• Title/Summary/Keyword: source quantification method

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Direct Quantitation of Amino Acids in Human Serum Using a Stepwise-Dilution Strategy and a Mixed-Mode Liquid Chromatography-Tandem Mass Spectrometry Method

  • Lee, Jaeick;Lee, Seunghwa;Kim, Byungjoo;Lee, Joonhee;Kwon, Oh-Seung;Cha, Eunju
    • Mass Spectrometry Letters
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    • v.9 no.1
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    • pp.30-36
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    • 2018
  • A quantitation method for free amino acids in human serum was developed using a stepwise-dilution method and a bimodal cation exchange (CEX)/hydrophilic interaction liquid chromatography (HILIC)-tandem mass spectrometry system equipped with an electrospray ionization source (ESI/MS/MS). This method, which was validated using quality control samples, was optimized for enhanced selectivity and sensitivity. Dithiothreitol (DTT) was used as a reducing agent to prevent the oxidation of a serum sample ($50{\mu}L$), which was then subjected to stepwise dilution using 3, 30, and 90 volumes of acetonitrile containing 0.1% formic acid. Chromatographic separation was performed on an Imtakt Intrada Amino Acid column ($50mm{\times}3mm$, $3{\mu}m$) in mixed mode packed with CEX and HILIC ligands embedded in the stationary phase. Underivatized free amino acids were eluted and separated within 10 min. As a result of the validation, the precision and accuracy for the inter- and intraday assays were determined as 2.11-11.51% and 92.82-109.40%, respectively. The lowest limit of quantification (LLOQ) was $0.5-4.0{\mu}g/mL$ and the matrix effect was 80.22-115.93%. The proposed method was successfully applied to the quantitative analysis of free amino acids in human serum.

Simultaneous Determination of Five Porphyrins in Human Urine and Plasma Using High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • Hur, Yeoun;Tae, Sookil;Koh, Yun-Joo;Hong, Sung-Hyun;Yoon, Young Ho;Jang, Haejong;Kim, Sooji;Kim, Kyeong Ho;Kang, Seung Woo;Lee, Youngshin;Han, Sang Beom
    • Mass Spectrometry Letters
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    • v.5 no.2
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    • pp.42-48
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    • 2014
  • A specific and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method (LC-ESI-MS/MS) was developed and validated for the simultaneous quantification of porphyrins (coproporphyrin, pentacarboxylporphyrin, hexacarboxylporphyrin, heptacarboxylporphyrin, and uroporphyrin) in human plasma and urine. Acidified plasma samples and urine samples were prepared by using liquid-liquid extraction using ethyl acetate and protein precipitation with acetonitrile, respectively. The separation was achieved onto a Synergi Fusion RP column ($150mm{\times}2.0mm$, $4{\mu}m$) with a gradient elution of mobile phase A (0.1% formic acid in 2 mmol/L ammonium acetate, v/v) and mobile phase B (20% methanol in acetonitrile, v/v) at a flow rate of $450{\mu}L$/min. Porphyrins and the internal standard (IS), coproporphyrin I-$^{15}N_4$, were detected by a tandem mass spectrometer equipped with an electrospray ion source operating in positive ion mode. Multiple reaction monitoring (MRM) transitions of the protonated precursor ions and the related product ions were optimized to increase selectivity and sensitivity. The proposed method was validated by assessing selectivity, linearity, limit of quantification (LOQ), precision, accuracy, recovery, and stability. The calibration curves were obtained in the range of 0.1-100 nmol/L and the LOQs were estimated as 0.1 nmol/L for all porphyrins. Results obtained from the validation study of porphyrins showed good accuracy, precision, recovery, and stability. Finally, the proposed method was successfully applied to clinical studies on the autism spectrum disorder (ASD) diagnosis of 203 Korean children.

