• Title/Summary/Keyword: Instrumental Analysis Method

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Development of Analytical Method for Ergot Alkaloids in Foods Using Liquid Chromatoraphy-Tandem Mass Spectrometry (LC-MS/MS를 이용한 식품 중 맥각 알칼로이드 시험법 개발)

  • Chun, So Young;Chong, Euna;Lee, Bomnae;Kwon, Jin-Wook;Park, Hye Young;Kim, Sheenhee;Gang, Giljin
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.158-169
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    • 2019
  • Ergot alkaloids are mycotoxin produced by fungi of the Claviceps genus, mainly by Claviceps purpurea in EU. Recently obtained informations indicates necessity for control the ergot in imported grains. Recent occurrence data of ergot alkaloids from EU countries indicate the necessities of management and control these toxins from the imported grains like rye, wheat, oat etc. The aim of this study is to optimize the liquid chromatography-tandem mass spectrometry method for determination of ergot alkaloids (ergometrine, ergosine, ergotamine, ergocornine, ergocryptine, ergocristine and their epimers (-inines) from grain and grain-based food. The test method was optimized by extracting the sample with acetonitrile containing 2 mM ammonium carbonate, purification with Mycosep cartridge, and instrumental analysis by LC-MS/MS using Syncronis C18 column. The standard calibration curves showed linearity with correlation coefficents; $R^2$ >0.99. Mean recoveries ranged from 72.0 to 111.3% at three different fortified levels (20, 50, and $100{\mu}g/kg$). The correlation coefficient expressed as precision was within the range of 1.9-12.9%. The limit or quantifications (LOQ) ranged from 0.012 to $0.058{\mu}g/kg$. The developed analytical method met the criteria of AOAC Int. and CAC validation parameters like accuracy and sensitivity. As a result, it was confirmed that the test method developed in this study is suitable for the simultaneous analysis of six species of ergot alkaloid from grains and grain products.

A Study on Corrosion Properties of Reinforced Concrete Structures in Subsurface Environment (지중 환경하에서의 철근콘크리트 구조물의 부식 특성 연구)

  • Kwon, Ki-jung;Jung, Haeryong;Park, Joo-Wan
    • The Journal of Engineering Geology
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    • v.26 no.1
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    • pp.79-85
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    • 2016
  • A concrete silo plays an important role in subsurface low- and intermediate-level waste facilities (LILW) by limiting the release of radionuclides from the silo geosphere. However, due to several physical and chemical processes the performance of the concrete structure decreases over time and consequently the concrete loses its effectiveness as a barrier against groundwater inflow and the release of radionuclides. Although a number of processes are responsible for degradation of the silo concrete, it is determined that the main cause is corrosion of the reinforcing steel. Therefore, the time it takes for the silo concrete to fail is calculated based on two factors: the initiation time of corrosion, defined as the time it takes for chloride ions to penetrate through the concrete cover, and the propagation time of corrosion. This paper aims to estimate the time taken for concrete to fail in a LILW disposal facility. Based on the United States Department of Energy (DOE) approach, which indicates that concrete fails completely once 50% of the volume of the reinforcing steel corrodes, the corrosion propagation time is calculated to be 640 years, which is the time it takes for corrosion to penetrate 0.640 cm into the reinforcing steel. In addition to the corrosion propagation time, a diffusion equation is used to calculate the initiation time of corrosion, yielding a time of 1284 years, which post-dates the closure time of the LILW disposal facility if we also consider the 640 years of corrosion propagation. The electrochemical conditions of the passive rebar surface were modified using an acceleration method. This is a useful approach because it can reduce the test time significantly by accelerating the transport of chlorides. Using instrumental analysis, the physicochemical properties of corrosion products were determined, thereby confirming that corrosion occurred, although we did not observe significant cracks in, or expansion of, the concrete. These results are consistent with those of Smartet al., 2006 who reported that corrosion products are easily compressed, meaning that cracks cannot be discerned by eye. Therefore, it is worth noting that rebar corrosion does not strongly influence the hydraulic conductivity of the concrete.

