Comparative evaluation of multi-residue methods for analysis of pesticide residues in black pepper by gas chromatography tandem mass spectrometry: critical evaluation of matrix co-extractives and method validation.

Abstract

A gas chromatography tandem mass spectrometry method was developed for simultaneous determination of 133 pesticides in Black pepper (Piper nigrum). QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation method is preferred over multistep methods. Extraction was done by using acetonitrile followed by clean up using graphitized carbon, primary secondary amine and octadecyl silica (C18). Even after the cleanup, non-volatile co-extractives stick to the liner and column which results in affecting the performance of the instrument and volatile co-extractives impact the analysis by enhancing the analyte concentration. So we evaluated a dilution procedure to overcome the drawbacks. The limit of quantification of 0.01mgkg-1 was achieved for fifty times diluted sample extract with S/N ≥ 10. The recovery was between 70 and 120% for 0.01, 0.025 and 0.05mgkg-1 for fortified samples and corresponding precision was between 3 and 16% RSD. The seven-level calibration curve shows a regression co-efficient of 0.99.