was analyzed by GC-mass spectrometry (MS), after samples burning. Samples showed different colors and forms, the majority of which is yellow (74.0%) or white (20.0%). Samples free of adulterants represented 76.3% of the total. Mean purity of the analyzed drug was 71.3%. Crack cocaine presented no correlations between macroscopic characteristics and purity. Smoke analysis showed compounds found also in the degradation of diesel and gasoline. Therefore, the drug marketed as crack cocaine in São Paulo has similar characteristics to coca paste. High purity can represent a greater risk of dependency and smoke compounds are possibly worsening drug health impact.


Subject(s)
Crack Cocaine/chemistry , Drug Contamination , Aminobenzoates/analysis , Benzene/analysis , Biphenyl Compounds/analysis , Brazil , Caffeine/analysis , Chromatography, Gas , Chromatography, Liquid/methods , Cyclooctanes/analysis , Lidocaine/analysis , Mass Spectrometry , Naphthalenes/analysis , Nitriles/analysis , Pyridines/analysis , Smoke/analysis
15.
Acta Odontol Scand ; 72(8): 630-8, 2014 Nov.
Article in English | MEDLINE | ID: mdl-24850506

ABSTRACT

OBJECTIVE: This study determined the chemical components derived from degradation of 2% chlorhexidine (CHX) gel and solution by using gas chromatography-mass spectrometry. MATERIALS AND METHODS: Three 2% CHX gels were used to identify the products of CHX gel degradation using gas chromatography-mass spectrometry. A solution of CHX was also evaluated to compare the degradation between gel and solution. Degradation was evaluated in four storage situations (on the worktable with light: on the worktable without light; in the Pasteur oven at 36.5°C without light; and in the refrigerator at 8°C without light). Measurements were made at four time points: initial analysis and 1, 3 and 6 months after. The conversion of CHX into para-chloroaniline in storage situations and in different periods was analyzed statistically using chi-square test (α = 5%). RESULTS: The 2% CHX gel or solution had already degraded vial found within the period of validity, at all time points and for all storage conditions. The amount of para-chloroaniline (pCA) was directly proportional to time in the case of CHX solution, but not in CHX gel due to lack of homogeneity. CHX homogeneity in hydroxyethylcellulose gel was directly dependent on compounding mode. CONCLUSIONS: Degradation products, such as para-chloroaniline (pCA), orto- chloroaniline (oCA), meta-chloroaniline (mCA), reactive oxygen species (ROS) and organochlorines (ortho-chlorophenyl isocyanate and 2-amino-5-clorobenzonitrila) were found in 2% CHX gel and solution, regardless of storage conditions or time. In relationship to gel homogenization an alternative to produce 2% CHX gel and a new homogenization method have been developed.


Subject(s)
Anti-Infective Agents, Local/analysis , Chlorhexidine/analogs & derivatives , Root Canal Irrigants/analysis , Aniline Compounds/analysis , Cellulose/analogs & derivatives , Cellulose/analysis , Chlorhexidine/analysis , Chromatography/methods , Cold Temperature , Darkness , Drug Compounding , Drug Storage , Gas Chromatography-Mass Spectrometry/methods , Gels , Hot Temperature , Humans , Isocyanates/analysis , Light , Materials Testing , Nitriles/analysis , Reactive Oxygen Species/analysis , Solutions , Spectrophotometry, Ultraviolet/methods , Time Factors
16.
Biomed Chromatogr ; 28(12): 1722-7, 2014 Dec.
Article in English | MEDLINE | ID: mdl-24771661

ABSTRACT

A novel LC-MS/MS method was developed for the quantification of vildagliptin in an aqueous matrix. The method was successfully validated, meeting all the requisites of US Food and Drug Administration guide for a bioanalytical method. The developed method presented a limit of quantification of 10 ng/mL and the range of concentration achieved was 10-1875 ng/mL. The injection volume necessary was only 10 µL, and retention time was 4.60 min. The mobile phase employed was methanol-ammonium acetate 5 mm (95:5). The stability of the drug was evaluated in the different conditions through which the samples passed. A pharmacokinetic experiment was conducted with diabetic male Wistar rats, and the concentration of drug in liver was evaluated through a microdialysis technique. The perfusion fluid employed was ultrapure water. The dose administrated was 50 mg/kg and the method allowed the quantification of vildagliptin for more than three half lives, successfully characterizing the pharmacokinetic profile when the developed method was applied. This is the first report on the tissue pharmacokinetics of a DPP-4 inhibitor and could contribute to drug dosage optimization in the future.