Quality Evaluation of Criterion Construction for Open Source Software (개방형 소프트웨어의 품질평가 기준 구축)

  • Kang, Sang-Won;Yang, Hae-Sool
    • Journal of Digital Convergence
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    • v.11 no.2
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    • pp.323-330
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    • 2013
  • The trend of the use of open softwares is increasing daily. Despite these increases in the use of open softwares, the importance of the problem of their quality is not considered enough. Also, if we look at the existing evaluation model which is used as the evaluation model of the existing open software, the level of the quantization is insufficient, the evaluator can show some subjectivity and as a clear evaluation method is not published, there are many problems to apply it in practice. Therefore, in this study, we have built an evaluation basis that can show consistent quantization without the influence of the evaluator and that can improve the evaluation speed with the automatization of the evaluation information acquisition. The built quality evaluation model will take an important role to evaluate and to improve the open software.

Effect of Distribution System Materials and Water Quality on Heterotrophic Plate Counts and Biofilm Proliferation

  • CHANG , YOUNG-CHEOL;JUNG, KWEON
    • Journal of Microbiology and Biotechnology
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    • v.14 no.6
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    • pp.1114-1119
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    • 2004
  • The biofilms on pipe walls in water distribution systems are of interest since they can lead to chlorine demand, coliform growth, pipe corrosion, and water taste and odor problems. As such, the study described in this paper is part of an AWWARF and Tampa Bay Water tailored collaboration project to determine the effect of blending different source waters on the water quality in various distribution systems. The project was based on 18 independent pilot distribution systems (PDS), each being fed by a different water blend (7 finished waters blended in different proportions). The source waters compared were groundwater, surface water, and brackish water, which were treated in a variety of pilot distribution systems, including reverse osmosis (RO) (desalination), both membrane and chemical softening, and ozonation-biological activated carbon (BAC), resulting in a total of 7 different finished waters. The observations from this study consistently demonstrated that unlined ductile iron was more heavily colonized by a biomass than galvanized steel, lined ductile iron, and PVC (in that order) and that the fixed biomass accumulation was more influenced by the nature of the supporting material than by the water quality (including the secondary residual levels). However, although the bulk liquid water cultivable bacterial counts (i.e. heterotrophic plate counts or HPCs) did not increase with a greater biofilm accumulation, the results also suggested that high HPCs corresponded to a low disinfectant residual more than a high biofilm inventory. Furthermore, temperature was found to affect the biofilms, plus the AOC was important when the residual was between 0.6 and 2.0 mg $Cl_2/l$. An additional aspect of the current study was that the potential of the exoproteolytic activity (PEPA) technique was used along with a traditional so-called destructive technique in which the biofilm was scrapped off the coupon surface, resuspended, and cultivated on an R2A agar. Both techniques indicated similar trends and relative comparisons among the PDSs, yet the culturable biofilm values for the traditional method were several orders of magnitude lower than the PEPA values.

Source Identification and Quantification of Coarse and Fine Particles by TTFA and PMF

  • Hwang, In-Jo;Bong, Choon-Keun;Lee, Tae-Jung;Kim, Dong-Sool
    • Journal of Korean Society for Atmospheric Environment
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    • v.18 no.E4
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    • pp.203-213
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    • 2002
  • Receptor modeling is one of statistical methods to achieve reasonable air pollution strategies. In order to maintain and manage ambient air quality, it is necessary to identify sources and to apportion its sources for ambient particulate matters. The main purpose of the study was to survey seasonal trends of inorganic elements in the coarse and fine particles. Second, this study has attempted emission sources qualitatively by a receptor method, the PMF mo-del. After that. both PMF (positive matrix factorization) model and TTFA (target transformation factor analysis) model were applied to compare and to estimate mass contribution of coarse and fine particle sources at the receptor. A total of 138 sets of samples was collected from 1989 to 1996 by a low volume cascade impactor with 9 size fraction stages at Kyung Hee University in Korea. Sixteen chemical species (Si, Ca, Fe, K, Pb, Na, Zn, Mg, Ba, Ni, V, Mn, Cr, Br, Cu. Co) were characterized by XRF. The study result showed that the weighted arithmetic mean of coarse and fine particles were 51.3 and 54.4 $\mu\textrm{g}$/㎥, respectively. Contribution of both particle fractions were esti-mated using TTFA and PMF models. The number of estimated sources was seven according to TTFA model and 8 according to PMF model. Comparison of TTFA and PMF revealed that both methodologies exhibited similar trends in their contribution pattern. However, large differences between contributions were observed in some sour-ces. The results of this study may help to suggest control strategies in local countries where known source profiles do not exist.

