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Development and Validation of an Analytical Method for Fenpropimorph in Agricultural Products Using QuEChERS and LC-MS/MS (QuEChERS법과 LC-MS/MS를 이용한 농산물 중 Fenpropimorph 시험법 개발 및 검증)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.115-123
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    • 2019
  • An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

Contents of vitamin B9 (folate) and B12 (cobalamins) in commonly consumed seafood menus in Korea (한국인 상용 수산물 식단의 비타민 B9과 B12 함량)

  • Park, Eun-Young;Jeong, Bomi;Chun, Jiyeon
    • Journal of Nutrition and Health
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    • v.54 no.2
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    • pp.211-223
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    • 2021
  • Purpose: A total of 39 seafood menus were prepared according to the Korean standard recipe, and analyzed for vitamin B9 (folate) and B12 (cobalamins) contents, using validated applied analytical methods. The menus included Guk/Tang/Jjigae (boiled or stewed dishes, n = 10), Bokkeum (stir-fried dishes, n = 10), Jjim/Jorim (braised or steamed dishes, n = 7), Gui (baked or grilled dishes, n = 7), Twigim (deep-fried dishes, n = 2) and Muchim (dried or blanched-seasoned dishes, n = 3). Methods: The contents of vitamin B9 and B12 in all food samples were determined by the trienzyme extraction-Lactobacillus casei and immunoaffinity-high-performance liquid chromatography/photodiode array detection methods. Analytical quality control was performed in order to assure reliability of the analysis. Results: Accuracy (97.4-100.6% recoveries) and precision (< 6% relative standard deviations for repeatability and reproducibility) of vitamin B9 and B12 analyses were determined to be excellent. The vitamin B9 and B12 contents of the 39 seafood menus evaluated, varied in the range of 1.83-523.08 ㎍/100 g and 0.11-38.30 ㎍/100 g, respectively, depending on the ingredients and cooking methods. The vitamin B9 content was highest in Jomi-gim (523.08 ㎍/100 g), followed by Geonsaeu-bokkeum (128.34 ㎍/100 g) and Janmyeolchi-bokkeum (121.53 ㎍/100 g). Vitamin B12 was detected in all seafood menus, with highest level obtained in Kkomack-jjim (41.58 ㎍/100 g). The seaweed dish was found to have high levels of both vitamin B9 and B12. All assays were performed under strict quality control. Conclusion: Guk and Tang menus, which contain a large amount of water, were relatively lower in the vitamin B9 and B12 contents than the other menus. Bokkeum menus containing various vegetables were high in the vitamin B9 content, but the vitamin B12 content was dependent on the type of seafood used in the menu.

Characterization of compounds and quantitative analysis of oleuropein in commercial olive leaf extracts (상업용 올리브 잎 추출물의 화합물 특성과 이들의 oleuropein 함량 비교분석)

  • Park, Mi Hyeon;Kim, Doo-Young;Arbianto, Alfan Danny;Kim, Jung-Hee;Lee, Seong Mi;Ryu, Hyung Won;Oh, Sei-Ryang
    • Journal of Applied Biological Chemistry
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    • v.64 no.2
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    • pp.113-119
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    • 2021
  • Olive (Olea europaea L.) leaves, a raw material for health functional foods and cosmetics have abundant polyphenols including oleuropein (major bioactive compound) with various biological activities: antioxidant, antibacterial, antiviral, anticancer activity, and inhibit platelet activation. Oleuropein has been reported as skin protectant, antioxidant, anti-ageing, anti-cancer, anti-inflammation, anti-atherogenic, anti-viral, and anti-microbial activity. Despite oleuropein is the important compound in olive leaves, there is still no quantitative approach to reveal oleuropein content in commercial products. Therefore, a validated method of analysis has to develop for oleuropein. In this study, the components and oleuropein content in 10 types of products were analyzed using a developed method with ultra-performance liquid chromatography to quadrupole time-of-flight mass spectrometry, charge of aerosol detector, and photodiode array. The total of 18 compounds including iridoids (1, 3, 4, 14, and 16-18), coumarin (2), phenylethanoids (5, 9, and 11), flavonoids (6-8, 10, 12, and 13), lignan (15), were tentatively identified in the leaves extract based high resolution mass spectrometry data, and the content of oleuropein in each product was almost identical between two detection methods. The oleuropein in three commercial product (A, G, H) was contained more over the suggested content, and it of five products (B, E, H, I, J) were analyzed within 5-10% error range. However, the two products (C, D) were found far lower than suggested contents. This study provides that analytical results of oleuropein could be a potential information for the quality control of leaf extract for a manufactured functional food.

