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Development of Analytical Method for Detection of Fungicide Validamycin A Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Validamycin A의 시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.22-29
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    • 2019
  • Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.

Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 Oxytetracycline의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, ong-hyun;Lee, Kangbong
    • 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.

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.

Musical Analysis of Jindo Dasiraegi music for the Scene of Performing Arts Contents (연희현장에서의 올바른 활용을 위한 진도다시래기 음악분석)

  • Han, Seung Seok;Nam, Cho Long
    • (The) Research of the performance art and culture
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    • no.25
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    • pp.253-289
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    • 2012
  • Dasiraegi is a traditional funeral rite performance of Jindo located in the South Jeolla Province of South Korea. With its unique stylistic structure including various dances, songs and witty dialogues, and a storyline depicting the birth of a new life in the wake of death, embodying the Buddhism belief that life and death is interconnected; it attracted great interest from performance organizers and performers who were desperately seeking new contents that can be put on stage as a performance. It is needless to say previous research on Dasiraegi had been most valuable in its recreation as it analyzed the performance from a wide range of perspectives. Despite its contributions, the previous researches were mainly academic focusing on: the symbolic meanings of the performance, basic introduction to the components of the performance such as script, lyrics, witty dialogue, appearance (costume and make-up), stage properties, rhythm, dance and etc., lacking accurate representation of the most crucial element of the performance which is sori (song). For this reason, the study analyzes the music of Dasiraegi and presents its musical characteristics along with its scores to provide practical support for performers who are active in the field. Out of all the numbers in Dasiraegi, this study analyzed all of Geosa-nori and Sadang-nori, the funeral dirge (mourning chant) sung as the performers come on stage and Gasangjae-nori, because among the five proceedings of the funeral rite they were the most commonly performed. There are a plethora of performance recordings to choose from, however, this study chose Jindo Dasiraegi, an album released by E&E Media. The album offers high quality recordings of performances, but more importantly, it is easy to obtain and utilize for performers who want to learn the Dasiraegi based on the script provided in this study. The musical analysis discovered a number of interesting findings. Firstly, most of the songs in Dasiraegi use a typical Yukjabaegi-tori which applies the Mi scale frequently containing cut-off (breaking) sounds. Although, Southern Kyoung-tori which applies the Sol scale was used, it was only in limited parts and was musically incomplete. Secondly, there was no musical affinity between Ssitgim-gut and Dasiraegi albeit both are for funeral rites. The fundamental difference in character and function of Ssitgim-gut and Dasiraegi may be the reason behind this lack of affinity, as Ssitgim-gut is sung to guide the deceased to heaven by comforting him/her, whereas, Dasiaregi is sung to reinvigorate the lives of the living. Lastly, traces of musical grammar found in Pansori are present in the earlier part of Dasiraegi. This may be attributed to the master artist (Designee of Important Intangible Cultural Heritage), who was instrumental in the restoration and hand-down of Dasiaregi, and his experience in a Changgeuk company. The performer's experience with Changgeuk may have induced the alterations in Dasiraegi, causing it to deviate from its original form. On the other hand, it expanded the performative bais by enhancing the performance aspect of Dasiraegi allowing it to be utilized as contents for Performing Arts. It would be meaningful to see this study utilized to benefit future performance artists, taking Dasiraegi as their inspiration, which overcomes the loss of death and invigorates the vibrancy of life.