Antioxidant Effects of Crotalaria sessiliflora L. Leaf Extracts Fractionated from Each Solvent (활나물 잎 추출물의 분획별 항산화 활성)

  • Kim, Tae-Su;Ko, Sang-Beom;Park, Chun-Geon;Seong, Ha-Jeong;Kang, Myung-Hwa
    • Journal of the East Asian Society of Dietary Life
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    • v.19 no.2
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    • pp.180-186
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    • 2009
  • In this study, Crotalaria sessiliflora L., leaf was extracted with a solvent mixture of $CH_2Cl_2$ and $CH_2OH$ (3:1). In order to draw or separate effective components from the leaf extract with high activity, a 1:1 solvent mixture of water and butanol was used after removal of the sugar and fat from the extract. From the decompressed and concentrated butanol layer, 10 small fractions (Fr1, Fr2, Fr3, Fr4, Fr5, Fr6, Fr7, Fr8, Fr9, and Fr10) were obtained using a chromatography column filled with sephadex LH-20. The activity of each fraction was measured by the same method as that used to measure the antioxidant effect of each part(p<0.05). The Fr1, Fr4, and Fr6 fractions showed the highest activity levels(p<0.05). The vital unknown material that vitality exists in the strong butanol fractions of F1, F4 and F6 will be isolated and identified. Currently, we are performing for a single compound from an unknown peak by instrumental analysis.

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The Relationship among the Indicator PCBs in Breast Milk and Dietary Habits and Demographic Factors in Women Living in Urban Areas (대도시에 거주하는 여성의 모유 중 Indicator PCBs와 식이습성 및 인구통계학적 인자간의 관계)

  • We, Sung-Ug;Kim, Ki-Ho;Cho, Bong-Hui;Cho, Yu-Jin;Yoon, Cho-Hee;Min, Byung-Yoon
    • Journal of Environmental Health Sciences
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    • v.36 no.3
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    • pp.199-207
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    • 2010
  • In this study, breast milk levels of indicator polychlorinated biphenyls (PCBs) were estimated, and statistics drawn, for 22 Koreans in the general population, aged 26-38, who had resided in metropolitan areas for more than 5 years without occupational exposure to organochlorine pollutants. Concentrations of indicator PCBs were measured using the isotope dilution method with a high resolution gas chromatograph/high resolution mass detector, which provided accurate and precise data for investigation of trends, and international comparisons. The geometric mean of total indicator PCB levels was 22.3 ng/g lipid, which is significantly lower than the level in individuals from European countries. Overall, the geometric mean and 95th percentile of the most abundant congener PCB 153 were 8.04 ng/g lipid and 16.4 ng/g lipid, respectively. PCB congeners 138, 153 and 180 together accounted for about 75% of the indicator congeners analyzed. Breast milk total indicator PCB concentrations were significantly associated with age and parity, but not with body mass index (BMI), rate of body weight increase, or smoking habits. The geometric mean level of PCB 153 in breast milk from mothers with a pre-pregnant BMI < $21\;kg/m^2$ was significantly higher than in pre-pregnant women with a BMI of ${\geqslant}\;21\;kg/m^2$ (p<0.05). Women who ate more fish, meat, and milk products did not have significantly higher total indicator PCB levels than those who ate less of these products, but a significant difference in PCB 153 levels was demonstrated between the subjects consuming higher (11.45 ng/g lipid) and lower (6.79 ng/g lipid) amounts of fish (p<0.05), after adjusting for confounders. These results suggest that age, parity and fish intake are the important factors affecting the concentrations of indicator PCBs in these subjects.

Evaluation of Cyantraniliprole Residues Translocated by Lettuce, Spinach and Radish (상추, 시금치 및 알타리무에 의한 Cyantraniliprole의 흡수이행 잔류량 평가)