A Study on the Use of Scientific Investigation Equipment to Support Decision-making of the Resident Evacuation in the Event of a Chemical Accident (화학사고 발생에 따른 주민대피 의사결정 지원을 위한 과학조사장비 활용방안 연구)

  • Oh, Joo-Yeon;Lee, Tae Wook;Cho, Kuk
    • Korean Journal of Remote Sensing
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    • v.38 no.6_3
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    • pp.1817-1826
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    • 2022
  • After the hydrogen fluoride leak in Gumi in 2012, the government has been systemizing the disaster management system, such as responding to and managing chemical accidents. In particular, the Ministry of the Interior and Safety (MOIS) is in charge of evacuation of residents following chemical accidents based on the Framework Act on Management of Disaster and Safety. In this study, an application plan was presented to support and utilize the decision-making support for evacuation of residents after a chemical accident using the chemical accident investigation equipment of the National Disaster Management Research Institute (NDMI). In the equipment operation system for scientific information collection due to chemical accidents, the roles and purpose of use of long/short distance measurement equipment were presented according to regular and emergency situations. Using the data acquired through long/short distance measurement equipment, it can be used as basic data for resident evacuation decision-making by monitoring whether chemicals are detected in an emergency and managing data on detected substances by company in a regular situation. As a result of measuring chemical substances in order to verify on-site usability by equipment only for the regular operation system, it was confirmed that real-time detection of chemical substances is possible with long distance measuring equipment. In addition, it was confirmed that it was necessary to check the measurable distance and range of the equipment in the future. In the case of short distance measurement equipment, hydrocarbon-based substances were mainly detected, and it was confirmed that it was measured at a higher level in Ulsan-Mipo National Industrial Complex than in Onsan National Industrial Complex. It is expected that it can be used as basic data to support decision-making in the event of chemical accidents through continuous data construction in the future.

Risk Assessment of Heavy Metals Migrated from Plastic Food Utensils, Containers, and Packaging Distributed in Korea (국내 유통 식품용 플라스틱 기구 및 용기, 포장의 중금속 위해도 평가)

  • Kyung Youn, Lee;Hyung Soo, Kim;Dae Yong, Jang;Ye Ji, Koo;Seung Ha, Lee;Hye Bin, Yeo;Ji Su, Yoon;Kyung-Min, Lim;Jaeyun, Choi
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.28 no.3
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    • pp.175-182
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    • 2022
  • Heavy metals can be intentionally or unintentionally introduced into plastic food utensils, containers, and packaging (PFUCP) as additives or contaminants, which can be ingested with food by humans. Here, seven-heavy metals (lead, cadmium, nickel, chromium, antimony, copper, and manganese) with toxicity concerns were selected, and risk assessment was done by establishing their migration from 137 PFUCP products made of 16 materials distributed in Korea. Migration of heavy metals was examined by applying 4% acetic acid as a food simulant (70℃, 30 minutes) to the PFUCP products. Inductively coupled plasma mass spectrometry (ICP-MS) was employed for the analysis of migrated heavy metals, and the reliability of quantitative results was confirmed by checking linearity, LOD, LOQ, recovery, precision, and expanded uncertainty. As a result of monitoring, heavy metals were detected at a level of non-detection to 8.76 ± 11.87 ㎍/L and most of the heavy metals investigated were only detected at trace amounts of less than 1 ㎍/L on average. However, antimony migrated from PET products was significantly higher than other groups. Risk assessment revealed that all the heavy metals investigated were safe with a margin of exposure above 311. Collectively, we demonstrated that heavy metals migrated from PFUCP products distributed in Korea appear to be within the safe range.

