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Development of Analytical Method for Kasugamycin in Agricultural Products using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Kasugamycin 시험법 개발)

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

Chemical compositions of different cultivars of astringent persimmon (Diospyros kaki Thunb.) and the effects of maturity (떫은감(Diospyros kaki Thunb.) 품종 및 수확시기에 따른 영양 성분 변화)

  • Yoo, Seul Ki;Kim, Jong Min;Park, Seon Kyeong;Kang, Jin Yong;Han, Hye Ju;Park, Hyo Won;Kim, Chul-Woo;Lee, Uk;Heo, Ho Jin
    • Korean Journal of Food Science and Technology
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    • v.51 no.3
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    • pp.248-257
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    • 2019
  • This study aimed to determine the chemical components of different cultivars (Gabjubaekmok, Sangjudungsi, and Godongsi) of persimmon (Diospyros kaki Thunb.) and the effects of maturity. The detected free sugars were fructose and glucose, and glucose levels tended to increase with maturity. Palmitic acid, oleic acid, linoleic acid and stearic acid, and potassium were major components. In the amino acid component analysis, the following were usually present in the following month: glutamic acid in Gabjubaekmok in July, lysine in Sangjudungsi in August, and threonine in Godongsi in October. Vitamin C tended to increase with aging, and fruit harvested in July had the highest total phenolic and flavonoid contents. In the metabolite analysis, there were significant differences among cultivars and with maturity. The major physiological compounds were analyzed using ultra performance liquid chromatography quadrupole time-of-flight tandem mass ($UPLC/Q-TOF/MS^2$) and were citric acid and gallic aicd. As maturity progressed, citric acid increased but gallic acid decreased.

Antioxidant and Anti-inflammatory Activities of Water and the Fermentation Liquid of Sea Tangle (Saccharina japonica) (다시마 물 추출액과 발효액의 항산화 및 항염증 활성)

  • Jung, Kyung Im;Kim, Bo Kyung;Kang, Jeong Hyeon;Oh, Geun Hye;Kim, In Kyung;Kim, Mihyang
    • Journal of Life Science
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    • v.29 no.5
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    • pp.596-606
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    • 2019
  • The study investigated the physiochemical properties and the antioxidant and anti-inflammatory activities of the sea tangle (Saccharina japonica) in a water extract before (STWE) and after (STFL) fermentation with Lactobacillus brevis. The pH values of STWE and STFL were 6.18 and 4.16, and the sugar contents were $8.50^{\circ}Brix$ and $7.40^{\circ}Brix$, respectively. The main free amino acids of STWE and STFL were glutamic acid, aspartic acid, and alanine, and the ${\gamma}$-amino butyric acid (GABA) content was increased by fermentation. The total polyphenol contents of STWE and STFL were 498.29 and 615.77 mg gallic acid equivalent (GAE)/ml, respectively. The 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activities of STWE and STFL were markedly increased in a dose-dependent manner, and revealed about 89.89% and 96.94% activities, respectively, at 10% concentration (p<0.05). The superoxide dismutase (SOD) activities of STWE and STFL were also markedly increased in a dose-dependent manner, and the activity of STFL was significantly increased when compared with STWE (p<0.05). The anti-inflammatory activity was examined in lipopolysaccharide (LPS)-stimulated RAW 264.7 cells. STWE and STFL decreased the production of reactive oxygen species (ROS), which had levels of about 189.90% and 174.69% at 1% concentration, respectively (p<0.05). The contents of pro-inflammatory cytokines, such as tumor necrosis factor-alpha ($TNF-{\alpha}$) and interleukin-6 (IL-6), were decreased more by addition of STFL than by addition of STWE. The STWE and STFL showed high antioxidant and anti-inflammatory activity, and these activities were increased by fermentation. Therefore, sea tangle extracts can be used as functional food materials.

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.

