Identification of Unknown Pesticides in Food Using Both LC/MSD TOF and Ion Trap MSn
The document outlines an identification scheme for unknown pesticides that combines liquid chromatography/mass selective detection (LC/MSD) with time-of-flight (TOF) and ion trap options. The approach involves accurate mass determination using LC/MSD TOF followed by MS/MS confirmation using the ion trap, and database analysis against Merck Index or ChemINDEX.
The procedure details a six-step process including initial detection of unknowns in vegetable extracts, checking for isotope patterns (A+2), searching databases for empirical formulas, performing ion trap MS/MS fragmentation analysis, combining data for tentative identification, and final confirmation with authentic standards. Two examples are provided where malathion and buprofezin were identified in cucumber and tomato extracts.
| Column | ZORBAX Eclipse XDB-C8, 4.6 mm x 150 mm x 5 um |
|---|---|
| Flow rate | 0.6 mL/min |
| Injection volume | 50 uL |
| Mobile phase A | ACN |
They are identified by checking for an A+2 ion pattern (approximately 8% intensity) and confirming with MS/MS fragmentation.
The maximum residue limit for banned compounds is set at 0.01 mg/kg.
The column dimensions are 4.6 mm x 150 mm with a particle size of 5 um.
The flow rate used in both methods is 0.6 mL/min.