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Simultaneous Analysis of 17 Organophosphorous Pesticides in Blood by Automated Head Space-SPME GC/MS (HS-SPME-GC/MS에 의한 혈액중 17종 유기인계 농약의 동시분석법)

  • Rhee, Jong-Sook;Jung, Jin-Mi;Lee, Han-Sun;Yeom, Hye-Sun;Lee, Sang-Ki;Park, Yoo-Sin;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.54 no.6
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    • pp.429-440
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    • 2010
  • HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 ${\mu}m$ polyacrylate), pH effect (0.5 N HCl), salt effect ($Na_2SO_4$, 0.2 g; 20%), headspace incubation temperature ($80^{\circ}C$), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l ($r^2$=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.

Simultaneous Determination of C22-C26 Very Long - Chain Fatty Acids Following tert-Butyldimethylsilyl Derivatization by Stable Isotope GC- MS for the Screening of Adrenoleucodystrophy

  • Yoon, Hye-Ran
    • Biomolecules & Therapeutics
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    • v.15 no.4
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    • pp.266-272
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    • 2007
  • A rapid analytical method was developed to quantify very long-chain fatty acids (VLCFAs, C22:0, C24:0, C26:0) in human plasma with good sensitivity and specificity using tert-butyldimethylsilyl (TBDMS) derivatization and stable isotope GC-MS selective ion monitoring (GC-MS/SIM). Two-hundred and fifty ${\mu}L$ of plasma was fortified with deuterated stable isotope internal standards (d3-C22:0, d3-C24:0, d3-C26:0) and standard mixtures of chloroform and methanol, and then extracted with hexane and acetonitrile. To upper layer of liquid-liquid-extraction, N-(t-Butyldimethylsilyl)-N-methyltrifluoroacetamide was added and then heated to $60^{\circ}C$ for 30 min to produce the TBDMS derivatives. Derivatives of VLCFAs were analyzed by GC-MS/SIM. Calibration curves showed a linear relationship for the target compounds in the concentration range of $10^{-4}{\sim}2{\times}10^3\;{\mu}g/mL$ with the correlation coefficient ranging from 0.996 to 0.999. The limit of quantification for the plasma was $10^{-4}{\sim}2{\times}10^{-4}\;{\mu}g/mL$ (S/N=3). When applied to the plasma specimens of patients with peroxisomal disorder, X-linked adrenoleucodystropy (ALD, Mckusick 202370), the method clearly differentiated normal subjects from ALD patients. The C24:0/C22:0 and C26:0/C22:0 ratios were significantly elevated in the plasma of patients with X-linked ALD compared to normal subjects. The new developed method might be useful for a rapid and sensitive diagnosis of X-linked ALD and other peroxisomal disorders.

The relationship between disability and clinical outcomes in maintenance dialysis patients

  • Kang, Seok Hui;Do, Jun Young;Kim, Jun Chul
    • Journal of Yeungnam Medical Science
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    • v.38 no.2
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    • pp.127-135
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    • 2021
  • Background: Dialysis patients are prone to having disabilities. We aimed to evaluate the association between disability and various clinical outcomes in Korean dialysis patients. Methods: This study consisted of 1,615 dialysis patients from 27 centers. We evaluated disability by using four questions on the activities of daily living (ADLs) concerning whether help was needed for feeding, dressing/undressing, getting in/out of bed, or taking a bath/shower. We divided the patients into three groups: no disability (Non-D, none of the four ADL domains required help; n=1,312), mild disability (Mild-D, one ADL domain required some/full help; n=163), or moderate to severe disability (MS-D, two or more ADL domains required some/full help; n=140). We evaluated falls, frailty, health-related quality of life (HRQoL), mortality, and hospitalization. Results: The numbers of participants with a fall during the last 1 year were 199 (15.2%), 42 (25.8%), and 44 (31.4%) in the Non-D, Mild-D, and MS-D groups, respectively (p<0.001). The numbers of participants with frailty in the Non-D, Mild-D, and MS-D groups were 381 (29.0%), 84 (51.5%), and 93 (66.4%), respectively (p<0.001). In both univariate and multivariate analyses, the physical component scale and mental component scale scores decreased as the grade of disability increased (p<0.001 for both scores). Hospitalization-free survival rate at 500 days was 64.2%, 56.7%, and 51.1% in the Non-D, Mild-D, and MS-D, respectively (p=0.001 for trend). Patient survival rate at 500 days was 95.3%, 89.5%, and 92.3% in the Non-D, Mild-D, and MS-D, respectively (p=0.005 for trend). Conclusion: Disability was associated with falls, frailty, HRQoL scales, and survival trends in Korean dialysis patients.