Optimization of Analytical Method for Annatto Pigment in Foods (식품 중 안나토색소 분석법 최적화 연구)

  • Lee, Jiyeon;Park, Juhee;Lee, Jihyun;Suh, Hee-Jae;Lee, Chan
    • Journal of Food Hygiene and Safety
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    • v.36 no.4
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    • pp.298-309
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    • 2021
  • In this study we sought to develop a simultaneous analysis method for cis-bixin and cis-norbixin, the main components, to detect annatto pigment in food. To establish the optimal test method, the HPLC analysis methods of the European Food Safety Authority (EFSA), Japan's Ministry of Health, Labor and Welfare (MHLW), and National Institute of Food and Drug Safety Evaluation (NIFDS) were compared and reviewed. In addition, a new pretreatment method applicable to various foods was developed after selecting conditions for simultaneous high-performance liquid chromatography (HPLC) analysis in consideration of linearity, limit of detection (LOD), limit of quantification (LOQ), and analysis time. The HPLC analysis method of NIFDS showed the best linearity (R2 ≥ 0.999), exhibiting low detection and quantification limits for cis-norbixin and cis-bixin as 0.03, 0.05 ㎍/mL, and 0.097, 0.16 ㎍/mL, respectively. All previously reported pretreatment methods had limitations in various food applications. However, the new pretreatment method showed a high recovery rate for all three main food groups of fish meat and meat products, processed cheese and beverages. This method showed an excellent simultaneous recovery rate of 98% or more for cis-bixin and cis-norbixin. The HPLC analysis method with a new pretreatment method showed high linearity with a coefficient of determination (R2) of 1 for both substances, and the accuracy (recovery rate) and precision (%RSD) were 98% and between 0.4-7.9, respectively. From this result, the optimized analytical method was considered to be very suitable for the simultaneous analysis of cis-bixin and cis-norbixin, two main components of annatto pigment in food.

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.

Effects of Hydrothermal Pretreatment on the Nutritional Values and In Vitro Fermentation Characteristics of Tall Fescue (Festuca arundinacea) and Corn Silage (열수 전처리에 따른 톨페스큐와 옥수수 사일리지의 영양적 가치와 in vitro 발효특성에 미치는 영향)

  • Kim, Dong Hyeon;Son, Jun Kyu;Lee, Ji Hwan;Kim, Sang Bum;Park, Beom Young;Kim, Doo San;Jang, Gul Won;Lim, Hyun Joo;Hur, Tai Young;Kim, Eun Tae
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.22 no.1
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    • pp.468-476
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    • 2021
  • This study examined the effects of a hydrothermal pretreatment (HP) on the nutritional values and in vitro fermentation characteristics of tall fescue and corn silage. This study was conducted through a factorial design of 2 (control or HP) × 2 (hay; tall fescue or silage; corn). For the HP, forage was placed into a glass bottle with 20% w/v of water, and the glass bottle was sealed and heated to reach a temperature of 121℃ (0.12 MPa). The solid residue and liquid were collected and oven-dried at 65℃ for three days. The dried materials were tested for in vitro fermentation at 39℃ for 24 and 48 h. The content of ADF increased significantly regardless of the forage type. After in vitro incubation for 24 h, the total VFA content was significantly lower after HP, regardless of the forage type (p ≤ 0.05), and the propionate concentration was increased in corn silage with HP (p ≤ 0.05). After 48 hours of in vitro incubation, the propionate content increased significantly (p ≤ 0.03) in corn silage with HP (p ≤ 0.05), but the butyrate content decreased significantly (p ≤ 0.05). There was no change in the in vitro dry matter and neutral detergent fiber digestibility by HP regardless of the forage type. Therefore, the use of hydrothermally pretreated corn silage could be advantageous for the supply of energy for ruminants.

A History of Termite Control and Improvements to Prevent Termites in Wooden Architectural Heritage (국내외 흰개미 방제 기술의 발달 과정과 목조건축문화재의 흰개미 피해 저감을 위한 방안)

