A simple and inexpensive "solvent in silicone tube extraction" approach and its evaluation in the gas chromatographic analysis of pesticides in fruits and vegetables

A novel, simple, and inexpensive approach to sorptive extraction, which we call solvent in silicone tube extraction (SiSTEx), was applied to pesticide residue analysis and its effectiveness and efficiency were evaluated. In SiSTEx, which is a form of open tubular sorptive extraction, a piece of silicone tubing (4 cm long, 1.47 mm ID, 1.96 min OD in this study) is attached to the cap of a 20 ml, glass vial that contains the aqueous sample. The tubing is plugged at the end dangling in the sample solution, and MeCN (e.g., 40 μL) added by syringe to the inner tube volume through a septum in the cap. A stir-bar is used to mix the sample for a certain time (e.g., 60 min), which allows chemicals to partition into the tubing where they diffuse across the silicone and partition into the MeCN. The final MeCN extract is then analyzed for the concentrated analytes. In this study, the SiSTEx approach was evaluated for the analysis of organophosphorus (OP) and organochlorine (OC) pesticides in fruits and vegetables using GC/pulsed flame photometric (PFPD) and halogen specific (XSD) detectors for analysis. The produced samples were initially extracted by a rapid MeCN procedure, and 5 mL of the initial extract was diluted four-fold with water to undergo sorptive extraction for 60 min. The final extract was analyzed by GC/PFPD + XSD for 14 OP and 22 OC pesticides. This simple approach was able to detect 26 of the 36 pesticides at 10 ng/g or less original equivalent sample concentration with average reproducibility of 11 %RSD. For those 26 pesticides, a 44-fold lower detection limit on average was achieved in matrix extracts using SiSTEx despite the four-fold dilution with water.