• Title/Summary/Keyword: Recoveries

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Quantification of Globotriaosylsphingosine in Urine using UPLC-ESI-MS/MS; Application for Screening Fabry Disease (파브리병의 신속한 진단을 위한 소변 중 Globotriaosylsphingosine의 UPLC-ESI-MS/MS 분석법)

  • Yoon, Hye-Ran
    • YAKHAK HOEJI
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    • v.60 no.1
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    • pp.15-20
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    • 2016
  • Globotriaosylsphingosine (lyso Gb3) is considered as one of the biomarkers for Fabry disease. A rapid and simple UPLC-MS/MS method was developed for the determination of reliable biomarker, lyso Gb3. Total analytical procedure takes only 15 min including sample preparation and MS/MS analysis. Limit of detection was 0.85 ng/ml (S/N=3). The calibration curve was linear over the range of 2.0~400.0 ng/ml ($R^2=0.9999$). Inter-day and intra-day assay accuracy were 93.4~100.6% (RSD, 0.6~6.0%) and 97.5~100.7% (RSD, 3.6~5.2%). Absolute recoveries of 97.6~98.6 showed excellence of a new analytical method. The method was applied to human and mice urines, proved the suitability for the quantification of lyso-Gb3 for screening, diagnosis and therapeutic monitoring of Fabry disease patients.

Determination of Icing Inhibitors (Ethylene Glycol Monomethyl Ether and Diethylene Glycol Monomethyl Ether) in Ground Water by Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang;Jung, Dong-Gyun
    • Bulletin of the Korean Chemical Society
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    • v.25 no.6
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    • pp.806-808
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    • 2004
  • A gas chromatography/mass spectrometric assay method has been developed for the simultaneous determination of icing inhibitors, ethylene glycol monomethyl ether and diethylene glycol monomethyl ether in ground water contaminated with JP-8. Ethylene glycol monobutyl ether and ethylene glycol monoethyl ether were used as the internal standard and surrogate, respectively. 100 mL of ground water was extracted twice with 20 mL of methylene chloride. The extract was concentrated to dryness, dissolved with 100 ${\mu}$L of methanol and analyzed by GC-MS (SIM). The use of an Innowax column gave the peaks good chromatographic properties, and the extraction of these compounds from samples gave recoveries of about 50% with small variations. The method detection limits of the target compounds were in a range of 0.5-0.8 ng/mL in ground water.

Development of Alternative Assay Method without Hazardous Reagent, Chloroform for Urazamide Tablets in Korean Pharmaceutical Codex (우라자미드 정의 유해시약 대체 시험법의 개발)

  • Lee, Yoo Rim;Kim, Hyun Ji;Seo, Narae;Kim, Kyeong Ho
    • YAKHAK HOEJI
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    • v.58 no.2
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    • pp.125-128
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    • 2014
  • We developed an alternative assay method without hazardous reagent of chloroform for urazamide tablets in Korean Pharmaceutical Codex. The HPLC analytical method was validated by system suitability, linearity, precision, accuracy and robustness. The linearity of the calibration curves in the desired concentration range is good ($r^2$ >0.999). Precision was obtained less than RSD 1.17%. Accuracy was obtained with recoveries in range of 98.12% and 99.47%. The developed assay could be expected to become valuable tools for revising the Korean Pharmaceutical Codex.

Influence of Aging Media and Filler System on Recovery Behaviors of Natural Rubber Composites (노화 매질과 충진 시스템이 천연고무 복합체의 회복 거동에 미치는 영향)

  • Choi, Sung-Seen;Kim, Ok-Bae
    • Elastomers and Composites
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    • v.47 no.2
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    • pp.156-161
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    • 2012
  • Difference in recovery behaviors from the circular deformation of natural rubber (NR) composites aged in air and distilled water, respectively were investigated. Recoveries of the samples aged in air were larger than those of the samples aged in distilled water. Recovery rates of the samples reinforced with filler were faster than those of the unreinforced ones. Recovery rates of the carbon black-filled samples were faster than those of the silica-filled ones. Difference in the recovery behaviors according to the aging media can be explained by the crosslinking density changes and the annealing effect.

On-line SPE-HPLC Method using Alumina Filtering to Selectively Extract Phenolic Compounds from Environmental Water

  • Lee, Sung-Kwang
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3755-3759
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    • 2010
  • A on-line SPE (solid phase extraction)-HPLC preconcentration method was developed for the determination of phenolic compounds at trace levels in environmental water sample. XAD-4 and Dowex 1-X8 were used as sorbent in the on-line SPE-HPLC method for the selective enrichment of nine phenolic compounds, which are included in the priority pollutants list of the US EPA. Also alumina prefiltering considerably reduced the amount of interfering peaks due to humic substances that could accumulated due to the preconcentration step and prevent quantification of polar phenolic compounds in environmental water samples. This method was used to determine the phenolic compounds in tap and river water and superiority to the US EPA 625 method in its enrichment factor, pretreatment time, recoveries, and detection limit. The limits of detection were in the range of $0.3-0.9\;{\mu}g/L$ in tap water sample.