Isolation of Antimicrobial Active Substances from Chinese Gall Nut (Schlechtendalia chinensis) against Watermelon Fruit Rot Pathogens (Acidovorax avenae subsp. Citrulli) (오배자(Schlechtendalia chinensis)로부터 수박 과실썩음병 병원균(Acidovorax avenae subsp. citrulli)에 대한 항균 활성물질 탐색)

  • Kim, Hyun-Woo;Choi, Yong-Hwa
    • Korean Journal of Organic Agriculture
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    • v.23 no.2
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    • pp.323-334
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    • 2015
  • This study was conducted to develop environment-friendly agricultural products with anti-microbial activity against Acidovorax avenae subsp. citrulli as a pathogen of bacterial fruit blotch in cucurbit. Schlechtendalia chinensis was extracted by MeOH and solvent fraction. The hexane fraction, which showed highest value of anti-microbial activity, was analyzed by GC-MS. Each mass spectra, corresponding to each peak of chromatogram, was compared to MS database of Wiley library. As a result, myristic acid, palmitic acid and 3-n-pentadecylphenol were identified as maine compounds showing antimicrobial activity against A. avenae subsp. citrulli. Bioassay using commercial myristic acid, palmitic acid and 3-n-pentadecylphenol to test for the anti-microbial activity conformed the anti-microbial activity of potential active compounds, and myristic acid and 3-n-pentadecylphenol showed strong activity. In conclusion, myristic acid and 3-n-pentadecylphenol identified from S. chinensis were anti-microbial chemicals.

Determination of N,N-Dimethylformamide in Ambient Air Using Adsorption Sampling and Thermal Desorption with GC/MS Analysis (흡착-열탈착-GC/MS를 이용한 환경대기 중 N,N-Dimethylformamide 농도 측정)

  • Seo, Young-Kyo;Hwang, Yoon-Jung;Lee, Soon-Jin;Lee, Min-Do;Han, Jin-Seok;Baek, Sung-Ok
    • Journal of Korean Society for Atmospheric Environment
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    • v.26 no.4
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    • pp.357-366
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    • 2010
  • The purpose of this study is to evaluate a method for the measurement of N,N-Dimethylformamide (DMF) and to apply the method to the ambient air samples. For the determination of DMF together with other general VOCs (e.g., benzene, toluene, and xylenes), adsorption sampling and thermal desorption with GC/MS was used in this study. The sampling and analytical approaches tested in this study showed a good repeatability and linearity with lower detection limits of less than 0.35 ppb. Field measurements were carried out at three industrial sites (Daegu-Seongseo, Siwha and Banwall industrial complexes) and one residential site in Daegu city during a period from October 2006 to November 2008. DMF was detected in 71.8% of the total samples from the Seongseo industrial complex, well known for textile industry. In contrast, DMF was detected in only 20.4% and 12.9% of all the samples from the other two sites in Banwall and Siwha industrial complexes, respectively. This implies that sources of DMF should be strongly associated with textile industry. The mean concentration of DMF also appeared to be the highest in Seongseo site (5.95 ppb), followed by a residential site in Daegu (3.28 ppb), Banwall (0.88 ppb) and Siwha (0.55 ppb). In this study, we demonstrated the environmental significance of DMF in urban ambient air. To our knowledge, the DMF measurement introduced in this paper is the first case of an official report in Korea.

Comparison of Proton T1 and T2 Relaxation Times of Cerebral Metabolites between 1.5T and 3.0T MRI using a Phantom (모형을 이용한 1.5T와 3.0T 자기공명에서의 뇌 대사물질들의 수소 T1과 T2 이완시간의 비교)

  • Kim, Ji-Hoon;Chang, Kee-Hyun;Song, In-Chan
    • Investigative Magnetic Resonance Imaging
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    • v.12 no.1
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    • pp.20-26
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    • 2008
  • Purpose : To present the T1 and T2 relaxation times of the major cerebral metabolites at 1.5T and 3.0T and compare those between 1.5T and 3.0T. Materials and Methods : Using the phantom containing N-acetyl aspartate (NAA), Choline (Cho), and Creatine (Cr) at both 1.5T and 3.0T MRI, the T1 relaxation times were calculated from the spectral data obtained with 5000 ms repetition time (TR), 20 ms echo time (TE), and 11 different mixing time (TM)s using STEAM (STimulated Echo-Acquisition Mode) method. The T2 relaxation times were obtained from the spectral data obtained with 3000 ms TR and 5 different TEs using PRESS (Point-RESolved Spectroscopy) method. The T1 and T2 relaxation times obtained at 1.5T were compared with those of 3.0T. Results : The T1 relaxation times of NAA were $2293\;{\pm}\;48\;ms$ at 1.5T and $2559\;{\pm}\;124\;ms$ at 3.0T (11.6% increase at 3.0T). The T1 relaxation times of Cho were $2540\;{\pm}\;57\;ms$ at 1.5T and $2644\;{\pm}\;76\;ms$ at 3.0T (4.1% increase at 3.0T). The T1 relaxation times of Cr were $2543\;{\pm}\;75\;ms$ at 1.5T and $2665\;{\pm}\;94\;ms$ at 3.0T (4.8% increase). The T2 relaxation times of NAA were $526\;{\pm}\;81\;ms$ at 1.5T and $468\;{\pm}\;74\;ms$ at 3.0T (11.0% decrease at 3.0T). The T2 relaxation times of Cho were $220\;{\pm}\;44ms$ at 1.5T and $182\;{\pm}\;35\;ms$ at 3.0T (17.3% decrease at 3.0T). The T2 relaxation times of Cr were $289\;{\pm}\;47\;ms$ at 1.5T and $275\;{\pm}\;57\;ms$ at 3.0T (4.8% decrease at 3.0T). Conclusion : The T1 relaxation times of the major cerebral metabolites (NAA, Cr, Cho), which were measured at the phantom, were 4.1%-11.6% longer at 3.0T than at 1.5T. The T2 relaxation times of them were 4.8%-17.3% shorter at 3.0T than at 1.5T. To optimize MR spectroscopy at 3.0T, TR should be lengthened and TE should be shortened.