Subject(s)
Adamantane/analogs & derivatives , Chromatography, High Pressure Liquid/methods , Diabetes Mellitus, Experimental/metabolism , Microdialysis/methods , Nitriles/analysis , Pyrrolidines/analysis , Adamantane/analysis , Adamantane/chemistry , Adamantane/pharmacokinetics , Animals , Dipeptidyl-Peptidase IV Inhibitors/analysis , Dipeptidyl-Peptidase IV Inhibitors/chemistry , Dipeptidyl-Peptidase IV Inhibitors/pharmacokinetics , Drug Stability , Liver/chemistry , Male , Muscles/chemistry , Nitriles/chemistry , Nitriles/pharmacokinetics , Pyrrolidines/chemistry , Pyrrolidines/pharmacokinetics , Rats , Rats, Wistar , Reproducibility of Results , Sensitivity and Specificity , Tandem Mass Spectrometry/methods , Tissue Distribution , Vildagliptin
17.
Environ Sci Process Impacts ; 16(4): 858-65, 2014 Apr.
Article in English | MEDLINE | ID: mdl-24458090

ABSTRACT

Some organic contaminants dissolved in natural waters tend to adsorb on suspended particles and sediments. In order to mimic the photodegradation routes in natural waters of bromoxynil (BXN) adsorbed on silica, we here prepare and characterize silica nanoparticles modified with BXN (NP-BXN). We measure the direct photolysis quantum yield of aqueous BXN at 307 nm (0.064 ± 0.001) and detect the formation of bromide ions as a reaction product. Under similar conditions the photolysis quantum yield of BXN bonded to NP-BXN is much lower (0.0021 ± 0.0004) and does not lead to formation of bromide ions. The rate constant of the reaction of NP-BXN with the excited triplet states of riboflavin, a molecule employed as a proxy of chromophore dissolved organic matter (DOM) was measured in laser flash-photolysis experiments. The rate constants for the overall (kt) and chemical interaction (kr) of singlet oxygen with NP-BXN were also measured. Kinetic computer simulations show that the relevance of the direct and indirect (through reactions with reactive species generated in photoinduced processes) photodegradation routes of BXN is very much affected by sorption on silica. Immobilization of the herbicide on the particles, on one hand, affects the photolysis mechanism and lowers its photolysis quantum yield. On the other hand, the results obtained in aqueous suspensions indicate that immobilization also lowers the rate of collisional encounter, which affects the quenching rate constants of excited triplet states and singlet oxygen with the herbicide.


Subject(s)
Herbicides/chemistry , Nanoparticles/chemistry , Nitriles/chemistry , Photolysis , Silicon Dioxide/chemistry , Adsorption , Herbicides/analysis , Kinetics , Models, Chemical , Nitriles/analysis , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/chemistry
18.
Bull Environ Contam Toxicol ; 91(2): 160-4, 2013 Aug.
Article in English | MEDLINE | ID: mdl-23722654

ABSTRACT

A method was developed using matrix solid-phase dispersion, together with liquid chromatography with ultraviolet diode array detector for determination of carbofuran, difenoconazole, ß-cyfluthrin, spirodiclofen and thiophanate-methyl in stem of coconut palm. The best results were obtained using 2.0 g of stem, 1.6 g of Florisil as sorbent and cyclohexane:acetone mixture (4:1). The method was validated using stem samples spiked with pesticides at four concentration levels (0.05-2.0 µg/g). Average recoveries ranged from 70 % to 114.3 %, with relative standard deviations between 1.2 % and 19.2 %. Detection and quantification limits were in the ranges 0.02-0.03 and 0.05-0.1 µg/g, respectively.