Deep Learning Approaches for Accurate Weed Area Assessment in Maize Fields (딥러닝 기반 옥수수 포장의 잡초 면적 평가)

  • Hyeok-jin Bak;Dongwon Kwon;Wan-Gyu Sang;Ho-young Ban;Sungyul Chang;Jae-Kyeong Baek;Yun-Ho Lee;Woo-jin Im;Myung-chul Seo;Jung-Il Cho
    • Korean Journal of Agricultural and Forest Meteorology
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    • v.25 no.1
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    • pp.17-27
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    • 2023
  • Weeds are one of the factors that reduce crop yield through nutrient and photosynthetic competition. Quantification of weed density are an important part of making accurate decisions for precision weeding. In this study, we tried to quantify the density of weeds in images of maize fields taken by unmanned aerial vehicle (UAV). UAV image data collection took place in maize fields from May 17 to June 4, 2021, when maize was in its early growth stage. UAV images were labeled with pixels from maize and those without and the cropped to be used as the input data of the semantic segmentation network for the maize detection model. We trained a model to separate maize from background using the deep learning segmentation networks DeepLabV3+, U-Net, Linknet, and FPN. All four models showed pixel accuracy of 0.97, and the mIOU score was 0.76 and 0.74 in DeepLabV3+ and U-Net, higher than 0.69 for Linknet and FPN. Weed density was calculated as the difference between the green area classified as ExGR (Excess green-Excess red) and the maize area predicted by the model. Each image evaluated for weed density was recombined to quantify and visualize the distribution and density of weeds in a wide range of maize fields. We propose a method to quantify weed density for accurate weeding by effectively separating weeds, maize, and background from UAV images of maize fields.

Development of a Simultaneous Analytical Method for Azocyclotin, Cyhexatin, and Fenbutatin Oxide Detection in Livestock Products using the LC-MS/MS (LC-MS/MS를 이용한 축산물 중 유기주석계 농약 Azocyclotin, Cyhexatin 및 Fenbutatin oxide의 동시시험법 개발)

  • Nam Young Kim;Eun-Ji Park;So-Ra Park;Jung Mi Lee;Yong Hyun Jung;Hae Jung Yoon
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.361-372
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    • 2023
  • Organotin pesticide is used as an acaricide in agriculture and may contaminate livestock products. This study aims to develop a rapid and straightforward analytical method for detecting organotin pesticides, specifically azocyclotin, cyhexatin, and fenbutatin oxide, in various livestock products, including beef, pork, chicken, egg, and milk, using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The extraction process involved the use of 1% acetic acid in a mixture of acetonitrile and ethyl acetate (1:1). This was followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium chloride. The extracts were subsequently purified using octadecyl (C18) and primary secondary amine (PSA), after which the supernatant was evaporated. Organotin pesticide recovery ranged from 75.7 to 115.3%, with a coefficient of variation (CV) below 25.3%. The results meet the criteria range of the Codex guidelines (CODEX CAC/GL 40). The analytical method in this study will be invaluable for the analysis of organotin pesticides in livestock products.

Analytical Method for Determination of Laccaic Acids in Foods with HPLC-PDA and Monitoring (식품 중 락카인산 성분 분리정제를 통한 분석법 확립 및 실태조사)

  • Jae Wook Shin;Hyun Ju Lee;Eunjoo Lim;Jung Bok Kim
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.390-401
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    • 2023
  • Major components of lac coloring include laccaic acids A, B, C, and E. The Korean Food Additive Code regulates the use of lac coloring and prohibits its use in ten types of food products including natural food products. Since no commercial standards are available for laccaic acids A, B, C, and E, a standard for lac pigment itself was used to separate laccaic acids from the lac pigment molecule. A standard for each laccaic acid was then obtained by fractionation. To obtain pure lac pigment for use in food by High performance Liquid Chromatography Photo Diode Array (PDA), a C8 column yielded the best resolution among various tested columns and mobile phases. A qualitative analytical method using High Performance Liquid Chromatography (HPLC) Tandem Mass(LC-MS/MS) was developed. The conditions for fast and precise sample preparation begin with extraction using methanol and 0.3% ammonium phosphate, followed by concentration. The degree of precision observed for the analyses of ham, tomato juice and Red pepper paste was 0.3-13.1% (Relative Standard Deviation (RSD%)), degree of accuracy was 90.3-122.2% with r2=0.999 or above, and recovery rate was 91.6-114.9%. The limit of detection was 0.01-0.15 ㎍/mL, and the limits of quantitation ranged from 0.02 to 0.47 ㎍/mL. Lac pigment was not detected in 117 food products in the 10 food categories for which the use of lac pigment is banned. Multiple laccaic acids were detected in 105 food products in 6 food categories that are allowed to use lac color. Lac pigment concentrations range from 0.08 to 16.67 ㎍/mL.