Experimental Evaluation of Direct Measurement for Excitation Forces Acting on the Hard-points of Suspension System to Predict Road-noise Performance (로드노이즈 성능 예측을 위한 현가장치 하드포인트의 가진력 직접 측정법에 대한 실험적 평가)

  • Kang, Yeon June;Kim, Heesoo;Song, David P.;Ih, Kang-Duck;Kim, HyoungGun
    • Transactions of the Korean Society for Noise and Vibration Engineering
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    • v.25 no.3
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    • pp.184-190
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    • 2015
  • NVH engineering has become a hot issue due to radical technology changes and development in automotive industry since customers' expectations and needs for their vehicle is taken to a higher level. However, the source identification and quantification of the road noise within a vehicle is still not at the level where it needs to be to meet their expectations due to its' complex transfer path and difficulties in path optimization. The primary focus of this research is on direct force obtaining method at suspension hard points using suspension test rig. Directly obtained forces at suspension to body mounting points are critical and crucial for determining the effects of design changes of the suspension has on road noise performance. Direct force obtaining method has its limitation in sensor installation within an actual vehicle therefore, many has been indirectly calculating forces using full matrix inversion method or dynamic stiffness method. In this study, to circumvent this limitation, a suspension rig is used. Then, the suspension rig is verified through a comparative analysis of its dynamic behavior between the actual vehicle by cleat test on chassis dynamometer.

Development of Isotope Dilution LC-MS/MS Method for Accurate Determination of Arsenobetaine in Oyster Certified Reference Material

  • Lee, Woo Young;Yim, Yong-Hyeon;Hwang, Euijin;Lim, Youngran;Kim, Tae Kyu;Lee, Kyoung-Seok
    • Bulletin of the Korean Chemical Society
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    • v.35 no.3
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    • pp.821-827
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    • 2014
  • An isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) method has been developed and applied to the determination of arsenobetaine (AsB, ${(CH_3)_3}^+AsCH_2COO^-$) from oyster candidate certified reference material (CRM). The exact matching isotope dilution approach was adopted for accurate determination of AsB using $^{13}C_2$-labeled AsB as an internal standard. Efficiencies of different AsB extraction methods were evaluated using a codfish reference material and a simple sonication method was selected as the method of choice for the certification of the oyster candidate CRM. The hydrophilic interaction liquid chromatography (HILIC) combined with electrospray ionization tandem mass spectrometry (ESI/MS/MS) in selected reaction monitoring (SRM) mode was optimized for adequate chromatographic retention and robust quantification of AsB from codfish and oyster samples. By analyzing 12 subsamples taken from each 12 bottles systematically selected from the whole oyster CRM batch, the certified value of AsB was determined as $6.60mg{\cdot}kg^{-1}{\pm}0.31mg{\cdot}kg^{-1}$ and it showed excellent between-bottle homogeneity of less than 0.42%, which is represented by relative standard deviation of 12 bottles from the CRM batch. The major source of uncertainty was the certified value of the AsB standard solution.

Interior Noise Reduction of Wheel Loader Using Transfer Path Analysis and Panel Contribution Analysis (전달 경로 분석과 패널 기여도 분석을 이용한 휠로더의 실내소음 저감에 관한 연구)

  • Kim, Bo-Yong;Shin, Chang-Woo;Jeong, Won-Tae;Park, Sung-Yong;Jang, Han-Kee;Kim, Seong-Jae;Kang, Yeong-June
    • Transactions of the Korean Society for Noise and Vibration Engineering
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    • v.18 no.8
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    • pp.805-815
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    • 2008
  • Transfer path analysis(TPA) and panel contribution analysis(PCA) have been used widely to reduce interior noise of mechanical systems. TPA enables us to decompose interior noise into air-borne and structure-borne noises and estimate the path contribution of noise sources. PCA is also used to identify the noise contribution of each sub-panel in vibro-acoustic systems. In this paper, TPA and PCA are applied to wheel loader, one of the heavy construction equipments. Firstly, TPA for air-borne noise is conducted to estimate the contribution of air-borne sources using pressure transfer function. Thereafter, TPA for structure -borne noise is employed to verify the results of air-borne source quantification through the synthesis of two results. Secondly, PCA is performed by both TPA using pressure transfer function between panels inside the cabin and boundry element method(BEM) for the cabin of wheel loader with various boundary conditions. As a results, it was found that TPA conducted by experiments and PCA accomplished by both experiments and BEM are very effective methods in analyzing the path and contribution of the noises for reducing an interior noise level in the wheel loader system.

