Negative Ion Chemical Ionization-Gas Chromatographic-Mass Spectrometric Determination of Residues of Different Pyrethroid Insecticides in Whole Blood and Serum

Abstract

A new rapid and sensitive analytical method using negative ion chemical ionization-gas chromatography-mass spectrometry in selective ion monitoring mode has been developed for the determination of residues of different synthetic pyrethroid insecticides, allethrin, bifenthrin, cypermethrin, cyphonothrin, cyfluthrin, lambda-cyhalothrin, deltamethrin, fenvalerate, fenpropathrin, permethrin, prallethrin, and trans-fluthrin, in whole blood. The residues of pyrethroid molecules were extracted from the whole blood using a hexane and acetone (8:2, v/v) solvent mixture without separating the serum. The method was found sensitive to detect the residues of pyrethroids up to the level 0.2 pg/mL. Experiments conducted with the whole blood samples at the fortification level 1-100 pg/mL showed 91-103% recovery, whereas blood serum samples collected after the fortification of pyrethroids in whole blood showed 36-54% recovery. Recovery experiments conducted by direct fortification of pyrethroids in blood serum samples showed 96-108%. The applications of the analytical method was tested by analyzing 73 human blood samples collected from the population exposed continuously to different pyrethroid-based formulations. None of the blood samples showed residues of pyrethroids. The results were also confirmed by the detection of the appropriate amounts in a number of these samples, which had subsequently been spiked with known quantity of pyrethroids.

Facile and Sensitive Spectrophotometric Determination of Synthetic Pyrithroids in Their Formulations, Water and Grain Samples

“…The insecticides are highly stable under acidic conditions, though unstable at pH 8.0. Because of its significance, several methods have been developed for the determination of synthetic pyrethroids such as spectrophotometry Naidu, 1992, 1994), gas chromatography (Serodio and Noguira, 2005;Leng and Gries, 2005;Ramesh and Ravi, 2004;Sassine et al, 2004;Sannino et al, 2003) and high performance liquid chromatography (Leon Gonzalez et al, 2005;Parrilla Vazquez et al, 2005;Ding et al, 2004;Bicker et al, 2004;Loper and Anderson, 2003).…”

Bioanalytical Methods for The Quantification of Cis -Permethrin and Trans -Permethrin in Biological Samples

“…Several analytical strategies for the separation and determination of PERM in biological matrices have been reported [6][7][8][9][10][11][12]. However, using GC-NCI-MS has provided the most sensitive method for the bioanalysis of PERM…”

“…Bioanalysis (2017) 9(19) future science group Editorial Hooshfar & Bartlett or its two isomers [7,9]. Additionally, the high number of theoretical plates available when using capillary stationary phases in GC allowed for an easy separation of the cis-isomers and trans-isomers in relatively short method run times [7].…”

“…Additionally, the high number of theoretical plates available when using capillary stationary phases in GC allowed for an easy separation of the cis-isomers and trans-isomers in relatively short method run times [7]. Ramesh and Ravi used both NCI and electron ionization for the quantitation of PERM in whole blood [9,13]. Using NCI they were able to decrease the LOQ of method to 0.02 ng/ml from the 0.2 ng/ml levels that were achieved when using electron ionization.…”

Simultaneous analysis of chlorpyrifos and cypermethrin in cord blood plasma by online solid-phase extraction coupled with liquid chromatography–heated electrospray ionization tandem mass spectrometry

“…After precipitation of proteins in blood samples, chlorpyrifos has been quantitated with LC/MS/MS directly or following column liquid chromatography. LODs of these methods ranged from sub-ppb to 1.5 ppb with an analysis time of approximately 8 min [15,16].…”