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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.

Determining the Authenticity of Labeled Traceability Information by DNA Identity Test for Hanwoo Meats Distributed in Seoul, Korea (DNA 동일성 검사를 통한 서울지역 유통 한우육의 표시 이력정보 진위 판별)

  • Yeon-jae Bak;Mi-ae Park;Su-min Lee;Hyung-suk Park
    • Journal of Food Hygiene and Safety
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    • v.38 no.1
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    • pp.12-18
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    • 2023
  • Beef traceability systems help prevent the distribution of Hanwoo (Korean native cattle) meat as imported beef. In particular, assigning a traceability number to each cattle can provide all information regarding the purchased Hanwoo meat to the consumers. In the present study, a DNA identity test was conducted on 344 samples of Hanwoo meat from large livestock product stores in Seoul between 2021 and 2022 to determine the authenticity of important label information, such as the traceability number. Traceability number mismatch was confirmed in 45 cases (13.1%). The mismatch rate decreased to 11.3% in 2022 from 14.7% in 2021, and the mismatch rate was higher in the northern region (16.9%) than in the southern region (10.2%). In addition, of the six brands, B and D showed satisfactory traceability system management, whereas E and A showed poor traceability system management, with significant differences (P<0.001). The actual traceability number confirmation rate was only 53.9% among the mismatch samples. However, examination of the authenticity of label information of the samples within the identified range revealed false marking in the order of the traceability number (13.1%), sex (2.9%), slaughterhouse name (2.2%), and grade (1.6%); no false marking of breed (Hanwoo) was noted. To prevent the distribution of erroneously marked livestock products, the authenticity of label information must be determined promptly. Therefore, a legal basis must be established mandating the filling of a daily work sheet, including the traceability number of beef, in partial meat subdivisions. Our findings can be used as reference data to guide the management direction of traceability systems for ensuring transparency in the distribution of livestock products.

Selection and Validation of an Analytical Method for Trifludimoxazin in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Trifludimoxazin의 시험법 선정 및 검증)

  • Sun Young Gu;Su Jung Lee;So eun Lee;Chae Young Park;Jung Mi Lee;Inju Park;Yun Mi Chung;Gui Hyun Jang;Guiim Moon
    • Journal of Food Hygiene and Safety
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    • v.38 no.3
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    • pp.79-88
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    • 2023
  • Trifludimoxazin is a triazinone herbicide that inhibits the synthesis of protoporphyrinogen oxidase (PPO). The lack of PPO damages the cell membranes, leading to plant cell death. An official analytical method for the safety management of trifludimoxazin is necessary because it is a newly registered herbicide in Korea. Therefore, this study aimed to develop a residual analysis method to detect trifludimoxazin in five representative agricultural products. The EN method was established as the final extraction method by comparing the recovery test and matrix effect with those of the QuEChERS method. Various sorbent agents were used to establish the clean-up method, and no differences were observed among them. MgSO4 and PSA were selected as the final clean-up conditions. We used LC-MS/MS considering the selectivity and sensitivity of the target pesticide and analyzed the samples in the MRM mode. The recovery test results using the established analysis method and inter-laboratory validation showed a valid range of 73.5-100.7%, with a relative standard deviation and coefficient of variation less than 12.6% and 14.5%, respectively. Therefore, the presence of trifludimoxazin can be analyzed using a modified QuEChERS method, which is widely available in Korea to ensure the safety of residual insecticides.