Open AccessComparative 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
Author(s) -
Chandrasekar Kandaswamy,
Anandaram Sreekanth,
S. I. Davis Presley,
Ahammed Shabeer
Publication year - 2020
Publication title -
journal of food science and technology/journal of food science and technology
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.656
H-Index - 68
eISSN - 0975-8402
pISSN - 0022-1155
DOI - 10.1007/s13197-020-04605-0
Subject(s) - quechers , chromatography , chemistry , gas chromatography/tandem mass spectrometry , gas chromatography–mass spectrometry , calibration curve , mass spectrometry , analyte , gas chromatography , pesticide residue , detection limit , sample preparation , residue (chemistry) , extraction (chemistry) , amine gas treating , pesticide , organic chemistry , agronomy , biology
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 (C 18 ). 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 0.01 mg kg -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 0.05 mg kg -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.