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Identification of triacylglycerols in coix seed extract by preparative thin layer chromatography and liquid chromatography atmospheric pressure chemical ionization tandem mass spectrometry

  • Sim, Hee-Jung;Lee, Seul gi;Park, Na-Hyun;Kim, Youna;Cho, Hyun-Woo;Hong, Jongki
    • Analytical Science and Technology
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    • v.30 no.2
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    • pp.102-111
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    • 2017
  • Here we reported a methodology for identification of triacylglycerols (TAGs) and diacylglycerols (DAGs) in coix seed by preparative thin layer chromatography (prep-TLC) and non-aqueous reversed-phase liquid chromatography (NARP LC)-atmospheric pressure chemical ionization (APCI) tandem mass spectrometry (MS/MS). Lipid components were extracted from coix seed by reflux extraction using n-hexane for 3 hr. TAGs and DAGs in coix seed extract were effectively purified and isolated from matrix interferences by prep-TLC and then analyzed by LC-APCI-MS and MS/MS for identification. TAGs were effectively identified taking into consideration of their LC retention behavior, APCI-MS spectra patterns, and MS/MS spectra of $[DAG]^+$ ions. In MS/MS spectra of TAGs, diacylglycerol-like fragment $[DAG]^+$ ions were useful to identify TAGs with isobaric fragment ions. Based on an established method, 27 TAGs and 8 DAGs were identified in coix seed extract. Among them, 15 TAGs and 8 DAGs were for the first time observed in coix seed. Interestingly, some of TAGs isolated by prep-TLC were partly converted into DAGs through probably photolysis process during storing in room temperature. Thus, degradation phenomenon of TAGs should be considered in the quality evaluation and nutritional property of coix seed. LC-APCI-MS/MS combined with prep-TLC will be practical method for precise TAG and DAG analysis of other herbal plants.

Phospholipid Analysis by Nanoflow Liquid Chromatography-Tandem Mass Spectrometry

  • Moon, Myeong Hee
    • Mass Spectrometry Letters
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    • v.5 no.1
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    • pp.1-11
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    • 2014
  • Lipids play important roles in biological systems; they store energy, play a structural role in the cell membrane, and are involved in cell growth, signal transduction, and apoptosis. Phospholipids (PLs) in particular have received attention in the medical and lipidomics research fields because of their involvement in human diseases such as diabetes, obesity, atherosclerosis, and many cancers associated with lipid metabolic disorders. Here I review experimental strategies for PL analysis based on nanoflow liquid chromatography-electrospray ionization-tandem mass spectrometry (nLC-ESI-MSn). In particular, discussed are lipid extraction methods, nanoflow LC separation of PLs, effect of ionization modifiers on the ESI of PLs, influence of chain lengths and unsaturation degree of acyl chains of PLs on MS intensity, structural determination of the molecular structure of PLs and their oxidized products, and quantitative profiling of PLs from biological samples such as tissue, urine, and plasma in relation to cancer and coronary artery disease.

A Dynamically setted Nmax_info_frames Parameter Under the BACnet MS/TP Network Environment (BACnet MS/TP 네트워크 환경에서 Nmax_info_frames 파라미터 환경 적응적 동적세팅)

  • Kwak, Young;Park, Myong-Soon
    • Annual Conference of KIPS
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    • 2007.11a
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    • pp.1046-1049
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    • 2007
  • BACnet MS/TP 네트워크를 구성할 때 네트워크 설계자는 Nmax_info_frames 값을 정해야 한다. 이 파라 미터는 노드가 토큰을 가질 때 메시지를 보낼 수 있는 횟수를 정하는 것으로 이 값이 너무 크면 특정 노드가 여러 개의 메시지를 보내는 동안 다른 노드들의 네트워크에 접근하지 못하므로 다른 노드의 서비스 지연을 야기시키고, 이 값이 너무 작으면 빈번한 토큰 교환으로 네트워크 오버헤드 발생과, 충분한 메시지 전송을 못하므로 토큰을 넘긴 노드의 서비스 지연을 야기 시킬 수 있다. 따라서 본 논문에서는 이 Nmax_info_frames 값을 네트워크 상황에 맞게 동적 설정하는 알고리즘을 제안한다.