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1.
Bull Environ Contam Toxicol ; 86(3): 331-5, 2011 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-21327612

RESUMO

Chlorfluazuron residues were determined in the peaches that were sprayed at dosage (a.i. 0.0167 kg 10a(-1)), using an analytical method that was validated as follows; r (2) = 0.9999, 0.02 mg kg(-1) (LOQ) and 87.8-93.6% (recovery). The residues from all samples were lower than the MRL (0.5 mg kg(-1), Korea). A maximum 0.27 mg kg(-1) of chlorfluazuron was detected in the samples applied at 6 days before harvest. The results signify that the 10% SC product would be used safely as an insecticide if it is applied two or three times onto peaches, with applications given until 6 days prior to harvest.


Assuntos
Inseticidas/análise , Resíduos de Praguicidas/análise , Compostos de Fenilureia/análise , Prunus/química , Piridinas/análise , Inseticidas/química , Resíduos de Praguicidas/química , Compostos de Fenilureia/química , Piridinas/química , Poluentes do Solo/análise , Poluentes do Solo/química
2.
Biomed Chromatogr ; 25(3): 405-11, 2011 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-20602509

RESUMO

In this study, a method for the detection of sarafloxacin in pig and chicken muscles was developed using HPLC-FLD as a regulatory residue technique. Good extraction efficiency was achieved using a mixture of 1% orthophosphoric acid-0.2 m MgCl(2) in water and acetonitrile as an extraction solvent, and n-hexane partitioning and centrifugation for cleanup was used in the absence of dehydration. Specificity, linearity, detection and quantification limits, recovery, accuracy and precision were all validated, and all results were sufficient for the SARA regulatory residue method in pig and chicken muscles. The method developed and described herein was not only simple but also reliable, and was applied to market samples to determine their residue contents.


Assuntos
Fracionamento Químico/métodos , Cromatografia Líquida de Alta Pressão/métodos , Ciprofloxacina/análogos & derivados , Resíduos de Drogas/análise , Carne/análise , Músculos/química , Acetonitrilas/química , Animais , Soluções Tampão , Galinhas , Ciprofloxacina/análise , Fluorometria/métodos , Análise de Alimentos/métodos , Hexanos/química , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Suínos
3.
Biomed Chromatogr ; 25(1-2): 155-63, 2011 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-21077268

RESUMO

In a continuation of our earlier work, a multiresidual analytical method using 48 frequently used neutral pesticides in a water matrix was developed and validated in this study. The samples were extracted with dichloromethane and the pesticides were analyzed via GC-NPD followed by confirmation with GC-MS. Good linearity was detected over a concentration range of 0.01-1.0 microg/mL with correlation coefficients (r(2) ) in excess of 0.982. The recoveries were measured between 70.7 and 111.4% for the majority of the targeted pesticides with relative standard deviations (RSDs) of less than 20%. The LODs and LOQs were in ranges of 0.1-2 and 0.33-6.6 microg/L, respectively. A total of 66 water samples were collected from different locations in Yeongsan and the Sumjin River, Republic of Korea, and were analyzed in accordance with the developed method. None of the water samples were determined to contain any of the targeted pesticides. The method has been shown to be simpler, faster, and more cost-effective than the method established by the Environmental Protection Agency (EPA).


Assuntos
Cromatografia Gasosa-Espectrometria de Massas/métodos , Resíduos de Praguicidas/análise , Praguicidas/análise , Rios/química , Poluentes Químicos da Água/análise , Cloreto de Metileno , Resíduos de Praguicidas/química , Praguicidas/química , Praguicidas/isolamento & purificação , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Poluentes Químicos da Água/química , Poluentes Químicos da Água/isolamento & purificação
4.
Biomed Chromatogr ; 25(9): 1003-9, 2011 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-21154886

