Gas chromatographic determination of selected pesticides in human serum by head-space solid-phase microextraction

Abstract

SummaryA simple and rapid method, employing head-space solid-phase microextraction then gas chromatography-mass spectrometry, has been developed for the simultaneous determination of nine organochlorine pesticides (0~-HCH, hexachlorobenzene, hndane, endosulfan ether, 0~-endosulfan, p,p'-DDE, p,p'-DDD, endosulfan sulfate, and p,p'-DDT) and five organophosphorus pesticides (fonofos, parathion methyl, fenitrothion, chlorpyrifos, and ethion) in human serum. Sulfuric acid (9 M, 50 I~L), water (2 mL), and surrogate/internal standard solution (p,p'-DDE-D8, hexachlorobenzene53C6, and fenitrothion D6; 5014) were added to the serum sample (1 mL) and the resulting solution was sampled by head-space SPME at 90 ~ for 30 min. Quantitation was performed by means of calibration curves prepared by use of serum, using areas relative to those of the surrogates. Precision was found to be better than 20% at three concentration levels assayed in the ng mL 1 range. The detection limits were in the range 0.1 to 6 ng mL 1 forall compounds.Finally application of the optimized procedure enabled the detection of some pesticides in serum samples obtained from agricultural workers. Hexachlorobenzene, p,p'-DDE, and chlorpyrifos were found most frequently in the samples analyzed.

Rapid multiresidue determination of organochlorine and organophosphorus compounds in human serum by solid-phase extraction and gas chromatography coupled to tandem mass spectrometry

“…These findings are in concordance with other authors' data showing that higher chlorinated PCBs congeners are the most frequently detected in biological samples [24,25]. Additionally, data in the present paper are in agreement with our previous findings in human serum and whole blood [26,27] and in human adipose tissue analyses [28,29] for general population, as regards frequency of detections and major components detected in samples.…”

“…The results obtained revealed the presence of several OCs (HCB, p,p′-DDE, PCB 153, PCB 138 and PCB 180). This finding is in agreement with data presented by other authors, as these persistent compounds are usually detected in biological fluids and/or adipose tissues of general population [24,25,26,27,28,29,30].…”

“…Results obtained were satisfactory for most compounds with recoveries of 70-110% and coefficients of variation (CV) lower than 15%, with a few exceptions. Phosmet was poorly recovered while methidathion and malathion showed recoveries higher than 120%, which is in agreement with our previous work in the case of malathion [26]. Data for β-HCH were not completely satisfactory with high CVs; this was probably due to the column bleeding which mainly affected this compound.…”

Determination of organochlorine pesticides and polychlorinated biphenyls in human serum using headspace solid-phase microextraction and gas chromatography-electron capture detection

“…With respect to the target analytes of this study, an SPME technique has been reported for the determination of OCPs and PCBs in different environmental matrices including water and biological tissues [17][18][19][20]. However, only few works have been devoted to OCP determination in human serum using SPME or HS-SPME [21,22]. Nevertheless, in the revised literature there are no references about the potential of HS-SPME technique for simultaneous PCBs and OCPs determination in serum.…”

“…The study considering the variables one by one to get the best possible conditions for HS-SPME has been showed in several studies working with volatile compounds in biological fluids [23,24], PCBs in water [17] and OCPs in water [20] and in human serum [22]. However, this procedure requires a high number of runs and is also time consuming.…”