Development of time-resolved chemiluminescence for the determination of antu in river water, wheat, barley, and oat grain samples.
A novel chemiluminescence method for the determination of antu has been developed based on the reaction between potassium permanganate in acid medium with this rat-poison in the presence of formaldehyde as an emission enhancer. The main feature of the system used is that the recording of the whole chemiluminescence intensity-vs-time profiles can be obtained, using the stopped-flow technique in a continuous-flow system. This enables the use of three quantitative parameters adjustable via software settings, one of them a typically kinetic parameter, such as rate of the light-decay reaction, and the others conventional parameters, such as maximum emission intensity and total emission area, which are proportional to the analyte concentration. The optimum chemical conditions for the chemiluminescence emission were investigated. The effect of common emission enhancers, such as formic acid, formaldehyde, glutaraldehyde, acetaldehyde, quinine, fluorescein, rhodamine B, and rhodamine 6G, was studied. The parameters selected were sulfuric acid 4.0 mol L(-)(1), permanganate 0.1 mmol L(-)(1), and formaldehyde 1.0 mol L(-)(1). The calibration graphs obtained with each one of the measurement parameters were linear for the concentration range from 0.05 to 3.00 microg mL(-)(1). The detection limits ranged from 0.005 to 0.010 microg mL(-)(1), and RSD values (n = 10) of 0.99-1.79% at a 0.30 microg mL(-)(1) concentration level and 1.71-2.22% at a 1.0 microg mL(-)(1) concentration level were obtained. The present chemiluminescence procedures were applied to the determination of antu in different kinds of samples, such as river water, wheat, barley, and oat grain samples. Recovery values not significantly different from the spiked amount were found for these determinations.
Murillo Pulgarín
José A
JA
Regional Institute for Applied Scientific Research, University of Castilla-La Mancha, 13071 Ciudad Real, Spain. joseantonio.murillo@uclm.es
García Bermejo
Luisa F
LF
Rubio Aranda
José A
JA
D018554:Avena / Q000737:chemistry; D002523:Edible Grain / Q000737:chemistry*; D001467:Hordeum / Q000737:chemistry; D008163:Luminescent Measurements / Q000379:methods*; D011196:Potassium Permanganate / Q000737:chemistry; D012378:Rodenticides / Q000032:analysis*; D012996:Solutions; D013890:Thiourea / Q000031:analogs & derivatives* / Q000032:analysis; D014908:Triticum / Q000737:chemistry; D014867:Water / Q000032:analysis*
D012378:Rodenticides; D012996:Solutions; D011196:Potassium Permanganate; D014867:Water; D013890:Thiourea; C005277:alpha-naphthyl thiourea