• Title/Summary/Keyword: SPE1

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Trifluralin in aquatic products: QuEChERS and Gas chromatography-tandem mass spectrometry for trace amount detection

  • Le-Thi Anh-Dao;Do Minh-Huy;Vo Hong-Phong;Nguyen Cong-Hau
    • Analytical Science and Technology
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    • v.36 no.5
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    • pp.205-215
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    • 2023
  • In the present study, an analytical method was proposed for detecting trifluralin in aquatic products at trace concentrations. The method employed QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) and gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) as the sample preparation and measurement, respectively. The effect of the aqueous phase volume used in the QuEChERS was demonstrated, and the ratio of 10:10 (mL) between water and acetonitrile phase was used for 5 g of sample. Besides, dSPE using C18 and primary-secondary amine (PSA) was applied to remove the potential interferences from the food matrices, indicating no remarkable analyte loss. The linear range was built up from 0.50 ㎍ L-1 to 3.0 ㎍ L-1 (R2 = 0.9993). Other criteria, i.e., repeatability (RSDr = 0.86-1.96 %), reproducibility (RSDR = 1.09-2.01 %), and recovery (over 90 %), were in accordance with Appendix F of AOAC (2016) for method performance. Although no trifluralin was detected for the commercial samples (fish, shrimp, and breaded shrimp), the spiked samples performed favorable recoveries and precision.

Determination of Pyribencarb and Its Metabolite KIE-9749 in Agricultural Commodities by High-Performance Liquid Chromatography (액체크로마토그래피를 이용한 농산물중 pyribencarb와 대사물 KIE-9749의 잔류 분석법)

  • Kwon, Hyeyoung;Hong, Su-Myeong;Kim, Taek-Kyum;Kim, Hyung-Jin;Moon, Byeong-Chul;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.20 no.3
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    • pp.236-246
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    • 2016
  • The aim of this study was to develop an analytical method for the determination of pyribencarb and its metabolite KIE-9749 in agricultural commodities. The experiment was performed with a range of concentrations $0.05{\sim}2.5{\mu}g/g$ in apple, green pepper, potato, hulled rice, soybean, pear, peach, grape and cucumber. Each samples were extracted with acetone and cleaned by dichloromethane/saline water partition and purified with Florisil solid phase extraction (SPE) cartridge and aminopropyl SPE cartridge. Pyribencarb and KIE-9749 were separated and quantified by HPLC/UVD at 265nm using acetonitrile and water as mobile phase. The recoveries of pyribencarb and KIE-9749 were within 78.3~108.4% and 73.9~113.7% with RSD below 12.2% and 15.0%, respectively. The limits of quantification (LOQ) were both $0.05{\mu}g/g$. LC/ESI-MS/MS was optimized for confirmation of residue identity.

Heat Integration and Economic Analysis of Dry Flue Gas Recirculation in a 500 MWe Oxy-coal Circulating Fluidized-bed (CFB) Power Plant with Ultra-supercritical Steam Cycle (순환 유동층 보일러와 초초임계 증기 사이클을 이용한 500 MWe급 순산소 화력발전소의 건식 재순환 흐름의 열 교환 및 경제성 분석)

  • Kim, Semie;Lim, Young-Il
    • Korean Chemical Engineering Research
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    • v.59 no.1
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    • pp.60-67
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    • 2021
  • This study presented techno-economic analysis of a 500 MWe oxy-coal power plant with CO2 capture. The power plant included a circulating fluidized-bed (CFB), ultra-supercritical steam turbine, flue gas conditioning (FGC), air separation unit (ASU), and CO2 processing unit (CPU). The dry flue gas recirculation (FGR) was used to control the combustion temperature of CFB. One FGR heat exchanger, one heat exchanger for N2 stream exiting ASU, and a heat recovery from CPU compressor were considered to enhance heat efficiency. The decrease in the temperature difference (ΔT) of the FGR heat exchanger that means the increase in heat recovery from flue gas enhanced the electricity and exergy efficiencies. The annual cost including the FGR heat exchanger and FGC cooling water was minimized at ΔT = 10 ℃, where the electricity efficiency, total capital cost, total production cost, and return on investment were 39%, 1371 M$, 90 M$, and 7%/y, respectively.

