• Title/Summary/Keyword: r-phase

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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.

Comparative Study on the Composition of Floral Volatile Components in the Flowering Stages of Robinia pseudoacacia L. (아까시나무(Robinia pseudoacacia L.) 꽃의 개화 단계별 향기성분 조성 비교)

  • Jung, Je Won;Lee, Hyun Sook;Noh, Gwang Rae;Lee, Andosung;Kim, Moon Sup;Kim, Sea Hyun;Kwon, Hyung Wook
    • Journal of Apiculture
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    • v.32 no.3
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    • pp.139-146
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    • 2017
  • Floral scent emitted from many plants is the critical factors for pollinator attraction and defense for adaptation in environments. The fragrance components of flowers are different in composition by geographical origins, climate factors and the development stages of flowers. In the present study, we investigated the volatile-floral compounds in flowers of Robinia pseudoacacia L. and defined the chemical contribution for flowering periods. The volatile compounds analysis was performed by gas chromatography with mass selective detector after solid phase microextraction (SPME). We reported different compositional features of fragrance compounds according to flowering periods. The abundant compounds identified in stage 1 were ${\alpha}$-pinene (66.80%) and ${\beta}$-pinene (26.53%). Those of the stage 2 were (Z)-${\beta}$-ocimene (37.57%), ${\alpha}$-pinene (15.16%), benzaldehyde (16.63%), linalool (12.13%). The volatiles of stage 3 comprised an abundance of (Z)-${\beta}$-ocimene (64.94%), ${\alpha}$-pinene (9.84%), linalool (8.92%), benzaldehyde (1.71%). Leaf volatiles were distinct from those in the reproductive plant parts by their high relative amount of (E)-${\beta}$-ocimene (23.50%) and (Z)-3-Hexenyl acetate (27.87%). Differences in flower scents of the different stages and leaves are discussed in light of biochemical constraints on volatile chemical synthesis and of the role of flower scent in evolutionary ecology of R. pseudoacacia.

Development of a Simultaneous Analytical Method for Determination of Insecticide Broflanilide and Its Metabolite Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살충제 Broflanilide 및 대사물질 동시시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Kim, Ji-Young;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.124-134
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    • 2019
  • An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl ($C_{18}$). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.