  • Yoon, Ji Hyun;Lee, Seung Won;Lim, Da Jung;Kim, Seon Wook;Kim, In Seon
    • Korean Journal of Environmental Agriculture
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    • v.40 no.4
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    • pp.335-344
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    • 2021
  • BACKGROUND: Cyantraniliprole is a systemic diamide insecticide that has been used to control lepidopteran pests in agriculture. Cyantraniliprole has become an issue due to its potentiality of unexpectable contamination in rotational crop cultivation. Thus, studies on the evaluation of cyantraniliprole translocated from soil into rotational crops are required. METHODS AND RESULTS: Cyantraniliprole was treated at a yearly maximum application level onto bare soil under greenhouse conditions in two geographically different regions. Lettuce was transplanted and spinach and radish were sown onto the soil 30 and 60 days-plant back intervals (PBIs) after cyantraniliprole treatment. The QuEChERS method was modified and coupled with LC/MS/MS analysis to determine the residues of cyantraniliprole in soil and plant samples. The methods for sample preparation and instrumental conditions were validated to meet the criteria of Codex guidelines and were successful to determine cyantraniliprole quantitatively and qualitatively in the samples. Cyantraniliprole residues in lettuce samples were 0.01 mg/kg for PBI 60 and 0.02 mg/kg for PBI 30, respectively. The residues in spinach samples were 0.01 mg/kg for PBI 60 and 0.01~0.02 mg/kg for PBI 30, respectively. Less than limit of the quantitation (LOQ) level (0.01 mg/kg) of cyantraniliprole was observed in radish samples. The residues in the plant samples were found as the levels less than maximum residue limit (MRL) for leafy and root vegetables. CONCLUSION(S): This study suggests PBI 30~60 days for rotational cultivation of lettuce, spinach and radish in greenhouse soil treated with cyantraniliprole at a yearly maximum application level.

Analysis of Occupational Therapy Intervention Research for Improving Memory: Focus on Single-Subject Research Design in Korean Academic Journals (기억력 향상을 위한 작업치료 중재 연구 분석: 국내 단일대상연구 중심으로)

  • Jung, Yu-Jin;Choi, Yoo-Im
    • Therapeutic Science for Rehabilitation
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    • v.10 no.4
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    • pp.39-52
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    • 2021
  • Objective : This study aimed to identify the characteristics and analyze the quality of studies on memory improvement using a single-subject research design. Methods : Six studies were selected through the Research Information Sharing Service (RISS), Korean Studies Information Service System (KISS), and National Digital Science Library (NDSL). Keywords were memory training, stroke, early dementia, mild cognitive impairment, and single-subject research design. The characteristics and quality levels were analyzed between January 2011 and October 2020. Results : Regarding the quality level, the middle level (7-10 points) was 66.7% of the four articles, and the high level (11-14 points) was 33.3% of the two articles. Reversal designs were used in all studies. Independent variables were errorless learning, smartphone application, cognitive training system (CoTras), spaced retrieval training (SRT) with errorless learning, spaced retrieval training, and iPad applications. The dependent variables included memory, attention, electroencephalogram, instrumental activities of daily living, depression etc., which increased after the intervention. The total session, study period, and intervention time were varied. Conclusion : In single-subject research design related to memory training, occupational therapy intervention was confirmed as an effective method for improving memory and attention. The quality level of single-subject research design was moderate or higher, and high-quality level of studies should be conducted by additional design to increase the validity in the future.

Methodological Comparison of the Quantification of Total Carbon and Organic Carbon in Marine Sediment (해양 퇴적물내 총탄소 및 유기탄소의 분석기법 고찰)

  • Kim, Kyeong-Hong;Son, Seung-Kyu;Son, Ju-Won;Ju, Se-Jong
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.9 no.4
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    • pp.235-242
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    • 2006
  • The precise estimation of total and organic carbon contents in sediments is fundamental to understand the benthic environment. To test the precision and accuracy of CHN analyzer and the procedure to quantify total and organic carbon contents(using in-situ acidification with sulfurous acid($H_2SO_3$)) in the sediment, the reference material s such as Acetanilide($C_8H_9NO$), Sulfanilammide($C_6H_8N_2O_2S$), and BCSS-1(standard estuary sediment) were used. The results indicate that CHN analyzer to quantify carbon and nitrogen content has high precision(percent error=3.29%) and accuracy(relative standard deviation=1.26%). Additionally, we conducted the instrumental comparison of carbon values analyzed using CHN analyzer and Coulometeric Carbon Analyzer. Total carbon contents measured from two different instruments were highly correlated($R^2=0.9993$, n=84, p<0.0001) with a linear relationship and show no significant differences(paired t-test, p=0.0003). The organic carbon contents from two instruments also showed the similar results with a significant linear relationship($R^2=0.8867$, n=84, p<0.0001) and no significant differences(paired t-test, p<0.0001). Although it is possible to overestimate organic carbon contents for some sediment types having high inorganic carbon contents(such as calcareous ooze) due to procedural and analytical errors, analysis of organic carbon contents in sediments using CHN Analyzer and current procedures seems to provide the best estimates. Therefore, we recommend that this method can be applied to measure the carbon content in normal any sediment samples and are considered to be one of the best procedure far routine analysis of total and organic carbon.

