Simultaneous determination of 223 pesticides in tobacco by GC with simultaneous electron capture and nitrogen-phosphorous detection and mass spectrometric confirmation

Abstract

LSE (liquid-solid extraction), MSPD (matrix solid phase dispersion) and QuEChERS (quick, easy, cheap, effective, rugged and safe) extractions followed by GC-µECD/NPD to determine 223 pesticide residues in tobacco simultaneously were developed and compared. The identities of ten model pesticides were confirmed by GC-MS/MS. The type and amount of dispersant (Florisil, silica gel and alumina), sample mass, cleanup adsorbent, and the eluent (hexane, acetone and acetonitrile) were optimized. Linearity, recovery, LOQ, LOD, and matrix effect were compared. Most recoveries were 71−120% (RSD < 18%). LOD and LOQ were much lower than the CORESTA GRLs. The best method was QuEChERS: acetonitrile extraction and dispersive solid-phase extraction using primary-secondary amine and graphitized carbon.

Influence of QuEChERS modifications on recovery and matrix effect during the multi-residue pesticide analysis in soil by GC/MS/MS and GC/ECD/NPD

“…In the presented work, we used configuration with a “Y” piece at the end of the GC column in order to divide the flux at the end of the GC column into two branches of equal flow (one to the NPD and the other to the ECD), thus allowing pesticides of different nature to be quantified in the same run; 180 pesticides were detected by the ECD, whereas 179 were analyzed by NPD, although ECD and NPD also provided a discernible signal for 143 of them (Łozowicka et al 2015). …”

“…Ouick, Easy, Cheap, Effective, Rugged and Safe ), developed by Anastassiades et al (2003), become a very popular technique for different matrix sample preparations such as: cereals (He et al 2015), fruit and vegetables (Lehotay et al 2010), honey (Bargańska et al 2013), tea (Lozano et al 2012) and tobacco (Łozowicka et al 2015), because of its simplicity, low cost, amenability to high throughput, and high efficiency with a minimal number of steps. It involves two steps, extraction based on partitioning between an aqueous and an organic layer via salting-out and dispersive SPE for further cleanup using combinations of MgSO 4 and different sorbents, such as C 18 , primary-secondary amine (PSA), or graphitized carbon (GCB) to remove interfering substances (Anastassiades et al 2003).…”

A novel and rapid extraction protocol for sensitive and accurate determination of prochloraz in orange juice samples: Vortex‐assisted spraying‐based fine droplet formation liquid‐phase microextraction before gas chromatography–mass spectrometry

“…Gas chromatography–mass spectrometry (GC‐MS) is still a reliable hyphenated instrumental technique to separate and quantify fungicides thanks to its great sensitivity and selectivity 14,17 . In gas chromatographic analyses, it is a common problem to eliminate matrix effects arising from complex matrices such as fruits, herbs, cereals 18,19 . Herein, sample preparation is essential for the identification and quantification of pesticides.…”

“…14,17 In gas chromatographic analyses, it is a common problem to eliminate matrix effects arising from complex matrices such as fruits, herbs, cereals. 18,19 Herein, sample preparation is essential for the identification and quantification of pesticides. Several sample preparation methods have been developed for the purification and preconcentration of the analyte(s) from complex matrices.…”

Application of Hydrophobic Magnetic Nanoparticles as Cleanup Adsorbents for Pesticide Residue Analysis in Fruit, Vegetable, and Various Soil Samples

“…In 2007, the QuEChERS procedure in combination with the dispersive Solid Phase Extraction (dSPE) method was considered one of the advance approach for sample preparation was approved by the International Association of Official Analytical Chemists (AOAC) for the determination of multipesticide residues in vegetables and fruits . Moreover, use of QuEChERS has quickly expanded outside of its traditional field of application to determine a wide variety of contaminants, antibiotics, and other pharmaceuticals, in a broader variety of matrices such as meat, fish, tea, tobacco, blood, rice, and even soil. , The method typically involves two stages. In the first stage, extraction is performed on the separation between the organic and aqueous layers by salting-out.…”