Optimization and Applicability Verification of Simultaneous Chlorogenic acid and Caffeine Analysis in Health Functional Foods using HPLC-UVD (HPLC-UVD를 이용한 건강기능식품에서 클로로겐산과 카페인 동시분석법 최적화 및 적용성 검증)

  • Hee-Sun Jeong;Se-Yun Lee;Kyu-Heon Kim;Mi-Young Lee;Jung-Ho Choi;Jeong-Sun Ahn;Jae-Myoung Oh;Kwang-Il Kwon;Hye-Young Lee
    • Journal of Food Hygiene and Safety
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    • v.39 no.2
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    • pp.61-71
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    • 2024
  • In this study, we analyzed chlorogenic acid indicator components in preparation for the additional listing of green coffee bean extract in the Health Functional Food Code and optimized caffeine for simultaneous analysis. We extracted chlorogenic acid and caffeine using 30% methanol, phosphoric acid solution, and acetonitrile-containing phosphoric acid and analyzed them at 330 and 280 nm, respectively, using liquid chromatography. Our analysis validation results yielded a correlation coefficient (R2) revealing a significance level of at least 0.999 within the linear quantitative range. The chlorogenic acid and caffeine detection and quantification limits were 0.5 and 0.2 ㎍/mL and 1.4, and 0.4 ㎍/mL, respectively. We confirmed that the precision and accuracy results were suitable using the AOAC validation guidelines. Finally, we developed a simultaneous chlorogenic acid and caffeine analysis approach. In addition, we confirmed that our analysis approach could simultaneously quantify chlorogenic acid and caffeine by examining the applicability of each formulation through prototypes and distribution products. In conclusion, the results of this study demonstrated that the standardized analysis would expectably increase chlorogenic acidcontaining health functional food quality control reliability.

Monitoring and Risk Assessment of Pesticide Residues in Herbal Medicines in Incheon (인천광역시 유통 한약재의 잔류농약 실태 조사 및 위해평가)

  • Min-jeong Kang;Sung-Hee Kwon;Sun-Hoi Kim;Mi-Sook Yeom;Byung-Kyu Park;Hee-jeong Lee;Ji-Hyeung Kim;Kwang-sig Joo;Myung-je Heo;Mun-ju Kwon
    • Journal of Food Hygiene and Safety
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    • v.39 no.2
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    • pp.118-127
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    • 2024
  • This study investigated the levels of 345 pesticide residues in 50 herbal medicines sold in Incheon metropolitan city to determine their safety. Pesticide residues are harmful substances that can cause serious health problems owing to their toxicity and carcinogenicity. The analysis of pesticide residues in the samples was conducted using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, known for its high analysis efficiency, to analyze a wide range of pesticides for which no standards have been set. The analysis was cross-validated with the pretreatment method outlined in the Korea Pharmacopoeia. Among the 50 samples encompassing 24 different herbs, 22 pesticide residues were detected in 24 samples, covering 7 distinct herbs, resulting in a detection rate of 48%. It is noteworthy that, except for two cases, all detected pesticides were those for which no standards were set. However, after conducting a risk evaluation considering the daily dosage of herb, it was determined that the levels of pesticide residues were within safe limits. Pesticides with high frequency within the same category of herbs were detected, indicating the necessity for continuous monitoring and regulation. In addition, comparative analysis using the pretreatment method outlined in the Korean Pharmacopoeia, yielded similar results, suggesting the possibility of analyzing pesticide residues in herbs using the QuEChERS method. The study emphasizes the importance of continuous monitoring of pesticide residues in herbs and the development of high-efficiency reliability analysis methods should continue to ensure consumer safety.