Subject(s)
Chromatography, High Pressure Liquid/methods , Cocos/chemistry , Pesticide Residues/analysis , Plant Stems/chemistry , Solid Phase Extraction/methods , 4-Butyrolactone/analogs & derivatives , 4-Butyrolactone/analysis , Acetone/chemistry , Carbofuran/analysis , Cyclohexanes/chemistry , Dioxolanes/analysis , Magnesium Silicates/chemistry , Nitriles/analysis , Pyrethrins/analysis , Reproducibility of Results , Spiro Compounds/analysis , Thiophanate/analysis , Triazoles/analysis
19.
Food Chem Toxicol ; 59: 230-5, 2013 Sep.
Article in English | MEDLINE | ID: mdl-23778051

ABSTRACT

Cassava (Manihot esculenta Crantz) is a plant widely used for food consumption in different processed products in rural areas of Africa, Asia, and Latin America. Cassava is a good source of carbohydrates and micronutrients. However, if it is not adequately processed or the consumer has nutritional deficiencies, then its cyanogenic glycoside (i.e., linamarin and lotaustralin) content makes it potentially neurotoxic. In the present study, the neurotoxic effects of different concentrations of linamarin (0.075, 0.15, 0.22, and 0.30 mg/kg) contained in cassava juice were evaluated in the open field and swim tests to identify locomotor alterations in adult male Wistar rats. The linamarin concentration in cassava juice was determined by high-performance liquid chromatography, and the juice was administered intraesophageally for 28 days. The results suggested that the consumption of linamarin in cassava juice increased the number of crossings and rearings in the open field test and caused behavioral deficiency, reflected by lateral swimming, in the swim test on days 21 and 28 of treatment. These alterations are possibly related to neuronal damage caused by linamarin in cassava juice in structures of the central nervous system involved in motor processing.


Subject(s)
Beverages/adverse effects , Manihot/adverse effects , Motor Neuron Disease/etiology , Neurotoxins/toxicity , Nitriles/toxicity , Plant Tubers/adverse effects , Animals , Behavior, Animal/drug effects , Beverages/analysis , Central Nervous System/drug effects , Exploratory Behavior/drug effects , Male , Manihot/chemistry , Mexico , Motor Activity/drug effects , Motor Neuron Disease/chemically induced , Motor Neurons/drug effects , Neurotoxins/administration & dosage , Neurotoxins/analysis , Nitriles/administration & dosage , Nitriles/analysis , Osmolar Concentration , Plant Tubers/chemistry , Rats , Rats, Wistar , Swimming , Time Factors
20.
Environ Int ; 47: 17-22, 2012 Oct 15.
Article in English | MEDLINE | ID: mdl-22717642

ABSTRACT

There is an assumption that pyrethroid pesticides are converted to non-toxic metabolites by hydrolysis in mammals. However, some recent works have shown their bioaccumulation in human breast milk collected in areas where pyrethroids have been widely used for agriculture or malaria control. In this work, thirteen pyrethroids have been studied in human breast milk samples coming from areas without pyrethroid use for malaria control, such as Brazil, Colombia and Spain. The concentrations of pyrethroids ranged from 1.45 to 24.2 ng g⁻¹ lw. Cypermethrin, λ-cyhalothrin, permethrin and esfenvalerate/fenvalerate were present in all the studied samples. The composition of pyrethroid mixture depended on the country of origin of the samples, bifenthrin being the most abundant in Brazilian samples, λ-cyhalothrin in Colombian and permethrin in Spanish ones. When the pyrethroid concentrations were confronted against the number of gestations, an exponential decay was observed. Moreover, a time trend study was carried out in Brazil, where additional archived pool samples were analyzed, corresponding to years when pyrethroids were applied for dengue epidemic control. In these cases, total pyrethroid levels reached up to 128 ng g⁻¹ lw, and concentrations decreased when massive use was not allowed. Finally, daily intake estimation of nursing infants was calculated in each country and compared to acceptable WHO levels. The estimated daily intakes for nursing infants were always below the acceptable daily intake levels, nevertheless in certain samples the detected concentrations were very close to the maximum acceptable levels.


Subject(s)
Breast Feeding/statistics & numerical data , Environmental Exposure/statistics & numerical data , Environmental Pollutants/metabolism , Insecticides/metabolism , Milk, Human/metabolism , Pyrethrins/metabolism , Adolescent , Adult , Agriculture/methods , Agriculture/statistics & numerical data , Brazil , Colombia , Environmental Pollutants/analysis , Environmental Pollution/statistics & numerical data , Female , Humans , Infant , Insecticides/analysis , Milk, Human/chemistry , Mosquito Control/methods , Mosquito Control/statistics & numerical data , Nitriles/analysis , Nitriles/metabolism , Permethrin/analysis , Permethrin/metabolism , Pyrethrins/analysis , Spain , Young Adult
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