Solid-phase microextraction for gas chromatographic/mass spectrometric analysis of dimethoate in human biological samples.
A new, simple and rapid procedure for the determination of dimethoate in urine and blood samples was developed using direct immersion solid-phase microextraction and gas chromatography/mass spectrometry. This technique required only 0.1 mL of sample, and ethion was used as internal standard. Two types of coated fibre were compared (100 microm polydimethylsiloxane, and 65 microm Carbowax/divinylbenzene). Other parameters, such as extraction temperature, adsorption and desorption time, salt addition, agitation and pH, were optimized to enhance the sensitivity of the method. Limits of detection (LODs) and quantitation (LOQs) were 50 and 100 ng/mL for urine and 200 and 500 ng/mL for blood, respectively. The method was found to be linear between the LOQ and 40 microg/mL for urine, and between the LOQ and 50 microg/mL for blood, with correlation coefficients ranging from 0.9923-0.9996. Precision (intra- and interday) and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The mean absolute recoveries of dimethoate were 1.24 and 0.50% for urine and blood, respectively. Because of its simplicity and the fact that small volumes of sample are used, the described method can be successfully used in the diagnosis of poisoning by this pesticide, namely in those situations where the sample volume is limited, as frequently occurs in forensic toxicology.
Gallardo
E
E
Instituto de Medicina Legal, Servicio de Toxicología Forense, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain.
Barroso
M
M
Margalho
C
C
Cruz
A
A
Vieira
D N
DN
López-Rivadulla
M
M
D004117:Dimethoate / Q000097:blood* / Q000652:urine*; D005554:Forensic Medicine / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D007306:Insecticides / Q000097:blood* / Q000652:urine*; D015203:Reproducibility of Results
D007306:Insecticides; D004117:Dimethoate