• Journal of Food Hygiene and Safety
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• v.30 no.3
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• pp.272-280
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• 2015

A simultaneous official method was developed for the determination of phorate and its metabolites (phorate sulfoxide, phorate sulfone, phorate oxon, phorate oxon sulfoxide, phorate oxon sulfone) in livestock samples. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Phorate and its metabolites were extracted from beef and milk samples with acidified acetonitrile (containing 1% acetic acid) and partitioned with anhydrous magnesium sulfate. Then, the extract was purified through primary secondary amine (PSA) and C18 dispersive sorbent. Matrix matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/L) for all the analytes into blank extract with $r^2$ > 0.996. For validation purposes, recovery studies were carried out at three different concentration levels (beef 0.004, 0.04 and 0.2 mg/kg; milk 0.008, 0.04 and 0.2 mg/kg, n = 5). The recoveries were within 79.2-113.9% with relative standard deviations (RSDs) less than 19.2% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines. The limit of quantification was quite lower than the maximum residue limit (MRL) set by the Ministry of Food and Drug Safety (0.05 mg/kg). The proposed analytical method was accurate, effective and sensitive for phorate and its metabolites determination and it will be used to as an official analytical method in Korea.

• Korean Journal of Environmental Agriculture
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• v.40 no.4
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• pp.353-358
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• 2021

BACKGROUND: Prochloraz has been widely used as an imidazole fungicide on fruits and vegetables in Korea. Analytical approaches to evaluate prochloraz residues in herbal medicine are required for their safety management. In this study, we developed a GC-ECD method for quantitative determination of prochloraz in Platycodi Radix. The metabolite 2,4,6-trichlorophenol (2,4,6-T) was used as a target compound to evaluate total prochloraz residues as it is categorized to a representative residue definition of prochloraz. All residues containing 2,4,6-T were converted to 2,4,6-T and subjected to GC-ECD. METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining prochloraz and it metabolite 2,4,6-T in Platycodi Radix. Prochloraz and its metabolite 2,4,6-T residuals were extracted using acetone. The extract was diluted with and partitioned directly into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was decomposed to 2,4,6-T, and then the partitioned ion-associate was finally purified by optimized aminopropyl solid-phase extraction (SPE). The limits of quantitation of the method (MLOQs) were 0.04 mg/kg and 0.02 mg/kg, respectively for prochloraz and 2,4,6-T, considering the maximum residue level (MRL) of prochloraz as 0.05 mg/kg in Platycodi Radix. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (82.1-89.7%). Good reproducibilities were obtained (coefficient of variation < 2.8%), and the linearities of calibration curves were reasonable (r² > 0.9986) in the range of 0.005-0.5 ㎍/mL. CONCLUSION(S): The method developed in this study was successfully validated to meet the guidelines required for quantitative determination of pesticides in herbal medicine. Thus, the method could be useful to monitor prochloraz institutionally in herbal medicine.

• Journal of Food Hygiene and Safety
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• v.34 no.4
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• pp.340-347
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• 2019

We performed a safety survey on residual pesticides in dried agricultural products. A total of 110 samples of dried agricultural products distributed in Gyeonggi-do were analyzed for 263 pesticides according to multi class pesiticide multiresidue method. Ten types of pesticides were detected in 10 samples. Chlorpyrifos was detected in Ricinus communis leaves, chlorpyrifos, hexaconazole, pyridalyl in Chwinamul (wild aster), diniconazole, isoprothiolane, lufenuron in radish leaves, hexaconazole in Cirsium setidens (Korean thistle), bifenthrin, and chlorothalonil, boscalid, and pyraclostrobin in pepper leaves. The detection rate of pesticides was 9.1%, and among these samples, one was detected over Maximum Residue Limits (MRLs). In the validation study, the values of limit of detection (LOD), limit of quantitation (LOQ), coefficient of determination ($R^2$) and recovery were in the range of 0.002~0.027 mg/kg, 0.006~0.083 mg/kg, 0.9964~1.0000 and 74.8~118.9%, respectively. The Positive List System (PLS) was newly introduced as part of the safety management of residual pesticide in agricultural products in Korea in 2019. With the application of the PLS, if the MRL is not established, 0.01 mg/kg limit is applied uniformly. In spite, these of strengthened residue limits, the MRLs of dried agricultural products are still insufficient. Therefore, this study could be utilized as basic data for the setting of proper MRLs.

• Korean Journal of Food Science and Technology
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• v.51 no.4
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• pp.316-323
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• 2019

It is difficult to analyze pymetrozine in citrus fruits using the hydromatrix method because of its low efficiency of purification and overlap of matrix and pymetrozine peaks. Liquid-liquid extraction can analyze pymetrozine in citrus fruits using dichloromethane. Since low pH interferes with the extraction of pymetrozine, the extracts of citrus fruits were maintained over pH 7.0 by adding borax buffer and 1 N NaOH in the improved method. According to the improved method, citrus fruits (such as lemon, lime, orange, tangerine, and grapefruit) were extracted and purified for HPLC-photo diode array analysis. The results of validation were as follows: $4.360{\mu}g/kg$ of limit of detection, $14.533{\mu}g/kg$ of limit of quantitation, and 0.007 mg/kg of method quantitative limit. Citrus fruits spiked with pymetrozine showed a recovery range from 71.8 to 83.7% and a coefficient of variation below 6%. Thus, the improved method can efficiently analyze pymetrozine in citrus fruits.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.283-289
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• 2019