Hyperparameter Optimization and Data Augmentation of Artificial Neural Networks for Prediction of Ammonia Emission Amount from Field-applied Manure (토양에 살포된 축산 분뇨로부터 암모니아 방출량 예측을 위한 인공신경망의 초매개변수 최적화와 데이터 증식)

  • Pyeong-Gon Jung;Young-Il Lim
    • Korean Chemical Engineering Research
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    • v.61 no.1
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    • pp.123-141
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    • 2023
  • A sufficient amount of data with quality is needed for training artificial neural networks (ANNs). However, developing ANN models with a small amount of data often appears in engineering fields. This paper presented an ANN model to improve prediction performance of the ammonia emission amount with 83 data. The ammonia emission rate included eleven inputs and two outputs (maximum ammonia loss, Nmax and time to reach half of Nmax, Km). Categorical input variables were transformed into multi-dimensional equal-distance variables, and 13 data were added into 66 training data using a generative adversarial network. Hyperparameters (number of layers, number of neurons, and activation function) of ANN were optimized using Gaussian process. Using 17 test data, the previous ANN model (Lim et al., 2007) showed the mean absolute error (MAE) of Km and Nmax to 0.0668 and 0.1860, respectively. The present ANN outperformed the previous model, reducing MAE by 38% and 56%.

The development of a fully automated homemade system for [11C] acetate synthesis using an open source PLC

  • Kang, Se Hun;Hong, Sung Tack;Park, Kwangseo;Kim, Seok-ki
    • Journal of Radiopharmaceuticals and Molecular Probes
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    • v.2 no.2
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    • pp.103-107
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    • 2016
  • Solid phase extraction (SPE) purification method is the efficient and well-known tool for automated [$^{11}C$]acetate synthesis. A fully automated homemade module adopting the SPE method and 'pinch' valves was developed very economically with a universal interface board, a relay card and an open source programmable logic controller. The radiochemical yield of the optimized [$^{11}C$]acetate synthesis by this system was $58.8{\pm}2.1%$ (n=10, decay-corrected) from $15.5{\pm}0.19GBq$ of $[^{11}C]CO_2$ as starting activity, and total synthetic time was 15 minutes. HPLC analysis showed its high radiochemical purity as $97.4{\pm}1.1%$ without possible by-products.

Determination of Cholesterol in Milk and Dairy Products by High-Performance Liquid Chromatography

  • Oh, H.I.;Shin, T.S.;Chang, E.J.
    • Asian-Australasian Journal of Animal Sciences
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    • v.14 no.10
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    • pp.1465-1469
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    • 2001
  • A sensitive high-performance liquid chromatographic method was developed to determine the content of cholesterol in milk and dairy products. To optimize separation of cholesterol, mobile phases including acetonitrile:2-propanol (8:1, v/v), acetonitrile:methanol (3:1, v/v), and acetonitrile:methanoI:2-propanol (7:3: I, v/v/v) were compared. Acetonitrile/methanol/2-propanol was superior to the other mobile phase systems for separating cholesterol. Liquid-liquid extraction (LLE) of cholesterol was simplified using a non-polar solvent, hexane, to remove interfering compounds, and had an excellent recovery $(100{\pm}1.0%)$ of cholesterol. A solid phase extraction (SPE) method using Sep-pak $C_{18}$ was developed and compared with LLE. The SPE method was rapid and highly reproducible. Both extraction methods were useful when used in combination with saponification of esterified cholesterol to facilitate total cholesterol determination. The detection limit of cholesterol was $0.01{\mu}g$. The newly developed HPLC method was rapid, simple, and accurate, and has advantages over the many methods commonly used.

Simultaneous Liquid Chromatography Tandem Mass Spectrometric Determination of 35 Prohibited Substances in Equine Plasma for Doping Control

  • Kwak, Young Beom;Yu, Jundong;Yoo, Hye Hyun
    • Mass Spectrometry Letters
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    • v.13 no.4
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    • pp.158-165
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    • 2022
  • Many therapeutic class drugs such as beta-blocker, corticosteroids, NSAIDs, etc are prohibited substances in the horse racing industry. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology makes it possible to isolate drugs from interference, enables various drug analyses in complex biological samples due to its sensitive sensitivity, and has been successfully applied to doping control. In this paper, we describe a rapid and sensitive method based on solid-phase extraction (SPE) using solid phase cartridge and LC-MS/MS to screen for different class's 35 drug targets in equine plasma. Plasma samples were pretreated by SPE with the NEXUS cartridge consisted non-polar carbon resin and minimum buffer solvent. Chromatographic separation of the analytes was performed on ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 ㎛). The elution gradient was conducted with 5 mM ammonium formate (pH 3.0) in distilled water and 0.1% formic acid in acetonitrile at a flow rate of 0.25 mL/min. The selected reaction monitoring (SRM) mode was used for drug screening with multiple transitions in the positive ionization mode. The specificity, limit of detection, recovery, and stability was evaluated for validation. The method was found to be sensitive and reproducible for drug screening. The method was applied to plasma sample analysis for the proficiency test from the Association of Racing Chemist.

