• Journal of Food Hygiene and Safety
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• v.36 no.3
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• pp.220-227
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• 2021

Fluoroimide is a fungicide and is also used as a pesticide for persimmons and potatoes. The established fluoroimide pesticide analysis method takes a long time to perform and uses benzene, a carcinogen. In addition, a lower limit of quantification is required due to enforcement of the Positive List System. Therefore, this study aimed to improve the analysis method for residual fluoroimide to resolve the problems associated with the current method. The analytical method was improved with reference to the increased stability of fluoroimide under acidic conditions. Fluoroimide was extracted under acidic conditions by hydrogen chloride (4 N) and acetic acid. MgSO₄ and NaCl were used with acetonitrile. C₁₈ (octadecylsilane) 500 mg and graphitized carbon black 40 mg were used in the purification process. The experiment was conducted with agricultural products (hulled rice, potato, soybean, mandarin, green pepper), and liquid chromatograph-tandem mass spectrometry was used for the instrumental analysis. Recovery of fluoroimide was 85.7-106.9% with relative standard deviations (RSDs) of less than 15.6%. This study reports an improved method for the analysis of fluoroimide that might contribute to safety by substituting the use of benzene, a harmful solvent. Furthermore, the use of QuEChERS increased the efficiency of the improved method. Finally, this research confirmed the precise limit of quantification and these results could be used to improve the analysis of other residual pesticides in agricultural products.

• Journal of Food Hygiene and Safety
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• v.37 no.2
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• pp.69-79
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• 2022

The purpose of this study is to monitor the pesticide residues in frozen fruits and vegetables distributed and sold in online and offline markets in Korea. For the study, 107 samples of 34 types of frozen fruits and vegetables were examined, and a total of 341 pesticide residues were analyzed by using multiclass pesticide multi-residue methods of the Korean Food Code. As a result, pesticide residues were detected from 16 of 64 frozen fruits samples and 15 of 43 frozen vegetables samples. Conclusively, residues were detected from 31 samples in total, showing a detection rate of 29.0%. Specifically, pyridaben exceeded the Maximum Residue Limits (MRLs) based on the Positive list system (PLS) in one of the frozen radish leaves, and the violation rate was 0.9%. Detection on frozen fruits and vegetables was made 23 times for 11 types and 36 times for 21 types. In total, 28 types of pesticide residues were detected 59 times. Fungicides were detected the most in frozen fruits, while insecticides were detected the most in frozen vegetables. The most detected pesticides were the insecticide, acaricide chlorfenapyr (5) and the fungicide boscalid (5). Chlorfenapyr was detected only in frozen vegetables, and boscalid was detected in frozen fruits except one.

• Journal of Food Hygiene and Safety
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• v.39 no.3
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• pp.221-230
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• 2024

Pesticide residues were monitored in dried red pepper and pepper powder samples purchased in Northern Gyeonggi-do and from domestic online markets. The QuEChERS method was used to prepare 88 samples. GC-MS/MS and LC-MS/MS were used to analyze 338 pesticide residues. In the study, pesticide residues were detected in 70 samples (79.5%), with residues exceeding the maximum residue limits (MRL) in 4 samples (4.5%). Pesticide levels exceeded the MRL in imported samples, with two samples of dried red pepper and two samples of pepper powder showing elevated levels. Among the 61 pesticides detected, tebuconazole, a fungicide was most frequently detected (52 times). Tricyclazole, which is used to control the main disease affecting rice, exceeding the MRL in 3 of 12 Vietnam-origin samples. Ethion exceeded the MRL in one Indian-origin sample. Both tricyclazole and ethion are banned for use in pepper products in Korea and are regulated under the positive list system (PLS). Conversely, pesticides detected in domestic samples were within the MRLs. Therefore, authorities should monitor pesticide residues in imported red pepper products.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.227-234
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• 2019

An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.