Determination for metabolites of organophosphorus pesticides in human urine by capillary gas chromatography-flame photometric detector
Wu-Chun-Hua; Zheng-Li-Xing; Zhou-Zhi-Jun
Fudan Xuebao 33(4): 552-555
Purpose To establish the procedure for the determination of dialkylphosphorus metabolites of organophosphorus pesticides in human urine by capillary gas chromatography (CGC) with flame photometric detector.Methods Dialkyphosphorus metabolites were extracted with acetonitrile. After purification and centrifugation, the organic phase was dried with anhydrous sodium sulphate. Derivatization reaction was performed by pentafluorobenzylbromide (PFBBr) at 50 degrees C for 16h for urinary metabolites simultaneously. Derivatives were identified by gas chromatography-mass spectrum with chemical ionization in total scan mode.Results Precise separation of the five dialkyphosphorus metabolites was achieved within 12 minutes. The recoveries of this method for fortified samples in different matrix were between 70.2% - 93.2%, and relative standard deviations below 10.0%.Conclusions The proposed method was accurate, reliable and sensitive. It has been applied to the analysis of urine samples from human exposed and non-exposed to organophosphates with satisfactory results.