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Paralytic shellfish toxins (PSTs) and tetrodotoxin (TTX) of Korean pufferfish

  • Lee, Ka Jeong;Ha, Kwang Soo;Jung, Yeoun Joong;Mok, Jong Soo;Son, Kwang Tae;Lee, Hee Chung;Kim, Ji Hoe
    • Fisheries and Aquatic Sciences
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    • v.24 no.11
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    • pp.360-369
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    • 2021
  • Paralytic shellfish toxins (PSTs) and tetrodotoxin (TTX) are neurotoxins that display pharmacological activity that is similar to that of specific sodium channel blockers; they are the principle toxins involved in shellfish and puffer fish poisoning. In Korea, puffer fish is a very popular seafood, and several cases of accidental poisoning by TTX have been reported. Therefore, it is necessary to determine whether puffer fish poisoning incidents are caused by PSTs or by TTX. In this study, we used mouse bioassay (MBA) and liquid chromatograph-tandem mass spectrometry (LC-MS/MS) to determine the presence of PSTs and TTX in puffer fish from an area near Mireuk-do, Tong-Yeong on the southern coast of Korea from January through March, 2014. The toxicity of PSTs and TTX extracts prepared from three organs of each specimen was analyzed by MBA. Most of the extracts killed mice with typical signs of TTX and PSTs. The LC-MS/MS analysis of seven specimens of Takifugu pardalis and Takifugu niphobles, each divided into muscles, intestines, and liver, were examined for TTX. In T. pardalis, the TTX levels were within the range of 1.3-1.6 ㎍/g in the muscles, 18.8-49.8 ㎍/g in the intestines, and 23.3-96.8 ㎍/g in the liver. In T. niphobles, the TTX levels were within the range of 2.0-4.5 ㎍/g in the muscles, 23.9-71.5 ㎍/g in the intestines, and 28.1-114.8 ㎍/g in the liver. Additionally, the toxicity profile of the detected PSTs revealed that dcGTX3 was the major component in T. pardalis and T. niphobles. When PSTs were calculated as saxitoxin equivalents the levels were all less than 0.5 ㎍/g, which is below the permitted maximum standard of 0.8 ㎍/g. These findings indicate that the toxicity of T. pardalis and T. niphobles from the southern coast of Korea is due mainly to TTX and that PSTs do not exert an effect.

Fermentation Efficiency and Effect on Morphological Change of Nitrogen and Phosphorous with the Litter Types of Cowshed (우사의 깔짚 종류에 따른 발효 효율과 질소와 인의 형태 변화에 미치는 영향)

  • Ryoo, Keon Sang
    • Journal of the Korean Chemical Society
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    • v.66 no.2
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    • pp.86-91
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    • 2022
  • The manure made of chaff and sawdust as litter was collected separately at a cowshed of a livestock farm in Andondg city. The fermentation efficiency of excreta is greatly influenced by the type and characteristics of litter and a factor to be considered for reducing N and P, the causes of eutrophication. Changes in weight with temperature and constituents of sample were examined using TG-DTA and XRF, respectively. NO2-, NO3-, and PO43- ions and NH4+, T-P and T-N eluted from manure by rain were analyzed using ion chromatograph and UV/Vis spectrometry, respectively. As a result, the fermentation efficiency of excreta in sawdust manure is three times higher as compared with chaff manure. The higher the fermentation efficiency, ammonia nitrogen was highly de-nitrogenated and organic phosphorous were also changed into phosphorous ions. Furthermore, phosphorous ions can be removed by transforming insoluble salts such as calcium phosphate (CaHPO4·3H2O) and struvite (NH4MgPO4·6H2O) with addition of Ca and Mg.

Comparison of sample storage containers for the analysis of volatile organic compounds (VOC) (휘발성유기물(VOC) 분석을 위한 시료보관 용기의 비교)

  • Kim, Seokyung;Kim, Dalho
    • Analytical Science and Technology
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    • v.35 no.3
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    • pp.116-123
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    • 2022
  • Polymer bags, metallic canisters, and glass bottles have been used as containers for analyzing the volatile organic compounds (VOCs) in air. In this study, various sampling containers were compared to investigate the short-term stability of VOCs, that is, from the time they are sampled to the time they are analyzed. Polyvinyl fluoride (PVF), polypropylene (PP), polyester aluminum (PE-Al) bags, canisters, and glass bottles were used as sample containers. A 100 nmol/mol standard gas mixture of benzene, toluene, ethylbenzene, m-xylene, styrene, and o-xylene was used for the VOC comparison. Changes in the concentrations of samples stored for 10~20 day in each container were measured using a thermal desorption-gas chromatograph-flame ionization detector (TD-GC-FID). As a result, VOCs stored in a canister and two kinds of amber glass bottles have shown immaterial decreases in concentration in one week, and more than 80 % of the initial concentration was maintained for two weeks. In the case of polymer bags, the concentration of all VOCs, except benzene and toluene, were remarkably decreased below 70% of the initial concentration in one day. Particularly, ethylbenzene, xylene, and styrene have shown dramatic decreases in concentration below 30 % of the initial concentration in all polymer bags in one day.

