• Title/Summary/Keyword: ion detection

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Establishment of Analytical Method for Pencycuron in Representative Agricultural Commodities by High-Performance Liquid Chromatography (대표 농산물 중 살균제 Pencycuron의 HPLC 정밀 잔류분석법 개발)

  • Lee, Hyeri;Choi, Hoon;Kim, Byung-Joon;Kim, Eunhye;Kim, Su-Hee;Lee, Jin-Beom;Lee, Young Deuk;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
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    • v.21 no.1
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    • pp.75-83
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    • 2017
  • The single residue analytical method was developed for determining fungicide pencycuron residues in various agricultural commodities with high-performance liquid chromatography (HPLC). Pencycuron residue was extracted with acetone from representative crops such as Korean cabbage, apple, brown rice and green pepper. After ethyl acetate/n-hexane partition and subsequent clean-up with silica gel chromatography, pencycuron residue was quantified by reversed phase HPLC with UV detection at 240 nm. The suspected residue of pencycuron was confirmed using selected-ion monitoring (SIM) LC/mass spectrometry (MS). Instrumental limit of quantitation (ILOQ) and method LOQ (MLOQ) were set at 2 ng and 0.02 mg/kg, respectively. Overall recoveries of pencycuron from different crop samples fortified at three levels (MLOQ, 10MLOQ, 100MLOQ) were 72~108%. This proposed method could be useful as official analytical method for quantification of pencycuron residues in agricultural commodities.

Survey and method validation of simultaneous quantitative analysis of T-2 and HT-2 toxins in cereals (곡류 중 T-2 및 HT-2 독소 동시 정량분석의 유효성 검증 및 실태조사)

  • Paek, Ockjin;Kang, Teabeom
    • Food Science and Preservation
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    • v.22 no.4
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    • pp.559-566
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    • 2015
  • The aim of this study was to develop an analytical method for determination of T-2 toxin and HT-2 toxin level in cereals and to survey their levels using LC-MS/MS. The T-2 and HT-2 toxins were simultaneously analyzed by electrospray ionization with a positive ion mode and multiple reaction monitoring (MRM) after filteration and immuno-affinity column clean-up. A matrix-matched standard calibration used for quantification and recoveries of T-2 and HT-3 toxins were in the range of $100.6{\pm}7.2%$ and $96.8{\pm}9.4%$, respectively. Limits of detection and quantification of T-2 and HT-2 toxins were estimated to be 0.5 and $1.5{\mu}g/kg$, respectively. Each repeatability (RSRr) of T-2 and HT-2 toxins was determined to be 0.9~6.0%, and 4.9~6.1%, respectively. Total 115 samples cereals were collected from 9 types of cereals for analysis. The positive percentages of T-2 and HT-2 toxins obtained from collected samples were found to be 72% and 80%, respectively. The contamination level of T-2 toxin and HT-2 toxin in cereals were $37.1{\mu}g/kg$, and $5.4{\mu}g/kg$, respectively. Therefore, this study suggests that the developed method could be an useful analytical method to determine the T-2 and HT-2 toxin level in cereals and the present data could be used as a reference to estimate the risk assessment.

Antioxidant capacity in seedling of colored-grain wheat under water deficit condition

