• Title/Summary/Keyword: 감도 계수법

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A New Analytical Method for the $Eu^{+3}$ and $Tb^{+3}$ Ions Using the Luminescence Enhancement by the Treatment of o-Phenanthroline on the Nylon Membrane (Nylon Membrane Filter에서의 발광증폭을 이용한 $Eu^{+3}$$Tb^{+3}$ 이온의 극미량 분석법)

  • An, Seong-Hee;Lee, Byung-Min;Park, Jong-Mok;Kim, Hai-Dong;Jeong, Hyuk
    • Journal of the Korean Chemical Society
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    • v.39 no.9
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    • pp.705-714
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    • 1995
  • A new analytical luminescence method for the Eu+3 and Tb+3 ions was studied using the luminescence enhancement by the treatment of the o-phenanthroline on the nylon membrane. Compared to the specific emission intensities of the ions in aqueous(or ethanol) solution, if the aqueous ion is spotted on the nylon membrane, the luminescence intensities were extremely enhanced. There was additional enhancement effect of the luminescence intensities of the ions on the nylon membrane, if the ion on the nylon membrane is treated with o-phenanthroline. Based on the luminescence enhancement, the detection limits were lowered by more than 7 order of magnitude compared to that of solution sample, and also lowered by about 1 order of magnitude compared to that of previous TLC method. The dynamic ranges and correlation coefficients of the calibration curves near the detection limit were 2∼3 order and ∼0.99, respectively. It was also shown that the luminescence intensity was in its maximum when the ion on the nylon is treated with ∼4 mole ratio of o-phenanthroline. The energy-transfer mechanism was explained for the theoretical background of the luminescence enhancement.

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Quantification of Entacapone in Human Plasma by HPLC Coupled to ESI-MS/MS Detection: Application to Bioequavalence Study (체외에서 ESI-MS/MS 탐지에 연결된 HPLC에 의한 Entacapon의 수량화: 생물학적 동등성 연구에 적용)

  • Balasekhara Reddy., Ch.;Baburao., Ch.;Chandrasekhar., K.B.;Kanchanamala., K.;RihanaParveen., S.K.;Ravikumar., Konda
    • Journal of the Korean Chemical Society
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    • v.54 no.5
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    • pp.523-532
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    • 2010
  • The proposed method is simple, sensitive and specific Liquid chromatography-tandem mass spectrometry (LCESI-MS/MS) method for the quantification of Entacapone (EA) in human plasma using Entacapone-d10 (EAD10) as an internal standard (IS). Chromatographic separation was performed on Zorbax SB-C18, $2.1{\times}50\;mm$, $5\;{\mu}m$ column, mobile phase composed of 10 mM Ammonium formate (pH 3.0): Acetonitrile (60:40 v/v), with a flow-rate of 0.7 mL/min, followed by Liquid-liquid extraction. EA and EAD10 were detected with proton adducts at m/z $306.1{\rightarrow}233.1$ and $316.3{\rightarrow}233.0$ in multiple reaction monitoring (MRM) positive mode respectively. The method was validated over a linear concentration range of 1.00 - 2000.00 ng/mL with correlation coefficient ($r^2$) $\geq$ 0.9993. Intra and inter-day Precision within 3.60 to 7.30 and 4.20 to 5.50% and Accuracy within 97.30 to 104.20 and 98.30 to 105.80% proved for EA. This method is successfully applied in the bioequivalence study of healthy Indian human volunteers.