Variation of AC Impedance of the $TiS_2$ Composite/SPE/Li Cell with Cycling ($TiS_2$ Composite/SPE/Li Cell의 충방전에 따른 AC 임피던스의 변화)

  • Kim, J.U.;Gu, H.B.;Moon, S.I.;Yun, M.S.
    • Proceedings of the KIEE Conference
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    • 1995.07c
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    • pp.1034-1038
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    • 1995
  • The purpose of this study is to research and develop $TiS_2$ composite cathode for lithium polymer battery(LPB). $TiS_2$ electrode represent a class of insertion positive electrode used in Li secondary batteries. In this study, we investigated preparation of $TiS_2$ composite cathode and AC impedance response of $TiS_2$ composite/SPE/Li cells as a function of state of charge(SOC) and cycling. The resistance of B type cell using $TiS_2PEO_8LiClO_4PC_5EC_5$ composite cathode was lower than that of A type cell using $TiS_2PEO$ composite cathode. The cell resistance of B type cell is high for the first few percent discharge, decreases for midium discharge and then increases again toward the end of discharge. We believe the magnitude of the cell resistance is dominated by passivation layer impedance and small cathode resistance. AC impedance results indicate that the cell internal resistance increase with cycling, and this is attributed to change of passivation layer impedance with cycling. The passivation layer resistance($R_f$) of B type cell decreases for the 2nd cycling and then increases again with cycling. Redox coulombic efficiency of B type cell was about 141% at 1st cycle and 100% at 12th cycle. Also, $TiS_2$ specific capacity was 115 mAh/g at 12 cycle.

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The Extraction and Derivatization of Organotins in Water Sample by Gas Chromatograph/Mass Spectrometer (기체크로마토그래프/질량분석기에 의한 물시료 중 Organotin의 추출 및 유도체 반응에 관한 연구)

  • Hong, Jee-Eun;Lee, Kang-Jin;Pyo, Hee Soo;Park, Song-Ja;Lee, Won
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.636-645
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    • 2000
  • A method is described for the determination of organotins in water samples by GC/MS. Optimized derivatization methods for ethylation and hydrogenation of organotins were surveyed according to various reaction conditions such as time, pH and concentration of reagents. The organotins were extracted with n-hexane in presence of 0.1% tropolone and hydrogenated with sodium borohydride. Extraction recoveries of organotins with hydrogenation were in the range of 61-112%. After ethylation, organotins in water samples were extracted by liquid-liquid extraction (LLE) and solid-phase extraction (SPE). Using LLE, extraction recoveries were in the range of 74-113%. The recoveries ranged from 61-97% in the case of SPE with styrene-divinylbenzene copolymers. Method detection limits of hydrogenated and ethylated organotins ranged from 0.05 to 0.5 ng/ml and from 0.02 to 0.05 ng/ml, respectively.

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Alternative Sample Preparation Techniques in Gas Chromatographic-Mass Spectrometric Analysis of Urinary Androgenic Steroids

  • Cho, Young-Dae;Choi, Man-Ho
    • Bulletin of the Korean Chemical Society
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    • v.27 no.9
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    • pp.1315-1322
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    • 2006
  • The following study describes the gas chromatography-mass spectrometry (GC-MS) based screening and confirmation analysis of urinary androgenic steroids. Four commercially available solid-phase extraction (SPE) cartridges, Serdolit PAD-1, Sep-pak $C_{18}$, amino-propyl, and Oasis HLB, and three different extractive organic solvents, diethyl ether, methyl tert-butyl ether (MTBE), and n-pentane, were tested for sample preparation. Overall, Oasis HLB combined with MTBE extraction provided the highest recoveries in 39 of 46 total androgenic steroids examined and it showed a good extraction yield (>82.1%) for polar steroids, such as metabolites of fluoxymesterone, oxandrolone, and stanozolol, which gave a poor recovery in both n-pentane (9.2-64.3%) and diethyl ether (22.2-73.6%) extractions. All SPE sorbents tested showed potential, because they were efficient in extraction for most or selective steroids. When applied to positive urine samples based on the results obtained, the present method allowed selective and sensitive analysis for detection of urinary androgenic steroids. The experiments showed that the high-resolution MS method is clearly more efficient than the low-resolution MS technique for the detection of many urinary steroids. However, comprehensive sample clean-up procedures also might be needed especially in confirmation analysis to increase detectability.