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A Novel Volumetric Method for Quantitation of Titanium Dioxide in Cosmetics (용량분석법을 이용한 화장품 중 티타늄옥사이드의 정량)

  • Kim, Young-So;Kim, Boo-Min;Park, Sang-Chul;Jeong, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.31 no.4 s.54
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    • pp.289-293
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    • 2005
  • Nowadays there are many sun protection cosmetics including organic or inorganic UV filter as an active ingredient. Chemically stable inorganic sunsEreen agents, usually metal oxides, we widely employed in high SPF products. Titanium dioxide is one of the most frequently used inorganic UV filters. It has been used as pigments for a long period of cosmetic history. With the development of micronization techniques, it becomes possible to incorporate titanium dioxide in sunscreen formulations without whitening effect and it becomes an important research topic. However, there are very few works related to quantitations of titanium dioxide in sunscreen products. In this research, we analyzed amounts of titanium dioxide in sunscreen cosmetics by adapting redof titration, reduction of Ti(IV) to Ti(III) and reoxidation to Ti(IV). After calcification of other organic ingredients of cosmetics, titanium dioxide is dissolved by hot sulfuric acid. The dissolved Ti(IV) is reduced to the Ti(III) by adding aluminum metals. The reduced Ti(III) is titrated against a standard oxidizing agent, Fe(III) (ammonium iron(III) sulfate), with potassium thiocyanate as an indicator In order to test accuracy and applicability of the proposed method, we analyzed the amounts of titanium dioxide in four types of sunscreen cosmetics, such as cream, make-up base, foundation and powder, after adding known amounts of titanium dioxide $(1{\sim}25w/w%)$. The percent recoveries of the titanium dioxide in four types of formulations were in the range between 96 and 105%. We also analyzed 7 commercial cosmetic products labeled titanium dioxide as an ingredient and compared the results with those of obtained from ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry), one of the most powerful atomic analysis techniques. The results showed that the titrated amounts were well coincided with the analyzed amounts of titanium dioxide by ICP-AES. Although instrumental analytical methods, ICP-MS (Inductively Coupled Plasma-Mass Spectrometry) and ICP-AES, are the best for the analysis of titanium, it is hard to adopt because of their high prices for small cosmetic companies. It was found that the volumetric method presented here gat e quantitative and reliable results with routine lab-wares and chemicals.

Establishment of Test Conditions and Interlaboratory Comparison Study of Neuro-2a Assay for Saxitoxin Detection (Saxitoxin 검출을 위한 Neuro-2a 시험법 조건 확립 및 실험실 간 변동성 비교 연구)