This study was performed to monitor the residual pesticides in agricultural products used in school foodservice in the Gwangju metropolitan area. Risk assessment was also carried out based on the amount of agricultural products consumed. A total of 320 agricultural products supplied to schools in Gwangju were analyzed from 2015 to 2017. The pre-treatment and residual pesticide analysis of these products was conducted in accordance with the second method for multi-residue analysis of pesticides in the Korean food code. The hazard index was calculated by dividing the estimated daily intake (EDI) of pesticides by the acceptable daily intake (ADI). The linearity correlation coefficient for the calibration curve was 0.9923 to 1.0000, LOD 0.004 to 0.019 mg/kg, LOQ 0.012 to 0.057 mg/kg, and recovery was 79.1 to 100.2%. Residual pesticides were detected in 18 (5.6%) of 320 agricultural products used for school foodservice, and one sample of sweet potato stem (0.3%) exceeded the maximum residual limit (MRL). The detection frequency for chili peppers and bell peppers was higher than that for other agricultural products. The frequently-detected pesticides were boscalid and acetamiprid. These results showed that residual pesticide management is needed for chili pepper, bell pepper and sweet potato stem among agricultural products supplied to schools. The hazard index of bifenthrin in sweet potato stem showed the highest (64.18%), and the other pesticides were 0.03-8.23%. These results indicated that agricultural products supplied to schools in Gwangju were safe for consumption. To minimize the intake of residual pesticides, it is necessary to not only thoroughly wash agricultural products but to also ensure the expanded supply of products that are pesticide-free.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.235-241
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• 2019

An analytical method was developed for the determination of an antibiotic fungicide, kasugamycin, in agricultural products (hulled rice, potato, soybean, mandarin and green pepper) using liquid chromatographytandem mass spectrometry (LC-MS/MS). Samples were extracted with methanol adjusted to pH 13 using 1 N sodium hydroxide, and purified with a HLB (hydrophilic lipophilic balance) cartridge. Linearity of a matrix-matched calibration curve using seven concentration levels, from 0.001 to 0.1 mg/kg, was excellent with a correlation coefficient ($R^2$) of more than 0.9998. The limits of detection (LOD) and quantification (LOQ) of instrument were 0.0005 and $0.001{\mu}g/mL$, respectively, and the LOQ of analytical method calculated as 0.01 mg/kg. The average recoveries at three spiking levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) were in the range of 71.2~95.4% with relative standard deviation of less than 12.1%. The developed method was simple and all optimized results was satisfied with the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. The present study could be served as a reference for the establishment of maximum residue limits (MRL) of kasugamycin and be used as basic data for safety management relative to kasugamycin residues in imported and domestic agricultural products.

• Korean Journal of Food Science and Technology
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• v.54 no.2
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• pp.218-223
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• 2022

This study, conducted during 2018-2021 in Gangseo, Seoul, monitored residual pesticides in 14 types of fresh-cut produce, including lettuce, tomato, and celery, in wholesale market and supermarkets. A total of 589 cases (2.9%) were inspected; 17 cases (2.9%) were detected within the criteria, and 2 cases (0.3%) exceeded the maximum residual limit (MRL). When assessing the distribution stage of the pesticide violation, there were two violations in the wholesale market (before distribution), which differed from the supermarkets (during distribution). The detected pesticides, mainly insecticides and fungicides, appeared in the order of flubendiamide, flufenoxuron, and diazinon. A violation rate of 0.3% was found for wholesale market, which is collection area dedicated to fresh-cut produce, and this was lower than that for general agricultural products (1.4-2.5%). Since fresh-cut produce are consumed immediately after simple processing, residual pesticides significantly affect the human body; therefore, continuous monitoring of pesticide residues is required.

• Journal of Food Hygiene and Safety
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• v.37 no.3
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• pp.136-142
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• 2022

The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO₄, primary secondary amine (PSA), and octadecyl (C₁₈), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R²) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.

• Journal of Food Hygiene and Safety
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• v.37 no.4
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• pp.249-259
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• 2022

This study investigated pesticide residues in 7,069 agricultural products distributed in the city of Incheon from 2019 to 2021. Ingestion of pesticides can cause serious carcinogenic, endocrine, neurological, and reproductive problems. Pesticide residues in the samples were analyzed using various multi-residue methods (GC-MS/MS, GC-ECD/NPD, LC-MS/MS, and HPLC-UVD) on the Korean Food Code. The violation rate of the samples exceeding the maximum residue level (MRL) of pesticide residues for the years 2019, 2020, and 2021 was 1.0%, 1.4%, and 1.1%, respectively. Diazinon, flubendiamide, procymidone, fluxametamide, and fluquinconazole were the most frequently reported violative pesticide residues. Most commonly encountered agricultural products exceeding MRLs were coriander leaves, chamnamul, chwinamul, welsh onion, and crown daisy. Agricultural products and pesticides frequently exceeding MRLs should be continuously inspected for food safety. Continuous monitoring of pesticide residues in agricultural products is indispensable to improve consumer safety by preventing the distribution of agricultural products exceeding MRLs.

• Journal of Food Hygiene and Safety
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• v.38 no.6
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• pp.457-463
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• 2023

To investigate residual pesticide levels in agricultural products contained in Meal-kits, 27 Meal-kit products were collected from marts, Meal-kit shops, and online stores in Incheon City, South Korea. Seventy-six vegetable and thirty-seven mushroom products were analyzed for residual levels of 339 pesticides. Residual pesticides were detected in 23 out of 76 vegetables and were not present in the 37 mushroom products. The residual pesticide detection rate was 20.4% (23/113 cases). The pesticides famoxadone 0.034 mg/kg (standard: 0.01 mg/kg or less, PLS) and fenpyroximate 0.302 mg/kg (standard: 0.01 mg/kg or less, PLS) exceeded their maximum residue levels (MRL). This survey revealed that various types of pesticides remain in agricultural products in Meal-kits. Due to the nature of Meal-kit products, there is no separate standard for residual pesticides in agricultural products. Therefore, continuous monitoring of residual pesticides is necessary.