• Title/Summary/Keyword: Sample matrix

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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.

Impact Toughness and Microstructure of the Weld Metal by Tandem Electro-Gas Welded EH40 Steel (EH40 강의 Tandem EGW 용접부 미세조직과 충격인성 특성)

  • Park, Tae Gyu;Kim, Jeon Min;Yoon, Hye Young;Lee, Je Hyun;Chung, Won Jee;Kim, Ho Kyeong
    • Korean Journal of Metals and Materials
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    • v.48 no.11
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    • pp.1021-1027
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    • 2010
  • The charpy impact property was lower at the surface and middle regions than that at the root region in metal welded by Tandem EGW of 82 mm thick EH40-TM steel plates. Temperature distribution in the weld sample and the heating/cooling temperature throughout the various regions in the weld metal were estimated by the commercial weld simulation program SYSWELD. The microstructure of the weld metal consisted of acicular ferrite and grain boundary ferrite. Grain boundary ferrite in the acicular ferrite matrix was found more in the surface and middle regions than in the root region, and the acicular ferrite was also coarser in the surface and middle regions where the impact toughness was lower and the input temperature was higher. Our results indicated that the impact toughness property was related to the microstructure morphology, the distribution of grain boundary ferrite, and the acicular ferrite.

Feature Selection for Image Classification of Hyperion Data (Hyperion 영상의 분류를 위한 밴드 추출)

  • 한동엽;조영욱;김용일;이용웅
    • Korean Journal of Remote Sensing
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    • v.19 no.2
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    • pp.170-179
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    • 2003
  • In order to classify Land Use/Land Cover using multispectral images, we have to give consequence to defining proper classes and selecting training sample with higher class separability. The process of satellite hyperspectral image which has a lot of bands is difficult and time-consuming. Furthermore, classification result of hyperspectral image with noise is often worse than that of a multispectral image. When selecting training fields according to the signatures in the study area, it is difficult to calculate covariance matrix in some clusters with pixels less than the number of bands. Therefore in this paper we presented an overview of feature extraction methods for classification of Hyperion data and examined effectiveness of feature extraction through the accuracy assesment of classified image. Also we evaluated the classification accuracy of optimal meaningful features by class separation distance, which is also a method for band reduction. As a result, the classification accuracies of feature-extracted image and original image are similar regardless of classifiers. But the number of bands used and computing time were reduced. The classifiers such as MLC, SAM and ECHO were used.

Separation of Goid, Palladium and Platinum in Chromite by Anion Exchange Chromatography for Inductively Coupled Plasma Atomic Emission Spectrometric Analysis

  • Choe, Gwang Sun;Lee, Chang Hyeon;Park, Yeong Jae;Jo, Gi Su;Kim, Won Ho
    • Bulletin of the Korean Chemical Society
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    • v.22 no.8
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    • pp.801-806
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    • 2001
  • A study has been carried out on the separation of gold, iridium, palladium, rhodium, ruthenium and platinum in chromite samples and their quantitative determination using inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution condition of the minerals by fusion with sodium peroxide was optimized and chromatographic elution behaviour of the rare metals was investigated by anion exchange chromatography. Spectral interference of chromium, a matrix of the minerals, was investigated on determination of gold. Chromium interfered on determination of gold at the concentration of 500 mg/L and higher. Gold plus trace amounts of iridium, palladium, rhodium and ruthenium, which must be preconcentrated before ICP-AES was separated by anion exchange chromatography after reducing Cr(Ⅵ) to Cr(III) by H2O2. AuCl4- retained on the resin column was selectively eluted with acetone- HNO3-H2O as an eluent. In addition, iridium, palladium, rhodium and ruthenium remaining on the resin column were eluted as a group with concentrated HCl. However, platinum was eluted with concentrated HNO3. The recovery yield of gold with acetone-HNO3-H2O was 100.7 ${\pm}2.0%$, and the yields of palladium and platinum with concentrated HCl and HNO3 were 96.1 ${\pm}1.8%$ and 96.6 ${\pm}1.3%$, respectively. The contents of gold and platinum in a Mongolian chromite sample were 32.6 ${\pm}$ 2.2 ${\mu}g$/g and 1.6 $\pm$ 0.14 ${\mu}g$/g, respectively. Palladium was not detected.

