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.

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 0.01 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.

Evaluation of ozonation technique for pesticide residue removal and its effect on ascorbic acid, cyanidin-3-glucoside, and polyphenols in apple (Malus domesticus) fruits.

Ozonated water dip technique was evaluated for the detoxification of six pesticides, i.e., chlorpyrifos, cypermethrin, azoxystrobin, hexaconazole, methyl parathion, and chlorothalonil from apple fruits. Results revealed that ozonation was better than washing alone. Ozonation for 15 min decreased residues of the test pesticides in the range of from 26.91 to 73.58%, while ozonation for 30 min could remove the pesticide residues by 39.39-95.14 % compared to 19.05-72.80 % by washing. Cypermethrin was the least removed pesticide by washing as well as by ozonation. Chlorothalonil, chlorpyrifos, and azoxystrobin were removed up to 71.45-95.14 % in a 30-min ozonation period. In case of methyl parathion removal, no extra advantage could be obtained by ozonation. The HPLC analysis indicated that ozonation also affected adversely the ascorbic acid and cyanidin-3-glucoside content of apples. However, 11 polyphenols studied showed a mixed trend. Gallic acid, 3,4-dihydroxybenzoic acid, catechin, epicatechin, p-coumaric acid, quercetin-3-O-glucoside, quercetin, and kaempferol were found to decrease while syringic acid, rutin, and resveratrol were found to increase in 30-min ozonation.