• Title/Summary/Keyword: Method detection limits

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Measurement of Carbonyl Compounds in Ambient Air using a DNPH Cartridge coupled with HPLC Method (DNPH 카트리지와 HPLC를 이용한 대기 중 카르보닐화합물의 농도측정)

  • 황윤정;박상곤;백성옥
    • Journal of Korean Society for Atmospheric Environment
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    • v.12 no.2
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    • pp.199-209
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    • 1996
  • The purpose of this study is to evaluate analytical method for the measurement of carbonyl compounds and to apply method to the measurement of indoor and outdoor concentrations of these compounds at public facilities. For sampling, 2.4-dinitrophenylhydrazine (DNPH) coated DNPH-Silica cartridges were uwed in this study. DNPH reacts with carbonyl compounds and forms carbonyl hydrazone, The carbonyl hydarzone was eluted from the cartridge with acetonitrile and analyzed by reverse-phase HPLC with UV detection. Possible interference caused by ozone during sampling was eliminated by using KI trap commected in series with the DNPH-Silica cartridge. A number of experimental studies were undertaken to evaluate and validate the analytical method, including collection efficiency, recovery, repeatability, lower limits of detection, and effect of ozone. Indoor and outdoor measurements of carbonyl compounds were simultaneously carried out at 14 public facilities located in Taegu city and Kyungsan city from June to July, 1995. Except for one or two sites, the indoor concentrations were found to be higher than the outdoor concentrations for carbonyl compounds. And the concentrations of carbonyl compounds measured in the morning and afternoon were showed higher than the concentrations measured in the evening.

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Chiral Purity Test of Bevantolol by Capillaryelectrophoresis and High Performance Liquid Chromatography

  • Long, Pham Hai;Trung, Tran Quoc;Oh, Joung-Won;Kim, Kyeong-Ho
    • Archives of Pharmacal Research
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    • v.29 no.9
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    • pp.808-813
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    • 2006
  • Two methods for the chiral purity determination of bevantolol were developed, namely capillary electrophoresis (CE) using carboxymethyl-${\beta}$-cyclodextrin (CM-${\beta}$-CD) as a chiral selector and high-perfomance liquid chromatography (HPLC) using a chiral stationary phase. In the HPLC method, the separation of bevantolol enantiomers was performed on a Chiralpak AD-H column by isocratic elution with n-hexane-ethanol-diethylamine (10:90:0.1, v/v/v) as mobile phase. In the CE method, bevantolol enantiomers were separated on an uncoated fused silica capillary with 50 mM amonium phosphate dibasic adjusted to a pH 6.5 with phosphoric acid containing 15 mM CM-${\beta}$-CD as running buffer. Validation data such as linearity, recovery, detection limit, and precision of the two methods are presented. The detection limits of S-(-)-bevantolol were 0.1% and 0.05% for CE and HPLC method, respectively and R-(+)-bevantolol were 0.15% and 0.05% for CE and HPLC method, respectively. There was generally good agreement between the HPLC and CE results.

Simultaneous analysis of β-lactam antibiotics and β-blockers by LC-MS/MS (LC-MS/MS를 이용한 베타락탐계 항생제와 베타차단제의 동시분석)

  • Son, Bo-young;Kim, Jun-il;An, Chi-hwa;Lee, Su-won;Kim, Bogsoon;Chung, Deukmo
    • Analytical Science and Technology
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    • v.29 no.4
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    • pp.179-185
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    • 2016
  • An effective analytical method has been developed for the determination of β-blockers(atenolol, metoprolol and propranolol) and 6 β-lactams(amoxicillin, penicillin G, cefaclor, cefadroxil, cephalexin and cephradine) in water samples using two different cartridges. The samples were extracted by solid-phase extraction (SPE) with the usage of polymeric hydrophile-lipophile balance(HLB cartridges) and strong cation-exchange mixed-mode polymeric sorbent (MCX cartridges). A XDB-C18 column(1.8 μm; 3.0 mm × 100 mm) was used for the sufficient chromatographic resolution. The calibration curves showed good linearity with high correlation coefficients (>0.995). The method detection limits (MDL) and the limits of quantification(LOQ) were from 1.1 to 3.9 ng/L and from 5 to 13 ng/L, respectively. The method was applied for the determination of the target compounds in tributaries and raw water of the Han River and these were found at N.D. to 0.209 μg/L.

