Optimization and validation of liquid-liquid extraction with low temperature partitioning for determination of carbamates in water.
Using a 2(3) experimental design, liquid-liquid extraction with low temperature partitioning (LLE-LTP) was optimized and validated for analysis of three carbamates (aldicarb, carbofuran and carbaryl) in water samples. In this method, 2.0 mL of sample is placed in contact with 4.0 mL of acetonitrile. After agitation, the sample is placed in a freezer for 3 h for phase separation. The organic extract is analyzed by high performance liquid chromatography with ultraviolet detection (HPLC-UV). For validation of the technique, the following figures of merit were evaluated: accuracy, precision, detection and quantification limits, linearity, sensibility and selectivity. Extraction recovery percentages of the carbamates aldicarb, carbofuran and carbaryl were 90%, 95% and 96%, respectively. Even though extremely low volumes of sample and solvent were used, the extraction method was selective and the detection and quantification limits were between 5.0 and 10.0 microg L(-1), and 17.0 and 33.0 microg L(-1), respectively.
Goulart
Simone Machado
SM
Departamento de Química, Universidade Federal de Viçosa, Vila Gianetti, Casa 24, 36 570-000 Viçosa, MG, Brazil.
Alves
Renata Domingos
RD
Neves
Antônio Augusto
AA
de Queiroz
José Humberto
JH
de Assis
Tamires Condé
TC
de Queiroz
Maria Eliana L R
ME
D000448:Aldicarb / Q000032:analysis; D002219:Carbamates / Q000032:analysis; D012721:Carbaryl / Q000032:analysis; D002235:Carbofuran / Q000032:analysis; D005591:Chemical Fractionation / Q000379:methods; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D057230:Limit of Detection; D010573:Pesticide Residues / Q000032:analysis; D014874:Water Pollutants, Chemical / Q000032:analysis
D002219:Carbamates; D010573:Pesticide Residues; D014874:Water Pollutants, Chemical; D000448:Aldicarb; D012721:Carbaryl; D002235:Carbofuran