항만개발에 의한 조석조류 및 수질변화 예측을 위한 시뮬레이션 모델 연구

  • 박석순;김소연;이진희
    • Proceedings of the Korea Society for Simulation Conference
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    • 1997.04a
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    • pp.114-114
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    • 1997
  • 항만개발 사업은 매립이나 준설과 같은 해안선과 해저지형을 변화시키는 공사가 이루어지며 이는 조석조류 현상의 변화를 유발하게 된다. 특히 해안지형이 복잡한 항만이나 하구에서는 변화정도가 크게 나타나며 방파제나 선박접안 시설과 같은 항내 구조물을 축조 할 경우에도 조석조류 변화가 야기된다. 조석조류 현상의 변화는 해양 수질과 생물상에 영 향을 줄뿐만 아니라 인접한 육지에 이르기까지 크다란 피해를 유발할 수가 있다. 창조시 해 수를 육지로 범람하게 하거나 퇴적이나 침식조건을 변화시킬 수도 있으며 오염물질이 외해 로 확산되는 과정을 방해하고 해양생물의 서식조건을 악화시켜 부근 해역의 어업에 피해를 유발할 수도 있다. 또한 해안 공사 과정에 해수로 유입되는 토사나 항만 이용시에 배출되는 폐수 등이 항내 수질과 생태계를 변화시킬 수 있다. 따라서 조석조류와 수질변화를 사전에 예측하고 이를 최소화하는 방안이 강구되어야 한다. 조석조류와 수질 변화를 사전에 예측하 는 방법으로 축소모형 실험과 컴퓨터 시뮬레이션이 사용된다. 축소모형 실험은 현장을 재현 하는데 많은 경비와 시간이 소모되며 예측에 한계가 있다. 반면에 컴퓨터 시뮬레이션은 대 상해역의 지형과 조류 그리고 수질특성에 적합하게 모델을 개발할 경우 예측력이 매우 높기 때문에 현재 가장 널리 이용되고 있다. 본 연구는 유한 요소법에 기초하여 미국 공병단 (United States Army Corps of Engineers)에서 개발한 TABS-2 모델을 이용하여 온산항에 서 시행되는 부두건설에 따른 조석조류 및 수질변화를 시뮬레이션하였다. 측정된 자료로 모 델 계수를 보정하고 검증하였으며 항내 매립과 준설이 이루어질 때 나타나는 조위와 조속변 화를 예측하였다. 매립과 준설공사시 유출되는 토사가 조석조류현상에 따라 이동 확산되는 범위와 농도분포를 예측하였다.ophobic components)은 75~80%, 친수성 물질(hydrophilic components)은 30~33%정도의 분포를 보였고, 전염소 및 전오존 공정을 거친 처리수에서는 각각 62.2-62.8%, 43.9~49.0% 및 50~ 55%, 40~57% 정도의 분포를 보였다. 그리고 웅집-침전을 거친 처리수에서는 그 분포가 77~82%, 24-48%였다. 전주리 공정을 통하여 소수성 물질(byoghobic components)의 분포가 감 소하는 것을 볼 때 전염소 및 전오존 처리가 용존유기물의 응집에는 오히려 역 효과를 나타내는 것으로 판단된다. 것으로 판단된다.여 황토 2g에 대하여 Hieltijes and Lijklema 방법에 의해 Adsorbed-p, Nonapatite inorganic-P(NAI-P), Apatite-p, Organic-P로 구분하여 분석하고, 총인(Total Phosphorus)을 Standard Methods에 따라 Persulfate digestion후 0.45 m membrane 여지 여과하여 여액에 대해 PO3-4-P의 농도를 Ascorbic Acid 법으로 측정한 결과, NAI-P가 가장 큰 비율을 차지하였고, 부원료로 첨가된 금속 양이온 중 Fe3-이온이 흡착에 기여하는 정도가 가장 큰 것으로 평가되었다.다당류 T-AS의 보체 활성화 기작은 classical과 alternative complement pathway의 양 경로를 통해 활성화 되었다. T-AS 분획은 mouse내의 특정 혈청단백을 증가시켰으며, 항체 생성능의 증가가 관찰되어 effect T 세포의 활성화가 나타나고 있음을 알 수 있었다. T-AS는 생체내 투여시에 대식세포의 탐식능이 증진되었으며, 대식세포 기능 저해제에 의한 대식세포의 기능 저해 현상이 회복되었다. 이와 같은 결과들로부터, T-AS의 항암 활성은 활성

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Development and Interlaboratory Validation of an Analytical Method for the Determination of Saflufenacil in Agricultural Products by HPLC-UVD and LC-MS