  • Kim, Dae Yeon;Hong, Min Jeong;Jung, Woo Joo;Seo, Yong Weon
    • Proceedings of the Korean Society of Crop Science Conference
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    • 2017.06a
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    • pp.140-140
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    • 2017
  • Nutritious and functional foods from crop have received great attention in recent years. Colored-grain wheat contains high phenolic compound and a large number of flavonoid. The anthocyanin and polyphenolic synthesis and accumulation is generally stimulated in response to biotic or abiotic stresses. Here, we analyzed genome wide transcripts in seedling of colored-grain wheat response to ABA and PEG treatment. About 900 and 1500 transcripts (p-value < 0.05) from ABA and PEG treatment were aligned to IWGSC1+popseq DB which is composed of over 110,000 transcripts including 100,934 coding genes. NR protein sequences of Poaceae from NCBI and protein sequence of transcription factors originated from 83 species in plant transcription factor database v3.0 were used for annotation of putative transcripts. Gene ontology analysis were conducted and KEGG mapping was performed to show expression pattern of biosynthesis genes related in flavonoid, isoflavonoid, flavons and anthocyanin biopathway. DroughtDB (http://pgsb.helmholtz-muenchen.de/droughtdb/) was used for detection of DEGs to explain that physiological and molecular drought avoidance by drought tolerance mechanisms. Drought response pathway, such as ABA signaling, water and ion channels, detoxification signaling, enzymes of osmolyte biosynthesis, phospholipid metabolism, signal transduction, and transcription factors related DEGs were selected to explain response mechanism under water deficit condition. Anthocyanin, phenol compound, and DPPH radical scavenging activity were measured and antioxidant activity enzyme assays were conducted to show biochemical adaptation under water deficit condition. Several MYB and bHLH transcription factors were up-regulated in both ABA and PEG treated condition, which means highly expressed MYB and bHLH transcription factors enhanced the expression of genes related in the biosynthesis pathways of flavonoids, such as anthocyanin and dihydroflavonols in colored wheat seedlings. Subsequently, the accumulation of total anthocyanin and phenol contents were observed in colored wheat seedlings, and antioxidant capacity was promoted by upregulation of genes involved in maintaining redox state and activation of antioxidant scavengers, such as CAT, APX, POD, and SOD in colored wheat seedlings under water deficit condition. This work may provide valuable and basic information for further investigation of the molecular responses of colored-grain wheat to water deficit stress and for further gene-based studies.

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Assessment for the Comparability between Korean Ministry of Environment Standard and ISO Standard for the Determination of Heavy Metals in Soil (토양 중금속 함량 측정에 대한 토양오염공정시험기준과 국제표준간의 적합성 평가)

  • Shin, Gun-Hwan;Lee, Goon-Teak;Lee, Won-Seok;Kim, Ji-In;Kim, Bo-Kyong;Park, Hyun-Jeong
    • Journal of Soil and Groundwater Environment
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    • v.17 no.3
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    • pp.1-9
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    • 2012
  • According to the agreement on WTO/TBT, we are under the situation to adopt international standard (ISO standard) as a national standard if it exists. However, in case of environmental area, it is a domestic legal obligation to use Korean environmental standard method(KESM) for analyzing various contaminants. Therefore it is necessary to assess the comparability between KEM and ISO standard prior to apply ISO standard to soil conservation law in Korea. The main purpose of this study is to assess the comparability of both methods for analyzing heavy metals in soil. We looked over various aspects like pre-treatment, calibration curve range, detection wavelength, soil organic matter content and so on. Apparently, the procedure of both methods is almost same. However in details, both methods are different in stationary time before aqua-regia extraction using reflux system, calibration curve range for Cu, Pb, Ni and measuring wavelength for Pb. According to the results of comparison test, the results were significantly different when the different calibration range was used. In case that all the extracts independent of methods were reanalyzed with the same calibration range of each method, both methods showed statistically same results. Other conditions like different stationary time, measuring wavelength of AAS and soil organic matter content did not have any influence on the analytical result. Therefore, we suggest to extend the calibration curve range to 0~8 mg/L which is used in KS I ISO standard(Korean standard related with environment which is translation version of ISO standard without any technical change). In case of $Cr^{6+}$, the results showed no significant differences between two methods even though the pretreatment, instrumentation and other analysis conditions were different. In addition to UV/Visble spectrometry of KESM for soil contamination, we suggest to adopt ion chromatography of ISO 15192(US EPA method 7199) for analyzing $Cr^{6+}$ with the consideration of laboratory work efficiency.

Patient-Specific Quality Assurance in a Multileaf Collimator-Based CyberKnife System Using the Planar Ion Chamber Array