Quantitative Determination of the Marker Components in Pyungwi-San Using LC-ESI-MS/MS (LC-ESI-MS/MS를 이용한 평위산 주요 성분의 함량 분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.49 no.3
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    • pp.270-277
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    • 2018
  • Pyungwi-san has been used to treat the digestive system diseases, physconia, nausea, anorexia, and dyspepsia in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was optimized for simultaneous determination of the 14 marker components, spinosin, liquiritirn apioside, liquiritin, narirutin, 6'''-feruloylspinosin, hesperidin, liquiritigenin, glycyrrhizin, 6-gingerol, atractylenolide III, honokiol, atractylenolide II, magnolol, and atractylenolide I in Pyungwi-san extract. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) with maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid and acetonitrile. The MS conditions were as follows: capillary voltage 3.3 kV, extractor voltage 3.0 V, RF lens voltage 0.3 V, source temperature $120^{\circ}C$, desolvation temperature $300^{\circ}C$, desolvation gas 600 L/h, cone gas 50 L/h and collision gas 0.14 mL/min. The coefficient of determination of 14 analytes was 0.9989-1.0000. The limits of detection and quantification values of the all analytes were 0.04-2.56 and 0.13-7.69 ng/mL, respectively. As a result of the analysis using the established LC-ESI-MS/MS method, the 5 components, spinosin, 6'''-feruloylspinosin, atractylenolide III, II, and I derived from Zizyphi Fructus and Atractylodis Rhizoma, were not detected in this extract. On the other hand, the 9 components except for the 5 components were 4.15-498.87 mg/kg in lyophilized Pyungwi-san extract. Among these components, glycyrrhizin, marker compound of Glycyrrhizae Radix et Rhizoma, was detected the most amount as a 498.87 mg/kg.

Quantitative Analysis of the Marker Constituents in Yongdamsagan-Tang using Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry (LC-ESI-MS/MS를 이용한 용담사간탕의 주요 성분 분석)

  • Seo, Chang-Seob;Ha, Hyekyung
    • Korean Journal of Pharmacognosy
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    • v.48 no.4
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    • pp.320-328
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    • 2017
  • Yongdamsagan-tang has been used to treat the urinary disorders, acute- and chronic-urethritis, and cystitis in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous analysis of the 20 bioactive marker compounds, geniposidic acid, chlorogenic acid, geniposide, liquiritin apioside, acteoside, calceolarioside B, liquiritin, nodakenin, baicalin, liquiritigenin, wogonoside, baicalein, glycyrrhizin, wogonin, glycyrrhizin, wogonin, saikosaponin A, decursin, decursinol angelate, alisol B, alisol B acetate, and pachymic acid in traditional herbal formula, Yongdamsagan-tang. Chromatographic separations of all marker compounds were conducted using a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was performed using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization source in the positive and negative modes. The flow rate was 0.3 mL/min and injection volume was $2.0{\mu}L$. The correlation coefficient of 20 marker compounds in the test ranges was 0.9943-1.0000. The limits of detection and quantification values of the all marker components were 0.11-6.66 and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the optimized LC-ESI-MS/MS method, three compounds, geniposidic acid (from Plantaginis Semen), alisol B (from Alismatis Rhizoma), and pachymic acid (from Poria Sclerotium), were not detected in this sample. While the amounts of the 17 compounds except for the geniposidic acid, alisol B, and pachymic acid were $0.04-548.13{\mu}g/g$ in Yongdamsagan-tang sample. Among these compounds, baicalin, bioactive marker compound of Scutellariae Radix, was detected at the highest amount as a $548.13{\mu}g/g$.