  • Do, Jung-Ah;Park, Hyejin;Kwon, Ji-Eun;Oh, Jae-Ho;Cho, Yoon-Jae;Chang, Moon-Ik;Choi, Won-Jo;Lee, Hyun-Sook;Hong, Jin-Hwan
    • Journal of Food Hygiene and Safety
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    • v.29 no.4
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    • pp.285-291
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    • 2014
  • Saflufenacil is a low-volatile and uracil-based herbicide. This herbicide is used for pre-and post-emergence control of major broadleaf weeds. The objective of present study was to develop and validate an analytical method for saflufenacil determination in agricultural products for ensuring the food safety. The saflufenacil residues in samples were extracted with acetone, dichloromethane, and then purified with silica and graphitized carbon cartridge. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. The linear range of saflufenacil was $0.1{\sim}5.0{\mu}gmL^{-1}$ with the correlation coefficient (r) = 0.999. Average recoveries of saflufenacil ranged from 80.5% to 110.2% at the spiked level of $0.02{\sim}0.5mgkg^{-1}$, while the relative standard deviation was 0.3~7.3%. In addition, the limit of detection and limit of quantification were 0.005 and $0.02mgL^{-1}$, respectively. Furthermore, an interlaboratory study among three labs was conducted to validate the method, and the results were satisfactory.

Rapid and simultaneous determination of metabolites of organic solvents in human urine by high-performance liquid chromatography using a monolithic column (Monolithic 칼럼을 이용한 뇨 중 유기용매 대사체의 신속한 HPLC 동시 분석)

  • Han, Sang Beom;Lee, Sang-Ju;Lee, Cheol-Woo;Yoon, Seo Hyun;Joung, Sun Kyung;Youm, Jeong-Rok
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.433-440
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    • 2006
  • A HPLC/UV method was developed and validated for the rapid and simultaneous determination of urinary metabolites of organic solvents, mandelic acid, hippuric acid, phenylglyoxylic acid, ortho-, meta- and para-methylhippuric acid, using a monolithic column. The mobile phase was composed of tetrabutylammonium bromide as ion-pairing reagent with a flow rate of 2.4 mL/min. The total run time was less than 2.5 min for all six analytes. Good linearities were obtained for all the metabolites with correlation coefficients above 0.9993. Intra-day precision, accuracy and inter-day precision was 0.01~7.32%, 83.9~116.3% and 0.01~7.16%, respectively. The method was validated and confirmed by quantification of the quality assurance samples of Industrial Safety and Health Research Institute, Korea Occupational Safety and Health Agency.

Determination of lercanidipine in human plasma by LC-MS/MS (LC-MS/MS를 이용한 혈장 중 레르카니디핀의 분석)

  • Jang, Moon-Sun;La, Sookie;Chang, Kyu Young;Kang, Seung Woo;Han, Sang Beom;Lee, Kyung Ryul;Lee, Hee Joo
    • Analytical Science and Technology
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    • v.21 no.1
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    • pp.34-40
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    • 2008
  • Liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the quantitative determination of lercanidipine in human plasma. After addition of internal standard (amlodipine), plasma was precipitated with acetonitrile and the supernatant was evaporated. The residues were dissolved in 50 % acetonitrile and analyzed by LC-MS/MS. Using MS/MS with multiple reaction monitoring(MRM) mode, lercanindipine were selectively detected without severe interference from human plasma. The standard calibration curve for lercanidipine was linear (r = 0.9994) over the concentration range 0.05-20.0 ng/mL in human plasma. The intra- and inter-day precision over the concentration range of lercanidipine was lower than 11.7 % (correlation of variance, CV), and accuracy was between 94.4-114.8 %. This method has been successfully applied to the pharmacokinetic study of lercanidipine in human plasma.

Sintering behavior and electrical properties of transition metal (Ni, Co, Mn) based spinel oxides for temperature sensor applications (복합전이금속(Ni, Co, Mn) 기반 스피넬계 산화물의 소결 거동 및 온도센서 특성 연구)

  • Younghee So;Eunseo Lee;Jinyoung Lee;Sungwook Mhin;Bin Lee;Hyung Tae Kim
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.34 no.2
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    • pp.73-77
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    • 2024
  • The spinel-type oxide (Nix, Mny, Co3-x-y)O4 (NMC) is widely utilized as a material for temperature sensors with a negative temperature coefficient (NTC), finding applications across various industries including electric vehicle battery management systems. Typically, NMC is manufactured using solid-state reaction methods employing powders of Ni, Mn, and Co compounds, with the densification process through sintering recognized as a crucial factor determining the electrical properties of the temperature sensor material. In this study, NMC pellets were synthesized via solid-state reaction and their crystallographic and microstructural characteristics were investigated. Also, the activation energy for densification behavior during the sintering process was determined. According to the analysis results, the room temperature resistance of the NMC pellets was measured at 10.03 Kohm, with the sensitivity parameter, B-value, recorded at 3601.8 K, indicating their potential applicability as temperature sensors across various industrial fields. Furthermore, the activation energy for densification was found to be 273.3 ± 0.4 kJ/mol, providing valuable insights into the thermodynamic aspects of the sintering process of the NMC.