  • Yoon, Jeongmin;Lee, Eungman;Park, Kwangwoo;Kim, Jin Sung;Kim, Yong Bae;Lee, Ho
    • Progress in Medical Physics
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    • v.29 no.2
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    • pp.59-65
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    • 2018
  • This paper describes the clinical use of the dose verification of multileaf collimator (MLC)-based CyberKnife plans by combining the Octavius 1000SRS detector and water-equivalent RW3 slab phantom. The slab phantom consists of 14 plates, each with a thickness of 10 mm. One plate was modified to support tracking by inserting 14 custom-made fiducials on surface holes positioned at the outer region of $10{\times}10cm^2$. The fiducial-inserted plate was placed on the 1000SRS detector and three plates were additionally stacked up to build the reference depth. Below the detector, 10 plates were placed to avoid longer delivery times caused by proximity detection program alerts. The cross-calibration factor prior to phantom delivery was obtained by performing with 200 monitor units (MU) on the field size of $95{\times}92.5mm^2$. After irradiation, the measured dose distribution of the coronal plane was compared with the dose distribution calculated by the MultiPlan treatment planning system. The results were assessed by comparing the absolute dose at the center point of 1000SRS and the 3-D Gamma (${\gamma}$) index using 220 patient-specific quality assurance (QA). The discrepancy between measured and calculated doses at the center point of 1000SRS detector ranged from -3.9% to 8.2%. In the dosimetric comparison using 3-D ${\gamma}$-function (3%/3 mm criteria), the mean passing rates with ${\gamma}$-parameter ${\leq}1$ were $97.4%{\pm}2.4%$. The combination of the 1000SRS detector and RW3 slab phantom can be utilized for dosimetry validation of patient-specific QA in the CyberKnife MLC system, which made it possible to measure absolute dose distributions regardless of tracking mode.

Application of Freezing Filtration Method to the Analysis of Alkylphenols, Chlorophenols and Bisphenol a in Korean Aquatic Biological Samples Using GC/MS-SIM (GC/MS-SIM을 이용한 우리나라 수중 생물시료 중 알킬페놀, 클로로페놀과 비스페놀 A의 분석을 위한 냉동필터법의 응용)

  • Kim, Hyub;Jang, Cheol-Hyeon
    • Journal of Korean Society of Environmental Engineers
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    • v.29 no.6
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    • pp.689-698
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    • 2007
  • A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples. The alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples were extracted with acetonitrile and then acetonitrile layer was refrigerated at $-60^{\circ}C$ for 2 hours(freezing filtration method). Also, solid-phase extraction(SPE) was used to XAD-4 and subsequent conversion to isobutoxycarbonyl(isoBOC) or tert-butyldimethylsilyl(TBDMS) derivatives for sensitive analysis with gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM) mode. For isoBOC derivatization and TBDMS derivatization the recoveries were $70.1\sim150.6%$ and $93.8\sim108.3%$, the method detection limit(MDLs) of bisphenol A for SIM were $0.062{\mu}g/kg$ and $0.010{\mu}g/kg$, and the SIM respectively. When these methods were applied to korean aquatic biological samples, the concentrations of the 11 phenolic EDCs were $0.675\sim1.970{\mu}g/kg$.

Evaluation of Testosterone Metabolites/Dehydroepiandrosterone As the Indicators of Testosterone Administration in Horse Doping (경주마 약물검사에서 testosterone 투여 여부표지자로서의 testosterone 대사체들에 대한 dehydroepiandrosterone의 비율 평가)

  • Kim, Jin Young;Choi, Man Ho;Kim, Sung Jean;Kyong, Jin Burm;Chung, Bong Chul
    • Analytical Science and Technology
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    • v.12 no.3
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    • pp.190-195
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    • 1999
  • The metabolism of testosterone ($17{\beta}$-hydroxy-androst-4-en-3-one) was confirmed in horse after a single intramuscular administration of testosterone cypionate (750 mg). Solvent extracts of urine obtained with enzymatic hydrolysis and methanolysis were analyzed by GC/MS after oxime t-butyldimethylsilyl (oxime-TBDMS) derivatization. The structures of four urinary metabolite after testosterone administration in horse were determined based on EI mass spectra and $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol and $5{\alpha}$-androstane-$3{\beta}$-ol-17-one as major was confirmed with authentic standard. Also the concentrations of $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol, $5{\alpha}$-androstane-$3{\beta}$, $17{\beta}$-diol, dehydroepiandrosterone (DHEA), $5{\alpha}$-androstane-$3{\beta}$-ol-17-one and testosterone were determined in the urine of normal subjects and the urine after administration. The recovery and detection limit in the most drugs were 86.3~94.7% and 1~3 ppb, respectively. Correlation coefficients for calibration were in the range of 0.984~0.999. Excretion profile of testosterone presents the rapid and large increasement up to maximum values at days 5 after administration and the slow regression. The relative ratios of testosterone, its metabolites over DHEA were determined for indication of testosterone administration in horse doping.