RESUMO

In this study, a multiresidue analytical method for the detection of 37 pesticides in a soil matrix was developed and validated. The soil sample was fortified with a known quantity of pesticides at two different concentration levels (0.1 and 0.01 µg/g) and the analytes were extracted via a liquid-solid extraction method. The pesticides were separated on an HP5 capillary column and were analyzed with a gas chromatograph coupled to a nitrogen-phosphorous detector (GC-NPD). Method validation was accomplished with good linearity (r(2) = 0.994-0.999) within a considerable range of concentrations. Satisfactory recoveries (70.5-110.4%) were obtained with 32 pesticides at both spiking concentration levels, whereas five pesticides-dimepiperate, buprofezin, prometryn, pirimicarb, and fludioxonil-were recovered at relatively low levels (43.6-61.8%). The applicability of the method was demonstrated by analyzing field samples collected from 24 different sites around Yeongsan and Sumjin rivers in the Republic of Korea. No residues of the selected pesticides were detected in any of the samples. The developed method could be employed as a simple and cost-effective method for the routine detection and analysis of 37 pesticides in soil samples.


Assuntos
Cromatografia Gasosa/métodos , Resíduos de Praguicidas/análise , Poluentes do Solo/análise , Cromatografia Gasosa/instrumentação
5.
Biomed Chromatogr ; 24(8): 893-901, 2010 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-20039336

RESUMO

The principal objective of the present study was to develop a multiresidue analytical method for 62 pesticides in a soil matrix. Soil samples were fortified with known quantities of pesticides at two different concentration levels (0.1 and 0.01 microg/g) and the analytes were extracted via a liquid-solid extraction method. The pesticides were separated on an HP5 capillary column and were detected by gas chromatography coupled to an electron capture detector (GC-ECD). The method was validated, considering its good linearities (r(2) = 0.978-0.999), specificity and recovery characteristics. Recoveries were found between 70.3 and 113.4% for all pesticides except edifenphos (67.5%) and dichlobenil (69.5%) spiked at a 0.1 microg/mL concentration level and 74.5-117% except ethalfluralin (63.3%) and dichlobenil (51.9%) spiked at a concentration of 0.01 microg/mL. The developed method could be utilized as a simple and cost-effective method for the routine analysis of 62 pesticides in soil samples.


Assuntos
Cromatografia Gasosa/métodos , Resíduos de Praguicidas/análise , Praguicidas/análise , Poluentes do Solo/análise , Solo/análise
6.
J Sep Sci ; 32(4): 559-74, 2009 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-19212978

RESUMO

Several methods used for the multiresidue analysis of pesticides from the environment and drinking water have been reported. However, most of these reports dealt with a small number of targeted pesticides or some special groups. A method that is simple, faster, and more cost-effective than the environmental protection agency (EPA) method has been developed for the analysis of 82 frequently used pesticides in water samples obtained from Yeongsan and Sumjin rivers, as well as rice fields located in various locations around the two rivers. The samples were extracted by dichloromethane, and the pesticides were analyzed using a GC-electron capture detector (ECD), followed by confirmation with GC-MS. Recoveries were found to be between 82 and 120.1% for most of the tested pesticides, which were in agreement with the standard values dictated by the EPA. The method was potentially applied to 66 water samples for human consumption and 90 water samples from the rice fields and irrigation ditches that were collected from June to September 2007. Oxadiazon, butachlor, and alachlor were detected in some of the river water samples collected in June, iprobenfos (IBP) was detected in samples collected in August, and no pesticide was detected in September. On the other hand, chlorpyrifos-methyl, IBP, hexaconazole, diazinon, oxadiazon, butachlor, and isoprothiolane were detected at relatively high concentrations in 48 rice paddy field water samples collected between June and September 2007. Alachlor in one sample and procymidone in some of the rice paddy field water samples were also detected in trace amounts. The results were consistent with the temporal pattern of pesticide application in Korean rice fields.


Assuntos
Cromatografia Gasosa/métodos , Praguicidas/análise , Praguicidas/química , Água/análise , Água/química , Oryza , Estados Unidos , United States Environmental Protection Agency
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