Development and Validation of an Official Analytical Method for Determination of Ipfencarbazone in Agricultural Products using GC-ECD (GC-ECD를 이용한 농산물 중 Ipfencarbazone의 신규분석법 개발 및 검증)

  • Jang, Jin;Kim, Heejung;Lee, Eun-Hyang;Ko, Ah-Young;Ju, Yunji;Kim, Sooyeon;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.210-217
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    • 2015
  • Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.

Development of analytical method for determination of spinetoram residues in livestock using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 Spinetoram 공정시험법 개발 및 검증)

  • Ko, Ah-Young;Kim, Heejung;Do, Jung Ah;Jang, Jin;Lee, Eun Hyang;Ju, Yun Ji;Kim, Ji Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • v.29 no.2
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    • pp.94-103
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    • 2016
  • An analytical method was developed to determine the amount of spinetoram (spinetoram J and spinetoram L) in livestock samples. The spinetoram was extracted with acetonitrile and purified through a primary secondary amine (PSA) sorbent. The spinetoram residues were then quantified and confirmed using a liquid chromatography–tandem mass spectrometer (LC-MS/MS) in the positive ion mode using multiple reactions monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/kg) into a blank extract with r2 > 0.994. The limits of detection and quantification were 0.002 and 0.01 mg/kg, respectively. The recovery results of spinetram ranged between 81.9-106.4% at different concentration levels (LOQ, 10LOQ, 50LOQ, n=5) with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003). An interlaboratory study was conducted to validate the method. The proposed analytical method proved to be accurate, effective, and sensitive for spinetoram determination. The method will be used as an official analytical method in Korea.

Determination of Soluble Carbohydrates in Soybean Seeds Using High Performance Liquid Chromatography with Evaporative Light Scattering Detection (증기화광산란 검출기를 이용한 콩 함유 수용성 탄수화물의 분석)

  • Kim, Gyeong-Ha;Hwang, Young-Sun;Ahn, Kyung-Geun;Kim, Gi-Ppeum;Kim, Min-Ji;Hong, Seung-Beom;Moon, Jung-Kyeong;Choung, Myoung-Gun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.7
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    • pp.1062-1067
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    • 2014
  • In the present study, a new analytical method was devised for the simultaneous determination of soluble carbohydrates in soybean seeds using high performance liquid chromatography/evaporative light scattering detection (HPLC/ELSD). The limit of quantification (LOQ) for soybean soluble carbohydrates ranged from 5.6~7.6 mg/kg using the HPLC/ELSD method and from 16.2~33.9 mg/kg using the high performance liquid chromatography/refractive index detection (HPLC/RID) method. Therefore, the HPLC/ELSD method was more sensitive than HPLC/RID. The precision values for retention time and peak area of the HPLC/ELSD method were evaluated by inter-day (n=5) and intra-day (n=10) assays using a standard solution. All precision values (CV<2.5%) for soybean soluble carbohydrates were acceptable and fulfilled international acceptance criteria. All linear calibration curves were obtained with a correlation coefficient of $R^2$ >0.999. The contents of soluble carbohydrates for the "Shingikong" (yellow soybean) and "Cheongjakong 3" (black soybean) samples were analyzed using the HPLC/RID and HPLC/ELSD methods. The difference in carbohydrate contents between the two detection methods was significant. Carbohydrate contents in the HPLC/ELSD method were higher than those in the HPLC/RID method. Overall, the HPLC/ELSD method showed satisfactory resolution with a favorable LOQ and reproducibility. Therefore, these results indicate that the HPLC/ELSD method may be applied to determine the contents of soluble carbohydrates in soybean seeds and related food stuffs.