  • LEE, Sangbin;IM, Ikgyun;KIM, Sihyun
    • Korean Journal of Heritage: History & Science
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    • v.54 no.2
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    • pp.194-215
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    • 2021
  • Termites are important decomposers in the ecosystem. They are also economically significant structural pests. In this study, we reviewed the developments of termite control and recent research on termite management to provide information on the prevention and control of termites. In Korea, most of the damage to wooden historical buildings is caused by subterranean termites. Reticulitermes speratus kyushuensis is the main species, which is widely found throughout the country. In the early 1900s, inorganic insecticides, such as arsenic dust, were used for termite control. After the synthesis of chlorinated hydrocarbon pesticide in the 1940s, it was widely utilized and demonstrated high termite control efficacy. However, chlorinated hydrocarbon insecticides were later banned, disappearing from markets after reports emerged concerning environmental contamination and toxicity to humans. Therefore, the termite control industry sought a new termiticide; hence many pesticides were utilized for termite control. Organophosphate (1960s), carbamate (1970s), pyrethroid, and insect growth inhibitor (1980s) were newly synthesized and adopted. In the 1990s, the first commercial baits using chitin synthesis inhibitors (CSI) were developed, providing a means to eliminate an entire colony of subterranean termites around a structure. Many studies have been carried out on soil termiticides (liquid termiticides) and CSI baits to increase their efficacy, and different baits such as aboveground bait stations, fluid bait, and high-durability bait were also developed in the 2000s. In addition, the paradigm of termite control has shifted from localized treatments using soil termiticides to area-wide pest management using CSI baits to create termite-free zones and protect buildings over time. Termite infestations in wooden historical buildings in Korea have been reported since 1980, and considerable attention was drawn in the 1990s when several UNESCO world heritages such as the Jongmyo Shrine and the Janggyeong Panjeon Depositories of Haeinsa Temple were infested by subterranean termites. Since then, a survey of termite infestation in wooden architectural heritage has been conducted, and the National Research Institute of Cultural Heritage and Heritage Care Program regularly monitors those properties. Finally, we suggest termite management using primarily CSI baits, selective application of various soil treatments applied to the object, foundation soil treatment, research and development of durable termite baits, application of area-wide programs for wooden-building complexes, application of integrated termite management (ITM), and regular education for owners and managers to prevent and reduce termite damage.

Implementation of Capacitor and Inductor Applied LCP Substrate for 35-GHz frequency band (35 GHz 대역을 위한 LCP 기판 적용된 커패시터 및 인덕터 구현)

  • Lee, Jiyeon;Ryu, Jongin;Choi, Sehwan;Lee, Jaeyoung
    • Journal of the Microelectronics and Packaging Society
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    • v.27 no.4
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    • pp.67-75
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    • 2020
  • In this paper, by applying LCP substrate, the capacitor and inductor are implemented with a variety of value that can be used in 35 GHz circuits. Depending on how to apply it to the circuit, it is required high value by designing the basic structures such as electrode capacitor and spiral inductor. However they are not available in high-frequency domain, because their SRF(Self-Resonant Frequency) is lower than the frequency of 35-GHz. By finding the limit, this paper devised classifying passive devices for the DC and the high-frequency domain. The basic structure is suitable for DC and microstrip λ/8 length stub structure can be used for high-frequency. The open and short stub structure operate as a capacitor and inductor respectively in the frequency of 35 GHz. If their impedance is known, it is possible to extract the value through the impedance-related equation. By producing with the permittivity 2.9 LCP substrate, the basic structure which are available in the DC constituted a library of capacitance of 1.12 to 13.9 pF and inductance of 0.96 to 4.69 nH, measured respectively. The stub structure available in the high-frequency domain were built libraries of capacitance of 0.07 to 2.88 pF and inductance of 0.34 to 1.27 nH, calculated respectively. The measurements have proven how to diversify value, so libraries can be built more variously. It is possible to integrate with the operation circuit of TRM(Transmit-Receive Module) for the frequency 35-GHz, it will be an alternative to the passive devices that can be properly utilized in the circuit.

Improvement of an Analytical Method for Fluoroimide Residue in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Fluoroimide의 잔류농약 분석법 개선)

  • Kim, Nam Young;Park, Eun-Ji;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.220-227
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    • 2021
  • Fluoroimide is a fungicide and is also used as a pesticide for persimmons and potatoes. The established fluoroimide pesticide analysis method takes a long time to perform and uses benzene, a carcinogen. In addition, a lower limit of quantification is required due to enforcement of the Positive List System. Therefore, this study aimed to improve the analysis method for residual fluoroimide to resolve the problems associated with the current method. The analytical method was improved with reference to the increased stability of fluoroimide under acidic conditions. Fluoroimide was extracted under acidic conditions by hydrogen chloride (4 N) and acetic acid. MgSO4 and NaCl were used with acetonitrile. C18 (octadecylsilane) 500 mg and graphitized carbon black 40 mg were used in the purification process. The experiment was conducted with agricultural products (hulled rice, potato, soybean, mandarin, green pepper), and liquid chromatograph-tandem mass spectrometry was used for the instrumental analysis. Recovery of fluoroimide was 85.7-106.9% with relative standard deviations (RSDs) of less than 15.6%. This study reports an improved method for the analysis of fluoroimide that might contribute to safety by substituting the use of benzene, a harmful solvent. Furthermore, the use of QuEChERS increased the efficiency of the improved method. Finally, this research confirmed the precise limit of quantification and these results could be used to improve the analysis of other residual pesticides in agricultural products.