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Abstract:

An assay of phosmet residues in human blood by gas chromatography coupled to mass spectrometry (GC/MS) Clarus® 600/560 DMS PerkinElmer® was developed and validated in human blood samples loaded by residues of this insecticide. The extraction of phosmet has been carried out in solid phase through C18 SPE cartridges. The proposed method of phosmet residue analysis by GC/MS uses a capillary type Supelco®, the oven temperature was programmed from 75°C to 320°C. The Helium was used as carrier gas with a flow rate of 0.8 ml / min. The Phosalone was used as internal standard (IS). The retention time of the analyte and EI are 14.34 and 14.67 ± 0.02 min, respectively. The calibration curve is linear in the concentration range between 10 and 100ppb with R2 = 0.998. The method was validated according to ICH guidelines Q2 (R1) in terms of the criteria of accuracy, precision, linearity and specificity. The validated method is selective and has a quantification limit of 10 ppb. It can be used routinely for the determination of phosmet residues in real samples of human blood.

A new method for pesticide residues analysis in human blood by gas chromatography coupled with mass spectroscopy (GC / MS) was developed and validated on human plasma samples loaded by pesticide residues (demethoate, endosulfan, befinthrin, phosmet and deltamethrin). The extraction of these pesticides was conducted in solid phase through C18 SPE cartridges.The method of analysis of pesticide residues by GC / MS proposed, using a capillary column supelco® type oven temperature was programmed from 75 ° C to 320 ° C. Helium was used as carrier gas with a flow rate of 0.8ml / min. Phosalone (100 ppb) was used as internal standard (EI). Calibrations curves pesticides are linear in a concentration range between 10 and 100 ppb with R2˃ 0.994 for all the pesticides. The method was validated according to the guidelines of the NF V03-110, in May 2010 in terms of the criteria of accuracy, fidelity, linearity and specificity. The validated method is selective and has a quantification limit of 10 ppb. It can be used routinely for the determination of pesticide residues in samples of human blood.

Abstract:

Repeated exposure or consumption of food contaminated with pesticide residues can cause various disorders for the human body, especially the immune and hormonal disturbances and the onset of certain cancers. The multirésiduel assay method of pesticides in blood by (GC-MS) Clarus® 600/560 DMS PerkinElmer® we developed allowed us to conduct a screening of the majority of pesticide residues used in Moroccan agriculture. The calibration range contains a mixture of the most used pesticides. The extraction was performed in a solid medium by CSPE cartridges. This method uses a capillary column of 30 meters type Supelco®, the oven temperature was programmed from 90 ° C to 290 ° C with a gradient of 10 ° C / min. Helium was used as carrier gas with a flow rate of 0.8ml / min. Phosalone was used as internal standard (IS). The calibration curves of different pesticides are linear with concentrations ranging between 10 and 70 ppb with satisfactory correlation coefficients (R2> 0.99) and CV <20% for all results. In these analytical conditions we analyzed blood samples of Endocrinology of the University Hospital of Rabat. The results showed that some patients are contaminated with pesticide residue; dimethoate and bifenthrin. The hypothesis of the involvement of these pesticides in the development of hormonal disorders in patients is very likely. This method may be expanded and supplemented to prove this causal link.

Keywords: Pesticides, GC-MS, assay, Patients.