Validated analytical methodology for the simultaneous determination of a wide range of pesticides in human blood using GC–MS/MS and LC–ESI/MS/MS and its application in two poisoning cases

Abstract

Pesticides are frequently responsible for human poisoning and often the information on the involved substance is lacking. The great variety of pesticides that could be responsible for intoxication makes necessary the development of powerful and versatile analytical methodologies, which allows the identification of the unknown toxic substance. Here we developed a methodology for simultaneous identification and quantification in human blood of 109 highly toxic pesticides. The application of this analytical scheme would help in minimizing the cost of this type of chemical identification, maximizing the chances of identifying the pesticide involved. In the methodology that we present here, we use a liquid-liquid extraction, followed by one single purification step, and quantitation of analytes by a combination of liquid and gas chromatography, both coupled to triple quadrupole mass spectrometry, which is operated in the mode of multiple reaction monitoring. The methodology has been fully validated, and its applicability has been demonstrated in two recent cases involving one self-poisoning fatality and one non-fatal homicidal attempt.

Optimization and validation of a QuEChERS-based method for the simultaneous environmental monitoring of 218 pesticide residues in clay loam soil

“…The chromatographic parameters had been previously optimized by our group, so no further modifications were made either to the oven temperature ramp or to the column type due to the good results obtained for similar analytes (Luzardo et al, 2015;Luzardo et al, 2014). However, as the solvent chosen in those methods had been cyclohexane, it was necessary to optimize some parameters.…”

A molecularly imprinted nanofilm‐based quartz crystal microbalance sensor for the real‐time detection of pirimicarb

“…In past years, pesticide residues in food were detected by different chromatographic methods . Although chromatographic methods possess the key advantages of accuracy and sensitivity, their disadvantages include high cost, difficulty of use, complex and higher‐quantity sample pretreatment, inability to perform online analysis, and the use of large amounts of organic solvents .…”

Pestisit Tayini için Nanopartiküllerle Duyarlılığı Arttırılmış Moleküler Baskılama Temelli Yüzey Plazmon Rezonans Sensörlerin Hazırlanması

“…Langmuir adsorpsiyon modelinin klorpirifos baskılı SPR sensör için en uygun model olduğu belirlendi. Nanosensör 0.015 nM seviyelerinde klorpirifos un tayininde kullanılan elektrokimyasal sensör metotları (Mauriz et al, 2006;Terese Marie and Drexel, 2017) ve kromatografik (Kouzayha et al, 2012;Luzardo et al, 2015) gibi farklı yöntemler ile karşılaştırılabilir. Bu yöntemlerin aksine, sunulan SPR biyosensör direkt olarak klorpirifosu yüksek hassasiyet ve seçicilikte tayin etmiştir.…”