Este trabalho descreve um procedimento de cromatografia por injeção seqüencial para a determinação de picloram em águas explorando a baixa pressão de uma coluna monolítica C 18 de 2,5 cm de comprimento. A separação do analito da matriz foi obtida em menos de 60 s usando como fase móvel uma mistura de acetonitrila e H 3 PO 4 5,0 mmol L -1 na proporção 20:80 (v v -1 ) e vazão de 30 mL s -1. Detecção foi feita a 223 nm com uma cela de 40 mm de caminho óptico. O limite de detecção do método é adequado para monitorar o nível de concentração máximo permitido para picloram em água potável (500 mg L -1 ). A frequência de amostragem é de 60 análises por hora, consumindo 300 mL de acetonitrila por análise. A metodologia foi aplicada a águas de rio fortificadas, não sendo observadas diferenças estatisticamente significativas em comparação com a metodologia convencional de HPLC-UV. This paper describes a sequential injection chromatography procedure for determination of picloram in waters exploring the low backpressure of a 2.5 cm long monolithic C 18 column. Separation of the analyte from the matrix was achieved in less than 60 s using a mobile phase composed by 20:80 (v v ). The sampling frequency is 60 analyses per hour, consuming only 300 mL of acetonitrile per analysis. The proposed methodology was applied to spiked river water samples and no statistically significant differences were observed in comparison to a conventional HPLC-UV method.Keywords: sequential injection chromatography, monolithic column, picloram, waters
IntroductionThe presence of pesticides in surface and ground waters is a consequence of the extensive use of these chemicals in agriculture and their runoff down through the soil profile. Picloram (4-amino-3,5,6-trichloro-2-pyridinecarboxilic acid) is a herbicide widely used to control weeds in crops of sugar cane (pre-emergency), rice, pasture and wheat (pos-emergency).2 This herbicide can stay active in soil for long time, depending on the type of soil, soil moisture and temperature. It may exist at toxic levels to plants for more than one year after application at normal rates. 2,3 It is chemically adsorbed onto clay particles and natural organic matter occurring in soils. If the soil is poor in clay or organic matter contents, the herbicide may be easily leached to surface and ground waters.
3-6Determination of picloram is usually made by gas-liquid chromatography with electron capture detector or mass spectrometry detectors, 7 although several high performance liquid chromatography methods have already been proposed using either UV absorption or mass spectrometry detection modes. [8][9][10][11] These methods are very sensitive, but require the use of large sample volumes, besides to extensive extraction steps, derivatization reactions and expensive instrumentation, so that new sensitive methods that reduce the time of analysis and the use of organic solvents are needed. Electroanalytical methods are known to attend the demand for minimal sample treatment and low consumption of organic solvent...