Medical Image Processing with Local Variati on of the Image Quality (화질의 국소적 변화를 고려한 의용화상처리)

  • 홍승홍
    • Journal of the Korean Institute of Telematics and Electronics
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    • v.12 no.1
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    • pp.1-6
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    • 1975
  • The boundary has been one of the most important information in radiographic images and the degrees of difficulty involved varies greatly with the quality of the picture. These Buantifications are the means to diagnoses. The purpose of this paper is to quantify intensity variation and the threshold decision which is based on statistical principles and is developed to detect limits in liver scintigrams the entire picture is devide4 into 64 small regions. The kurtosis and variances for each smal region are used as indications to select the histograms the thresholds are computed according to the method o(maximum likelihood which minimizes the probability o( misclassification. Therefore Ive have demonstrated the applicability of the boundary detection and proved good agreement with human recognition, and we can use it for the diagnosis data of liver disease.

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Simultaneous Determination of the Flavonoids and Limonoids in Citrus junos Seed Shells Using a UPLC-DAD-ESI/MS

  • Jo, Ara;Shin, Ji hun;Song, Hwa young;Lee, Ye Eun;Jeong, Da Eun;Oh, Sung Hwa;Mun, Myung Jae;Lee, Mina
    • Natural Product Sciences
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    • v.26 no.1
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    • pp.64-70
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    • 2020
  • Citrus junos seeds (CS) have been traditionally used for the treatment of cancer and neuralgia. They are also used to manufacture edible oil and cosmetic perfume. A large amount of CS shells without oil (CSS) are discarded after the oil in CS is used as foods or herbal remedy. To efficiently utilize CSS as a by-products, it needs to be studied through chemical analysis. Therefore, we developed an ultra-performance liquid chromatography (UPLC)-diode array detection (DAD) method for simultaneous determination and quantitative analysis of five components (two flavonoids and threes limonoids) in CSS. A Waters Acquity UPLC HSS T3 column C18 (2.1 × 100 mm, 1.8 ㎛) was used for this separation. It was maintained at 40 ℃. The mobile phase used for the analysis was distilled water and acetonitrile with gradient elution. To identify the quantity of the five components, a mass spectrometer (MS) with an electrospray ionization (ESI) source was used. The regression equation showed great linearity, with correlation coefficient ≥ 0.9912. Limits of detection (LOD) and limits of quantification (LOQ) of the five compounds were 0.09 - 0.13 and 0.26 - 0.38 ㎍/mL, respectively. Recoveries of extraction ranged from 97.45% to 101.91%. Relative standard deviation (RSD) values of intra- and inter-day precision were 0.06 - 1.15% and 0.19 - 0.25%, respectively. This UPLC-DAD method can be validated to simultaneously analyze quantities of marker flavonoids and limonoids in CSS.

Development of an analytical method for the determination of dl-methylephedrine hydrochloride in porcine muscle using liquid chromatography-tandem mass spectrometry (LC-MS/MS를 이용한 돼지 근육조직 중 dl-methylephedrine hydrochloride의 잔류 분석법 개발)

  • Chae, Won-Seok;Kim, Suk;Lee, Hu-Jang
    • Korean Journal of Veterinary Research
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    • v.60 no.4
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    • pp.209-213
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    • 2020
  • This study examined the residue of dl-methylephedrine hydrochloride (MEP) on the muscle of pigs administered orally with MEP 12 g/ton feed for seven consecutive days. Twenty healthy cross swine were administered MEP. Four treated animals were selected arbitrarily to be sacrificed at 1, 2, 3, 4, and 5 days after treatment. MEP residue concentrations in the muscle were determined by liquid chromatography coupled with tandem mass spectrometry. The drug was extracted from muscle samples using 10 mM ammonium formate in acetonitrile followed by clean-up with n-hexane. The analyte was separated on an XBridgeTM hydrophilic interaction liquid chromatography column using 10 mM ammonium formate in deionized distilled water and acetonitrile. The correlation coefficient (R2) of the calibration curve was 0.9974, and the limits of detection and quantification were 0.05 and 0.15 ㎍/kg, respectively. The recoveries at three spiking levels were 94.5-101.2%, and the relative Standard Deviations was less than 4.06%. In the MEP-treated group, MEP residues on one day post-treatment were below the maximum residue limit in the muscle. The developed method is sensitive and reliable for the detection of MEP in porcine muscle tissues. Furthermore, it exhibits low quantification limits for animal-derived food products destined for human consumption.