Determination of Mefenamic Acid in Human Urine by Means of Two Spectroscopic Methods by Using Cloud Point Extraction Methodology as a Tool for Treatment of Samples

  • Tabrizi, Ahad Bavili
    • Bulletin of the Korean Chemical Society
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    • v.27 no.11
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    • pp.1780-1784
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    • 2006
  • Cloud point extraction was used to extract mefenamic acid (MF) from human urine, and spectrofluorimetry and spectrophotometry were used to analyze extracted MF. The variables affecting extraction and phase separation, i.e. HCl and Triton X-114 concentration, temperature and time of equilibration, were optimized. Under the experimental conditions used the limit of detection for extraction of 25 mL of sample was 0.006 and 0.045 mg $L^{-1}$, with relative standard deviations of 2.52 and 1.45% (n = 5) for spectrofluorimetric or spectrophotometric methods, respectively. Good recoveries in the range of 95-107% were obtained for spiked samples. The proposed methods were applied to the determination of MF in human urine.

Determination of N. N-dimethylaniline in penicillins by GC-MS

  • Choi, Jung-Kap;Park, Man-Ki
    • Archives of Pharmacal Research
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    • v.4 no.2
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    • pp.85-90
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    • 1981
  • A quantitative GC-MS spectrometric assay was used for the determination of residual N, N-dimethylaniline as a contaminant in commercial penicillin derivatives from various sources. The assay utilizes selective ion focusing to monitor in a GC effluent the molecular ions of DMA generated by electron impact ionization. This method includes dissolution of the sample in alkaline solution, extraction of organic base with cyclohexane and injection into GC-MS with a 3% OV-17 column. Levels of 50 ppb of DMA were easily measured with a coeffecient of varation less than 5 % and recoveries from spiked samples exceeded 97 %. The results of the determinations of DMA in various commercial penicillins were relatively free of this contaminant.

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Implementational Architecture of Learning Organizations: System Dynamic Approach to Organizational Learning, Unlearning, and Knowledge Management in Public Sector Organizations (학습조직 구현방안: 공공조직의 조직학습 및 폐기학습, 지식관리를 중심으로 한 시스템 다이내믹 접근)

  • Hong, Min Kee
    • Korean System Dynamics Review
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    • v.17 no.3
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    • pp.51-90
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    • 2016
  • Learning is naturally embedded in organizational ongoing-processes and routines. Recent many research models of organizational failure ignore how failing masks breakdowns and recoveries of organization-embedded learning as a naturally occurring process. Organizational learning is the platform in tandem with base-modules of organization in this point. Organizations learn and unlearn while they acquire, discard, and forget organizational experiences or knowledges. These processes in public sector organizations are different from learning behaviors in private sector. This study expects to explore architectural components of learning organization in public sector, focusing on distinct characteristics of public organizations, and to implement learning model based on system thinking(system dynamic) approach.

Determination of Monocrotophos Residues by HPLC

  • Lee, Young-Deuk;Kwon, Chan-Hyeok
    • Korean Journal of Environmental Agriculture
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    • v.23 no.4
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    • pp.245-250
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    • 2004
  • An analytical method was developed to determine monocrotophos residues in apple, citrus, and soil using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. Monocrotophos was extracted with acetone from apple, citrus and moist soil samples. The extract was concentrated, added with saline water, and subjected to n-hexane washing to remove nonpolar co-extractives. Dichloromethane partition was then followed to recover monocrotophos from the aqueous phase. Silica gel column chromatography was employed to further purify the extract prior to HPLC determination. Reverse-phase HPLC using an oct-adecylsilyl column was successfully applied to separate and quantitate the monocrotophos residue in sample extracts at the wavelength of 230 nm. Overall recoveries of monocrotophos from fortified samples averaged $95.3{\pm}2.1%$ (n=6), $970{\pm}0.7%$ (n=6), and $92.8{\pm}4.3%$ (n=12) for apple, citrus, and soil, respectively. The proposed method was quite reproducible and sensitive enough to replace the troublesome gas-liquid chromatographic analysis for monocrotophos residues.

Determination of Heavy Metal in Polyurethane by New Digestion Method and ICP-AES (새로운 전처리 방법과 ICP-AES에 의한 폴리우레탄 중의 중금속 분석)

  • Lim, Heon-Sung;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.363-367
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    • 2004
  • A simple and convenient digestion method was developed for the determination of heavy metal in polyurethane sample using only nitric acid in open system without heating. This digestion method had prevented loss of volatile elements of Hg and As and reduced the pretreatment time for the sample digestion. The detection limit is lowered over 10 times than that of microwave digestion method. Recoveries in polyurethane material were 108% for As, 96 ~ 99% for Hg, 102 ~ 103% for Cr, 98 ~ 102% for Pb, 86 ~ 90% for Cd, and 90 ~ 93% for Cu.