Study on the Morphological Change and Reduction Plan of Nitrogen and Phosphorous in Litter and Manure of Cow House (우사의 깔짚과 퇴비에 있는 질소와 인의 형태적 변화와 저감 방안에 관한 연구)

  • Kim, Younjung;Ryoo, Keon Sang
    • Journal of the Korean Chemical Society
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    • v.65 no.4
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    • pp.249-253
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    • 2021
  • Litter and manure were obtained at a cow house of a livestock farm in Andondg city. We examined the change of formation of nitrogen and phosphorous from these samples and tried to suggest a more useful and realistic way for removing them. Constituent and its content of sample were identified by XRF. NO2-, NO3-, and PO43- ions and NH4+, T-P and T-N released from sample were analyzed using ion chromatograph and UV/Vis spectrometry, respectively. As the results of this study, the ammonia nitrogen in the early stage of cow excretion is a need to make an ammonia gas state that can be immediately volatile by increasing the pH. Nitrogen and phosphorous, the main source of nutrition in green algal bloom can be removed by transforming insoluble salts such as calcium phosphate (CaHPO4·3H2O) and struvite (NH4MgPO4·6H2O), respectively, with addition of Ca and Mg after stimulating fermentation of manure.

Bioassay of Allelopathy Substance Related Injury by Successive Cropping in Alfalfa(Medicago sativa L.) (알팔파 연작장해에 관여하는 타감작용 물질의 탐색 및 생물검정)

  • Jeon, In-Soo;Kim, Myung-Cho;Hur, Jang-Hyun;Yu, Chang-Yeon;Cho, Dong-Ha;Kim, E-Hun
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.42 no.2
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    • pp.228-235
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    • 1997
  • This experiments were conducted to determine the effect of allelopathy and autotoxicity in alfalfa. Among several alfalfa cultivars, the substances exudated from seven cultivars including Medicago sativa, c.v. Luna, Sparta, Magnum, Husky, Milkmaker, Challenger and Anchor inhibited the germination and seedling growth of radish, ranging from 60 to 80%. When allelopathic substances were exudated from the soil of the alfalfa-cultivated field, the increased levels of substance retarded the germination rate and seedling growth of radish and alfalfa. The inhibition rate was about 80%, compared with that of control. Thus, this study indicates that the allelopathy and autotoxicity substances of alfalfa influenced the germination and seedling growth in alfalfa itself and radish. When allelopathic substances were analysed by using gas chromatograph, several kinds of phenol compounds were detected as follows; Salicylic acid, hydroxybenzoic acid, vanillic acid, syringic acid, coumaric acid, and ferulic acid.

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Analysis of polycyclic aromatic hydrocarbons in cooked fish and shellfish (조리어패류 중 다환방향족탄화수소 분석)

  • Hu, Soojung;Park, Sungkuk;Jin, Sunhee;Choi, Dongmi
    • Analytical Science and Technology
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    • v.22 no.1
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    • pp.109-117
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    • 2009
  • The following concentrations of some PAHs were investigated; [benzo(a)anthracene, chrysene, benzo (b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g, h, i)perylene, indeno (1,2,3-c,d)pyrene] in fish(n=168) and shellfish(n=40). The methodology involved saponification and extraction with n-hexane, clean-up on Sep-Pak Florisil Cartridges and determination by HPLC/FLD (High Performance Liquid Chromatograph/Fluorescence Detector). Overall method recoveries for 8 PAHs spiked into these products ranged from 88 to 112%. The mean level of benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k) fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene and indeno(1,2,3-c,d)pyrene in cooked fish was ND, ND, 0.0009, ND, 0.01, ND, ND, ND and in cooked shellfish was 1.84, 3.51, 0.81, 0.38, 0.39, 0.04, 0.20, ND, respectively.

Current status of brominated flame retardants (BFR) and polybrominated dibenzo-p-dioxins and furans (PBDDs/PBDFs) (브롬화난연제 및 브롬화다이옥신류의 연구동향)

  • Kwon, Myung-Hee;Song, Ki-Bong;Kang, Yung-Ryul;Hwang, Seung-Ryu;Shin, Sun Kyoung;Kim, Kum-Hee;Park, Jin Soo;Kim, Sue-Jin;Lee, Su-Yung;Kim, Dong-Hoon;Jung, Kwang-Yong
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.443-458
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    • 2008
  • Brominated flame retardants (BFRs) are chemical compounds that inhibit the combustion of organic materials by scavenging free radicals that would otherwise encourage the spread of flames. These compounds are found in a wide variety of materials including paints, plastics, textiles, furniture and electronics. Mounting evidence, however, suggests that the non-reactive BFRs can easily leach into the environment and pose significant environmental and health concerns. PBDDs/PBDFs are often formed in the process of manufacturing brominated flame retardants and from the combustion of waste products containing flame retardants BFR. Therefore, this paper describes the general characteristics, management status, residual concentration in environments and analytical method.

