Dissipation kinetics, pre-harvest residue limits, and hazard quotient assessments of pesticides flubendiamide and fluopicolide in Korean melon (Cucumis melo L. var. makuwa) grown under regulated conditions in plastic greenhouses.

The dissipation kinetics, pre-harvest residue limits, and hazard quotient (HQ) assessments of the pesticides flubendiamide and fluopicolide were conducted for Korean melon (Cucumis melo L. var. makuwa) cultivated at two different sites. A single extraction and cleanup procedure was carried out using acetone (partitioned with dichloromethane) and amino solid-phase extraction cartridges, respectively. Residue analysis was performed by HPLC with ultraviolet detection. Both pesticides showed excellent linearity with correlation coefficients of 0.9999 and 0.9996 for flubendiamide and fluopicolide, respectively. The accuracy (expressed as recovery %) at three spiking levels was 92.0-103.6 and 82.8-105.3%, and the precision (expressed as relative standard deviation) was 1.7-3.4 and 2.7-5.3% for flubendiamide and fluopicolide, respectively. The initial residues of flubendiamide/fluopicolide were 0.326/0.376 and 0.206/0.298 mg/kg at sites 1 and 2, respectively. These amounts were substantially lower than the maximum residue limits (MRLs = 1 and 0.5 mg/kg for flubendiamide and fluopicolide, respectively) established by the Korean Ministry of Food and Drug Safety. The half-lives of flubendiamide were 5.8 and 6.5 days, and those of fluopicolide were 6.7 and 9.1 days at sites 1 and 2, respectively. The shorter half-lives were attributed to seasonal variations (higher temperatures) and enzymatic and metabolic profiling. The risk assessment HQs of flubendiamide were 0.217/0.249 on day 0, which decreased to 0.102/0.168 on day 5, and to 0.065/0.88 on day 10; the HQ values for fluopicolide were 0.029/0.042, 0.022/0.025, and 0.010/0.019 on day 0, day 5, and day 10, for sites 1/2, respectively. From this data, we concluded that the fruits could be consumed safely.

A Liquid Chromatography - Tandem Mass Spectrometry Approach for the Identification of Mebendazole Residue in Pork, Chicken, and Horse.

A confirmatory and quantitative method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of mebendazole and its hydrolyzed and reduced metabolites in pork, chicken, and horse muscles was developed and validated in this study. Anthelmintic compounds were extracted with ethyl acetate after sample mixture was made alkaline followed by liquid chromatographic separation using a reversed phase C18 column. Gradient elution was performed with a mobile phase consisting of water containing 10 mM ammonium formate and methanol. This confirmatory method was validated according to EU requirements. Evaluated validation parameters included specificity, accuracy, precision (repeatability and within-laboratory reproducibility), analytical limits (decision limit and detection limit), and applicability. Most parameters were proved to be conforming to the EU requirements. The decision limit (CCα) and detection capability (CCß) for all analytes ranged from 15.84 to 17.96 µgkg-1. The limit of detection (LOD) and the limit of quantification (LOQ) for all analytes were 0.07 µgkg-1 and 0.2 µgkg-1, respectively. The developed method was successfully applied to monitoring samples collected from the markets in major cities and proven great potential to be used as a regulatory tool to determine mebendazole residues in animal based foods.

Estimation of Apple Intake for the Exposure Assessment of Residual Chemicals Using Korea National Health and Nutrition Examination Survey Database.

The aims of this study were to develop strategies and algorithms of calculating food commodity intake suitable for exposure assessment of residual chemicals by using the food intake database of Korea National Health and Nutrition Examination Survey (KNHANES). In this study, apples and their processed food products were chosen as a model food for accurate calculation of food commodity intakes uthrough the recently developed Korea food commodity intake calculation (KFCIC) software. The average daily intakes of total apples in Korea Health Statistics were 29.60 g in 2008, 32.40 g in 2009, 34.30 g in 2010, 28.10 g in 2011, and 24.60 g in 2012. The average daily intakes of apples by KFCIC software was 2.65 g higher than that by Korea Health Statistics. The food intake data in Korea Health Statistics might have less reflected the intake of apples from mixed and processed foods than KFCIC software has. These results can affect outcome of risk assessment for residual chemicals in foods. Therefore, the accurate estimation of the average daily intake of food commodities is very important, and more data for food intakes and recipes have to be applied to improve the quality of data. Nevertheless, this study can contribute to the predictive estimation of exposure to possible residual chemicals and subsequent analysis for their potential risks.

Contributing effect of various washing procedures and additives on the decline pattern of diethofencarb in crown daisy, a model of leafy vegetables.

The effects of various washing procedures, including stagnant, running, and stagnant and running tap water, and the use of washing solutions and additives, namely NaCl (1% and 2%), vinegar (2%, 5%, and 10%), detergent (0.5% and 1%), and charcoal (1% and 2%), on the reduction rate of diethofencarb were estimated in field-incurred crown daisy, a model of leafy vegetables, grown under greenhouses located in 3 different areas (Gwangju, Naju, and Muan). The original Quick, Easy, Cheap, Effective, Rugged, and Safe "QuEChERS" method was modified for extraction and liquid chromatography-tandem mass spectrometry (LC/MS/MS) was used for analysis. The recovery of diethofencarb in unwashed and washed samples was satisfactory and ranged between 84.28% and 115.32% with relative standard deviations (RSDs) of <6%. The residual levels decreased following washing with stagnant, running, and stagnant+running tap water (i.e., decline in levels increased from 65.08% to 85.02%, 69.99 to 86.79, and 74.75 to 88.96, respectively). The percentage of decline increased and ranged from 77.46% to 91.19% following washing with various solutions. Application of 1% detergent was found to be the most effective washing method for reducing the residues in crown daisy. Additionally, washing with stagnant and running tap water or even stagnant water for 5 min might reduce the residue levels substantially, making the prepared food safe for human consumption.

Detection of pyridaben residue levels in hot pepper fruit and leaves by liquid chromatography-tandem mass spectrometry: effect of household processes.

Following quick, easy, cheap, effective, rugged and safe (QuEChERS) and LC/MS/MS analysis, pyridaben residual levels were determined in unprocessed and processed hot pepper fruit and leaves. The linearities were satisfactory with determination coefficients (R(2)) in excess of 0.995 in processed and unprocessed pepper fruit and leaves. Recoveries at various concentrations were 79.9-105.1% with relative standard deviations ≤15%. The limits of quantitation of 0.003-0.012 mg/kg were very low compared with the maximum residue limits (2-5 mg/kg) set by the Ministry of Food and Drug Safety, Republic of Korea. The effects of various household processes, including washing, blanching, frying and drying under different conditions (water volume, blanching time and temperature) on residual concentrations were evaluated. Both washing and blanching (in combination with high water volume and time factor) significantly reduced residue levels in hot pepper fruit and leaves compared with other processes. In sum, the developed method was satisfactory and could be used to accurately detect residues in unprocessed and processed pepper fruit and leaves. It is recommended that pepper fruit/leaves be blanched after washing before being consumed to protect consumers from the negative health effects of detected pesticide residues.