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Preconcentration and Determination of Trace Cobalt and Nickel by the Adsorption of Metal-PDC Complexes on the Anion-Exchange Resin Suspension (금속-PDC 착물의 음이온교환 수지 상 흡착에 의한 흔적량 코발트와 니켈의 동시 예비농축 및 정량)

  • Han, Chul-Woo;In, Gyo;Choi, Jong-Moon;Kim, Sun Tae;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.608-615
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    • 2000
  • A determination method of trace nickel and cobalt in water samples was studied and developed by adsorbing their complexes on ion exchange resin suspension. The analytical ions were formed as complexes with a ligand of APDC (ammonium pyrrolidinedithiocarbamate) and adsorbed on anion exchange resin of Dowex 2-X8. After the suspension was filtered out with membrane filter, the complexes were dissolved in HCl solution by an ultrasonic vibrator for ET-AAS determination. Several conditions were optimized as followings. pH of sample solution: 5.0, amount of ligand APDC: more than 430 times in mole ratio, the type and concentration of acid: 0.1 M HCl, and vibration time: 7 minutes. The addition of palladium in the HCl solution could improve the reproducibility and sensitivity by a matrix modification in the absorbance measurement. This procedure was applied for the analysis of three kinds of real water samples. The detection limits equivalent to 3 times standard deviation of blank were Co 0.36 ng/mL and Ni 0.27 ng/mL and recoveries in spiked samples were 99-102% for cobalt and 100-105% for nickel.

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High Sensitive Strain Detection of FeCoSiB Amorphous Films (아몰퍼스 FeCoSiB 박막의 고감도 스트레인 검출특성)

  • Shin, Kwang-Ho;Arai, Ken-Ichi;SaGong, Geon
    • Journal of Sensor Science and Technology
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    • v.9 no.1
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    • pp.22-27
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    • 2000
  • Amorphous FeCoSiB films with high saturation magnetostriction and excellent soft magnetic properties have been studied to evaluate their strain sensitivity. Films were subjected to a strain by bending of their substrates, which caused a change in the magnetic anisotropy of films via magnetoelastic coupling. Films were exhibited a figure of merit $F=({\Delta}{\mu}/{\mu})/{\varepsilon}$ (change in film permeability $\mu$ per unit strain $\varepsilon$) of $1.2{\times}10^5$, which is comparable with that of amorphous ribbons. To make a study of application of magnetostrictive films as strain sensor elements, we have prepared a micro-patterned film by means of the photolithography and ion milling processes. Impedance change in the patterned films, when strain was applied, was measured over the frequency range from 1 MHz to 1 GHz. Reflecting a large value of figure of merit F, a variation of 46% impedance of films was shown at 100 MHz frequency when a strain of $300{\times}10^{-6}$ was applied.

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A Study on the Reinforcement and Environmental Impact of LW Injection (LW주입에 의한 지반보강 및 환경영향성에 관한 연구)

  • Chun, Byungsik;Do, Jongnam;Sung, Hwadon;Lim, Jooheon
    • Journal of the Korean GEO-environmental Society
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    • v.7 no.6
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    • pp.121-131
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    • 2006
  • This study is performed to examine the ground reinforcement effect and the environmental impact of LW injection, which is widely used during the excavation of high-rise apartment buildings. In addition, it proved that by conducting field exploration and laboratory test the engineering ground reinforcement effect of LW injection in the ground has low coefficient of permeability. The environmentally friendly aspect was evaluated through an assessment of environmental impact. The results of laboratory test shows that LW coagulating material with SC type soil structure has significant improvement of uniaxial compressive strength, increasing by three times and the shear strength increasing by twice, coefficient of permeability decreasing six to seven times. And the result of environmental impact tests show that from 6 hour after where the pH increases until 7.96 to initially it diminished, it started and to 80 hour after it recovered a pH 7.25 initially with 7.30. The chemical composition analysis test result that unpolluted water and polluted water hydrogen ion concentration (pH) show that the unpolluted water pH 7.36, polluted water pH 7.85, which is inside the Ministry of Environment standard of drinking water (the pH 5.8~8.5). The assessment of environmental impact and chemical analysis test also demonstrate that the LW coagulating material is environmentally friendly. In the $Cr^{6+}$ and the salinity detection test, it was proven that the salinity is slight and the $Cr^{6+}$ is not detected.

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