Simultaneous Spectrometric Determination of Caffeic Acid, Gallic Acid, and Quercetin in Some Aromatic Herbs, Using Chemometric Tools

  • Kachbi, Abdelmalek;Abdelfettah-Kara, Dalila;Benamor, Mohamed;Senhadji-Kebiche, Ounissa
    • Journal of the Korean Chemical Society
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    • v.65 no.4
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    • pp.254-259
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    • 2021
  • The purpose of this work is the development of a method for an effective, less expensive, rapid, and simultaneous determination of three phenolic compounds (caffeic acid, gallic acid, and quercetin) widely present in food resources and known for their antioxidant powers. The method relies on partial least squares (PLS) calibration of UV-visible spectroscopic data. This model was applied to simultaneously determine, the concentrations of caffeic acid (CA), gallic acid (GA), and quercetin (Q) in six herb infusion extracts: basil, chive, laurel, mint, parsley, and thyme. A wavelength range (250-400) nm, and an experimental calibration matrix with 21 samples of ternary mixtures composed of CA (6.0-21.0 mg/L), GA (10.0-35.2 mg/L), and Q (6.4-17.5 mg/L) were chosen. Spectroscopic data were mean-centered before calibration. Two latent variables were determined using the contiguous block cross-validation procedure after calculating the root mean square error cross-validation RMSECV. Other statistic parameters: RMSEP, R2, and Recovery (%) were used to determine the predictive ability of the model. The results obtained demonstrated that UV-visible spectrometry and PLS regression were successfully applied to simultaneously quantify the three phenolic compounds in synthetic ternary mixtures. Moreover, the concentrations of CA, GA and Q in herb infusion extracts were easily predicted and found to be 3.918-18.055, 9.014-23.825, and 9.040-13.350 mg/g of dry sample, respectively.

Effect of Biological and Liquid Hot Water Pretreatments on Ethanol Yield from Mengkuang (Pandanus artocarpus Griff)

  • Yanti, Hikma;Syafii, Wasrin;Wistara, Nyoman J;Febrianto, Fauzi;Kim, Nam Hun
    • Journal of the Korean Wood Science and Technology
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    • v.47 no.2
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    • pp.145-162
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    • 2019
  • This study aimed to increase the sugar and ethanol yield from the mengkuang plant biomass through biological and liquid hot water (LHW) pretreatment and their combination. The results showed that biological pretreatments with 5% inoculum of the fungus Trametes versicolor resulted in the highest alpha cellulose content incubated for 30 days, and 10% inoculum resulted in the lowest lignin content. LHW pretreatment decreased the hemicellulose content of pulps from 10.17% to 9.99%. T. versicolor altered the structure of the mengkuang pulp by degrading the lignin and lignocellulose matrix. The resulting delignification and cellulose degradation facilitate the hydrolysis of cellulose into sugars. The alpha cellulose content after biological-LHW pretreatment was higher (78.99%) compared to LHW-biological pretreatment (76.85%). Scanning electron microscopy analysis showed that biological-LHW combinated treatment degrades the cell wall structures. The ethanol yield for biological-LHW pretreated sample was observed 43.86% (13.11 g/L ethanol by weight of the substrate, which is much higher than that of LHW-biological pretreatment (34.02%; 9.097 g/L). The highest reducing sugar content about 45.10% was observed with a resulting ethanol content of 15.5 g/L at LHW pretreatment temperature of $180^{\circ}C$ for 30 min.

Assessment of technological characteristics and microbiological quality of marinated turkey meat with the use of dairy products and lemon juice

  • Augustynska-Prejsnar, Anna;Hanus, Pawel;Sokolowicz, Zofia;Kacaniova, Miroslava
    • Animal Bioscience
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    • v.34 no.12
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    • pp.2003-2011
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    • 2021
  • Objective: The aim of this study was to evaluate the effect of marinating turkey meat with buttermilk and acid whey on the technological traits and microbiological quality of the product. Methods: Slices of turkey meat muscles were marinated for 12 hours in buttermilk (n = 30), acid whey (n = 30) and comparatively, in lemon juice (n = 30). The control group (n = 30) consisted of unmarinated slices of turkey breast muscles. Physical parameters (pH, water holding capacity, colour L*a*b*, shear force, weight loss) were assessed and quantitative and qualitative microbiological evaluation of raw and roasted products was performed. The microbiological parameters were determined as the total viable counts of mesophilic aerobic bacteria, of the Enterobacteriaceae family, and Pseudomonas spp. Bacterial identification was performed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Results: Marinating turkey meat in buttermilk and whey compared to marinating in lemon juice and the control sample resulted in a higher (p<0.05) degree of yellow color saturation (b*) and a reduction (p<0.05) in the number of mesophilic aerobic bacteria, Pseudomonas spp. and Enterobacteriaceae family as well as the number of identified mesophilic aerobic bacteria in both raw and roasted samples. The lowest (p<0.05) shear force values were found in products marinated in whey. Conclusion: The use of buttermilk and acid whey as a marinade for meat increases the microbiological safety of the product compared to marinating in lemon juice, while maintaining good technological features of the product.

