title: Development of extraction procedures for the determination of imidacloprid: application to residue analysis and dynamics of two formulations in Chinese cabbage.
abstract: This study was undertaken to investigate whether an additional column clean-up procedure can affect the accuracy of an analytical method developed for the determination of imidacloprid residues in Chinese cabbage. Thereafter, the residue levels and the degradation rates of imidacloprid were investigated in experimental Chinese cabbage plots after treatment with two different commercial formulations: emulsifiable concentrate (EC) and wettable powder (WP). The analyte was determined using high-performance liquid chromatography-ultraviolet detection (HPLC-UVD) and confirmed by high-performance liquid chromatography-mass spectrometry (HPLC-MS) in the select ion-monitoring mode. The mean recoveries ranged from 75.34 to 98.00% and 96.95 to 100.97%, with relative standard deviations of 0.86-4.14 and 1.22-3.52%, in samples treated with and without additional column clean-up procedures, respectively. The minimum detectable amount of imidacloprid was 4 ng, while the limits of detection and quantitation were 0.2 and 0.5 ppm, respectively. The degradation of pesticide was monitored throughout a period of 13 days under greenhouse conditions. Although the behaviors of the EC and WP formulations appear to be similar, the absolute residue levels obtained with EC and WP treatments differed slightly. When imidacloprid formulations were applied (as foliar treatments) according to the recommended rate, the final residues (13 days post-treatment) in Chinese cabbage were much lower than the maximum residue limit (MRL = 3.5 ppm) established by the Korean Food and Drug Administration. Taken together, our study suggests that the analysis of imidacloprid can be performed without an additional column clean-up procedure, and the decline curve and the residue levels in Chinese cabbage could change if the same active ingredient is used in different formulations.
authors.affiliation: Natural Products Chemistry Laboratory, Institute of Agricultural Science and Technology, College of Agriculture and Life Science, Chonnam National University, 300 Yong-Bong Dong, Buk-Ku, Gwangju 500-757, Republic of Korea.
authors.forename: Sathya
authors.initials: S
authors.lastname: Khay
authors.forename: A M
authors.initials: AM
authors.lastname: Abd El-Aty
authors.forename: Soon-Kil
authors.initials: SK
authors.lastname: Cho
authors.forename: Jeong-Heui
authors.initials: JH
authors.lastname: Choi
authors.forename: M I R
authors.initials: MI
authors.lastname: Mamun
authors.forename: Ayman
authors.initials: A
authors.lastname: Goudah
authors.forename: Ho-Chul
authors.initials: HC
authors.lastname: Shin
authors.forename: Jae-Han
authors.initials: JH
authors.lastname: Shim
mesh_terms: D001937:Brassica / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D007093:Imidazoles / Q000032:analysis*; D007306:Insecticides / Q000032:analysis*; D000073943:Neonicotinoids; D009574:Nitro Compounds / Q000032:analysis*; D010573:Pesticide Residues / Q000032:analysis*; D010936:Plant Extracts / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013056:Spectrophotometry, Ultraviolet
chemical_list: D007093:Imidazoles; D007306:Insecticides; D000073943:Neonicotinoids; D009574:Nitro Compounds; D010573:Pesticide Residues; D010936:Plant Extracts; C082359:imidacloprid