Analysis of Petrological Characteristics and Lacquer Gilding Materials of the Stone Buddha Head Excavated from the Temple Site No.4 of Yaksugok-Valley in Namsan Mountain, Gyeongju (경주 남산 약수곡 제4사지 출토 석재 불두의 암석학적 특징과 옻칠 도금 재료 분석)

  • Yu Jia;Lee Myeongseong;Lee Eunwoo
    • Conservation Science in Museum
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    • v.30
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    • pp.47-70
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    • 2023
  • In 2019, the first excavation survey was conducted at the Temple Site No. 4 of Yaksugok Vally in Namsan Mountain, Gyeongju to determine the original location of the headless stone Buddha statue and the structure of the temple site. The survey excavated a stone Buddha head that was confirmed in a comparative analysis to be petrologically and mineralogically identical to a headless stone seated Buddha statue found derelict nearby. Traces of gold leaf and black adhesive were found on a portion of the right side of the face of the Buddha head buried in the ground. Since it is exceedingly rare for lacquer and gilding techniques to have been applied to a large stone Buddha statue without a base layer, this study examines the gilding techniques of the time by analyzing the characteristics of the materials used. In this process, the structure of the gold foil was observed through analytical microscopy and scanning electron microscopy with energy dispersive X-ray spectrometry, and the gold (Au) component was identified. As a result of analyzing the black adhesive using pyrolysis-gas chromatograph/mass spectrometry (pyrolysis-GC/MS), pyrolysis compounds such as hydrocarbons, fatty acids, catechol, and catechol oxidation products were detected. This was identical to the characteristics identified upon analyzing lacquer collected from species of lacquer tree whose main component is urushiol. Therefore, it was confirmed that the stone Buddha head excavated from the Temple Site No. 4 of Yaksugok Valley was separated from a nearby stone seated Buddha statue, and that the gold foil was attached using lacquer sap collected from lacquer trees, which grow in Korea, China, and Japan.

Development and Validation of Analytical Method for Determination of Fungicide Spiroxamine Residue in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Spiroxamine의 시험법 개발 및 검증)

  • Park, Shin-Min;Do, Jung-Ah;Lim, Seung-Hee;Yoon, Ji-Hye;Pak, Won-Min;Shin, Hye-Sun;Kuk, Ju-Hee;Chung, Hyung-Wook
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.296-305
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    • 2018
  • Spiroxamine, one of fungicides, is used to control powdery mildew in various crops and black yellow sigatoka in bananas. The major strength of spiroxamine is to control powdery mildew in various crops and bananas yellow sigatoka in bananas. The compound has shown a high level of activity, good persistence and crop tolerance. Besides powdery mildew, good control of rust, net blotch and Rhynchosporium diseases been indicated in cereals, together with a complementary activity against Septoria diseases. In 2017, the maximum residue limit (MRL) of spiroxamine established in Korea. According to Ministry of ood and rug afety) regulations, spiroxamine residues defined only parent compound. Thus, a analytical method is needed to estimate the residue level of the parent compound. The objective of this study was to develop and validate analytical method for spiroxamine in representative agricultural commodities. Samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interfering substances. The analyte were quantified and confirmed 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 ($0.0005{\sim}0.1{\mu}g/mL$) for the analyte in blank extract with coefficient of determination ($r^2$) > 0.99. For validation purposes, recovery studies will be carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries 70.6~104.6% with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges in the Codex guidelines (CAC/GL40, 2003) and MFDS guidelines. proposed analytical method be used as an official analytical method in the Republic of Korea.

Analysis of Physicochemical Characterization and Volatiles in Pure or Refined Olive Oils (국내 유통되는 퓨어 및 정제 올리브유의 이화학적 특성 및 향기 분석)

  • Nam, Ha-Young;Lee, Ju-Woon;Hong, Jang-Hwan;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.36 no.11
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    • pp.1409-1416
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    • 2007
  • Seven selected commercial pure or refined olive oils were obtained from the market, and their physicochemical properties and volatile characterizations were investigated. Fatty acid profiles of the analyzed olive oils showed oleic $(61.2{\sim}74.7mole%)$, palmitic $(10.2{\sim}16.8mole%)$, linoleic $(9.4{\sim}18.0mole%)$, stearic $(1.9{\sim}3.0mole%)$, palmitoleic $(0.7{\sim}2.4mole%)$ and linolenic acid $(0.5{\sim}0.9mole%)$. According to Hunter#s color measurement, pure or refined olive oils showed $L^*$ value of $92.2{\sim}99.0$, $a^*$ value of $-22.2{\sim}-3.2$, and $b^*$ value of $18.5{\sim}55.0$. Their total phenol contents ranged from 1.9 to $13.3mg/100g$ while ${\alpha}-tocopherol$ content showed $7.91{\sim}13.88mg/100g$. Oxidation stability of the pure or refined olive oils were observed by Rancimat. The induction period ranged from 17.37 to 34.72 hr while their POV were $6.83{\sim}20.31meq/kg$ oil. Electronic nose and gas chromatograph-mass spectrometry with head-space solid phase microextraction were applied to identify and discriminate the volatile compounds and flavors in pure or refined olive oils, respectively.