Micro-CT - a digital 3D microstructural voyage into scaffolds: a systematic review of the reported methods and results

  • Cengiz, Ibrahim Fatih;Oliveira, Joaquim Miguel;Reis, Rui L.
    • Biomaterials Research
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    • v.22 no.4
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    • pp.279-289
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    • 2018
  • Background: Cell behavior is the key to tissue regeneration. Given the fact that most of the cells used in tissue engineering are anchorage-dependent, their behavior including adhesion, growth, migration, matrix synthesis, and differentiation is related to the design of the scaffolds. Thus, characterization of the scaffolds is highly required. Micro-computed tomography (micro-CT) provides a powerful platform to analyze, visualize, and explore any portion of interest in the scaffold in a 3D fashion without cutting or destroying it with the benefit of almost no sample preparation need. Main body: This review highlights the relationship between the scaffold microstructure and cell behavior, and provides the basics of the micro-CT method. In this work, we also analyzed the original papers that were published in 2016 through a systematic search to address the need for specific improvements in the methods section of the papers including the amount of provided information from the obtained results. Conclusion: Micro-CT offers a unique microstructural analysis of biomaterials, notwithstanding the associated challenges and limitations. Future studies that will include micro-CT characterization of scaffolds should report the important details of the method, and the derived quantitative and qualitative information can be maximized.

A Simple and Efficient Method to Determine Montelukast in Rat Plasma Using Liquid-Liquid Extraction and Tandem Mass Spectrometry

  • Kim, Dong Yoon;Lee, Hyo Chun;Jang, Yong Jin;Kim, Jin Hee;Lee, Ha Ryeong;Kang, Myung Joo;Choi, Yong Seok
    • Mass Spectrometry Letters
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    • v.11 no.4
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    • pp.71-76
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    • 2020
  • While montelukast (ML), a cysteinyl-leukotriene type 1 receptor (CysLT1) antagonist is widely used to treat symptoms of rhinitis or asthma, its formulations are mainly limited to solid preparation due to its instability. Recently, there have been attempts to develop various ML dosage forms, and this situation increases the demand of sensitive and creditable methods to determine ML in various samples such as plasma. Thus, here, a simple and efficient method to determine ML in rat plasma using liquid-liquid extraction (LLE) and multiple reaction monitoring was presented. The mixture of DCM:EtOAc (25:75, v/v), the optimized extract solvent for LLE was found to be effective to extract ML without hydrophilic salts and proteins from the sample with limited volume. Also, the use of zafirlukast, instead of expensive ML-d6, as the internal standard makes the present method economical. The developed method was successfully validated in terms of selectivity, matrix effects (-14.8--6.9%), linearity (r230.998 within 0.5-500 ng/mL), sensitivity (the limit of detection and the lower limit of quantitation, ≤0.5 ng/mL), accuracy (88.4-100.6%), precision (3.0-13.3%), and recovery (80.8-86.3%) by following the FDA guidelines. Finally, the applicability of the validated method to pharmacokinetics (PK) studies was confirmed by the successful determination of PK parameters through it following oral administration of Singulair® granule in rats. Therefore, the present method can contribute to the development of new ML formulations through its performance to determine ML in rat plasma efficiently and sensitively.

An Evaluation of Importance and Performance for the Silver Orchestra Program Using IPA (중요도-만족도 분석(IPA) 기법을 활용한 노인복지관의 실버 오케스트라 프로그램 평가에 대한 연구)

  • Her, Soon-Goo
    • The Journal of the Korea Contents Association
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    • v.20 no.12
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    • pp.287-300
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    • 2020
  • The present study applied the IPA(Importance-Performance Analysis) to derive several practical alternatives for the improvement of Chuncheon Silver Orchestra program using IPA(importance-performance analysis). Most importantly, this work performed a comparative study using sample data collected from two groups of silver member(N=53) and program operator(N=32). A careful literature review leaded to the development of six types of evaluation sectors, including 'connection with the local community', 'budget operation', 'program operation', 'manpower operation', 'public relations strategy' as well as 'environment for program operation'. This work further devised twenty-two evaluation items. The results indicated that silver member group rated 'manpower operation' the highest in their both perceived importance and performance. Program operator group rated 'budget operation' and 'manpower operation' rated the highest in their perceived importance and performance, respectively. The results form IPA matrix analysis provides an important implication that much efforts and interests should be sustainably given from the perspective of the silver member group and the program operator group coupled with four types of IPA quadrant, accordingly.