  • Youngjin Kim;Jooree Seo;Jun Kim;Jeong-In Park;Jong Hee Kim;Hyun Park;Young-Seok Han;Youn-Jung Kim
    • Journal of Marine Life Science
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    • v.9 no.1
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    • pp.9-21
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    • 2024
  • Paralytic shellfish poisoning (PSP) including Saxitoxin (STX) is caused by harmful algae, and poisoning occurs when the contaminated seafood is consumed. The mouse bioassay (MBA), a standard test method for detecting PSP, is being sanctioned in many countries due to its low detection limit and the animal concerns. An alternative to the MBA is the Neuro-2a cell-based assay. This study aimed to establish various test conditions for Neuro-2a assay, including cell density, culture conditions, and STX treatment conditions, to suit the domestic laboratory environment. As a result, the initial cell density was set to 40,000 cells/well and the incubation time to 24 hours. Additionally, the concentration of Ouabain and Veratridine (O/V) was set to 500/50 μM, at which most cells died. In this study, we identified eight concentrations of STX, ranging from 368 to 47,056 fg/μl, which produced an S-shaped dose-response curve when treated with O/V. Through inter-laboratory variability comparison of the Neuro-2a assay, we established five Quality Control Criteria to verify the appropriateness of the experiments and six Data Criteria (Top and Bottom OD, EC50, EC20, Hill slop, and R2 of graph) to determine the reliability of the experimental data. The Neuro-2a assay conducted under the established conditions showed an EC50 value of approximately 1,800~3,500 fg/μl. The intra- & inter-lab variability comparison results showed that the coefficients of variation (CVs) for the Quality Control and Data values ranged from 1.98% to 29.15%, confirming the reproducibility of the experiments. This study presented Quality Control Criteria and Data Criteria to assess the appropriateness of the experiments and confirmed the excellent repeatability and reproducibility of the Neuro-2a assay. To apply the Neuro-2a assay as an alternative method for detecting PSP in domestic seafood, it is essential to establish a toxin extraction method from seafood and toxin quantification methods, and perform correlation analysis with MBA and instrumental analysis methods.

Recent Research for the Seismic Activities and Crustal Velocity Structure (국내 지진활동 및 지각구조 연구동향)

  • Kim, Sung-Kyun;Jun, Myung-Soon;Jeon, Jeong-Soo
    • Economic and Environmental Geology
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    • v.39 no.4 s.179
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    • pp.369-384
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    • 2006
  • Korean Peninsula, located on the southeastern part of Eurasian plate, belongs to the intraplate region. The characteristics of intraplate earthquake show the low and rare seismicity and the sparse and irregular distribution of epicenters comparing to interplate earthquake. To evaluate the exact seismic activity in intraplate region, long-term seismic data including historical earthquake data should be archived. Fortunately the long-term historical earthquake records about 2,000 years are available in Korea Peninsula. By the analysis of this historical and instrumental earthquake data, seismic activity was very high in 16-18 centuries and is more active at the Yellow sea area than East sea area. Comparing to the high seismic activity of the north-eastern China in 16-18 centuries, it is inferred that seismic activity in two regions shows close relationship. Also general trend of epicenter distribution shows the SE-NW direction. In Korea Peninsula, the first seismic station was installed at Incheon in 1905 and 5 additional seismic stations were installed till 1943. There was no seismic station from 1945 to 1962, but a World Wide Standardized Seismograph was installed at Seoul in 1963. In 1990, Korean Meteorological Adminstration(KMA) had established centralized modem seismic network in real-time, consisted of 12 stations. After that time, many institutes tried to expand their own seismic networks in Korea Peninsula. Now KMA operates 35 velocity-type seismic stations and 75 accelerometers and Korea Institute of Geoscience and Mineral Resources operates 32 and 16 stations, respectively. Korea Institute of Nuclear Safety and Korea Electric Power Research Institute operate 4 and 13 stations, consisted of velocity-type and accelerometer. In and around the Korean Peninsula, 27 intraplate earthquake mechanisms since 1936 were analyzed to understand the regional stress orientation and tectonics. These earthquakes are largest ones in this century and may represent the characteristics of earthquake in this region. Focal mechanism of these earthquakes show predominant strike-slip faulting with small amount of thrust components. The average P-axis is almost horizontal ENE-WSW. In north-eastern China, strike-slip faulting is dominant and nearly horizontal average P-axis in ENE-WSW is very similar with the Korean Peninsula. On the other hand, in the eastern part of East Sea, thrust faulting is dominant and average P-axis is horizontal with ESE-WNW. This indicate that not only the subducting Pacific Plate in east but also the indenting Indian Plate controls earthquake mechanism in the far east of the Eurasian Plate. Crustal velocity model is very important to determine the hypocenters of the local earthquakes. But the crust model in and around Korean Peninsula is not clear till now, because the sufficient seismic data could not accumulated. To solve this problem, reflection and refraction seismic survey and seismic wave analysis method were simultaneously applied to two long cross-section traversing the southern Korean Peninsula since 2002. This survey should be continuously conducted.