Label-free and sensitive detection of purine catabolites in complex solutions by surface-enhanced raman spectroscopy

  • Davaa-Ochir, Batmend;Ansah, Iris Baffour;Park, Sung Gyu;Kim, Dong-Ho
    • Journal of the Korean institute of surface engineering
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    • v.55 no.6
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    • pp.342-352
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    • 2022
  • Purine catabolite screening enables reliable diagnosis of certain diseases. In this regard, the development of a facile detection strategy with high sensitivity and selectivity is demanded for point-of-care applications. In this work, the simultaneous detection of uric acid (UA), xanthine (XA), and hypoxanthine (HX) was carried out as model purine catabolites by surface-enhanced Raman Spectroscopy (SERS). The detection assay was conducted by employing high-aspect ratio Au nanopillar substrates coupled with in-situ Au electrodeposition on the substrates. The additional modification of the Au nanopillar substrates via electrodeposition was found to be an effective method to encapsulate molecules in solution into nanogaps of growing Au films that increase metal-molecule contact and improve substrate's sensitivity and selectivity. In complex solutions, the approach facilitated ternary identification of UA, XA, and HX down to concentration limits of 4.33 𝜇M, 0.71 𝜇M, and 0.22 𝜇M, respectively, which are comparable to their existing levels in normal human physiology. These results demonstrate that the proposed platform is reliable for practical point-of-care analysis of biofluids where solution matrix effects greatly reduce selectivity and sensitivity for rapid on-site disease diagnosis.

Islanding Detection Method for Grid-connected PV System using Automatic Phase-shift (자동 위상 이동을 이용한 계통 연계형 태양광 발전 시스템의 고립운전 검출기법)

  • Yun, Jung-Hyeok;Choi, Jong-Woo;So, Jung-Hun;Yu, Gwon-Jong;Kim, Heung-Geun
    • The Transactions of the Korean Institute of Power Electronics
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    • v.12 no.2
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    • pp.107-114
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    • 2007
  • Islanding of PV systems occurs when the utility grid is removed but the PV systems continue to operate and provide power to local loads. Islanding is one of the serious problems in an electric power system connected with dispersed power sources. This can present safety hazards and the possibility of damage to other electric equipments. In the passive method, the voltage and frequency of PCC are measured and it determines islanding phenomena if their values excess the allowed limits. If the real and reactive power of RLC load and those of the PV system are closely matched, islanding phenomena can't be detected by the passive methods. Several active methods were proposed to detect islanding operation in the region where the passive method can not detect it. The most effective method is SFS method which was suggested by Sandia National Laboratory. In this paper, a new islanding detection method using automatic phase-shift is proposed and its validity is verified through the simulation and experimental results.

An HPLC-UV-based quantitative analytical method for Chrysanthemum morifolium: development, validation, and application

  • Jung, Dasom;Jin, Yan;Kang, Seulgi;Lee, Heesoo;Park, Keunbae;Li, Ke;Kim, Jin Hak;Geum, Jeong Ho;Lee, Jeongmi
    • Analytical Science and Technology
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    • v.32 no.4
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    • pp.139-146
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    • 2019
  • A simple and reliable analytical method based on high-performance liquid chromatography-ultraviolet detection was established for the analysis of the flowers of Chrysanthemum morifolium (CM). Luteolin-7-O-glucoside (LU7G) was chosen as a target analyte considering its content, availability, and ease of analysis. Chromatographic separation of LU7G was achieved using a Phenomenex Gemini $C_{18}$ column ($250{\times}4.6mm$, $5{\mu}m$) run with a mobile phase consisting of 0.5 % acetic acid in water and 0.5 % acetic acid in acetonitrile at a flow rate of $1.0mL\;min^{-1}$. The detection wavelength and column temperature were set at 350 nm and $40^{\circ}C$, respectively. Method validation was performed according to the AOAC guidelines and the method was specific, linear ($R^2=0.9991$ for $50-300{\mu}g\;mL^{-1}$), precise (${\leq}3.91%$RSD), and accurate (100.1-105.7 %). The limits of detection and quantification were 3.62 and $10.96{\mu}g\;mL^{-1}$, respectively. The established method was successfully applied to determine the contents of LU7G in various batches of bulk CM extracts and labscale CM extract. The developed method is a readily applicable method for the quality assessment of CM and its related products.

Quantitative Determination of Flavonoids from Stems of Spatholobus suberectus

  • Park, Jinseon;Park, So Yeon;Shim, Sang Hee
    • Natural Product Sciences
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    • v.19 no.2
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    • pp.145-149
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    • 2013
  • A simple reversed phase HPLC method was established for quantitative determination of liquiritigenin (1), genistein (2), isoliquiritigenin (3), and 7-hydroxyflavanone (4) from stems of Spatholobus suberectus Dunn (Leguminosae) using a binary gradient of $H_2O$ and MeOH as a mobile phase with UV detection at 280 nm. All calibration curves showed good linear regression ($r^2$ > 0.998) within test ranges. The detection limits of the four compounds were $0.43{\sim}1.63{\mu}g/mL$. The contents of four flavonoids (1 - 4) from the stem of S. suberectus were 6.54 mg/g, 1.66 mg/g, 6.65 mg/g, and 1.93 mg/g, respectively.