• 제목/요약/키워드: Quantitation

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LC-Tandem Mass Spectrometry를 활용한 농업용수 중 Perfluorochemicals 분석시료 전처리법 (Sample Preparation Method for Perfluorochemicals with LC-Tandem Mass Spectrometry in Agricultural Water)

  • 김진효;진초롱;최근형;박병준
    • 농약과학회지
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    • 제19권1호
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    • pp.1-4
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    • 2015
  • 잔류성 유기오염물질인 과불화합물 중 perfluorooctanesufonic acid (PFOS)와 perfluorooctanoic acid (PFOA)의 잔류분석은 환경부 "잔류성 유기오염물질 공정시험기준"에 따라 hydrophilic-lipophilic balance (HLB) solid phase extraction (SPE) 전처리 후 LC-$MS^n$를 이용해 정량 분석하고 있다. 본 연구에서는 환경부 설정 공정시험법에 따라 농업용수 전처리 후, 시험법에서 제거하지 못한 미지의 불순물을 Envi-Carb$^{TM}$을 통해 회수율에 영향을 주지 않고 손쉽게 제거하였다. 또한, 과불화합물 분석에 사용되는 LC-$MS^n$ 중 quadrupole-time-of-flight mass spectrometry (qTOFMS)에서 측정된 PFCs의 정량한계를 평가한 결과, 시험에 사용된 장비간 정량한계 편차가 크게 관찰되었으나, 시험대상 장비 모두 농업용수 중 ng/L 수준으로 잔류하는 과불화합물의 정밀 잔류분석에 사용가능 한 것으로 확인되었다.

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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    • 제9권1호
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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.

Carotenoids 화학의 연구방법 (Methodology of Carotenoids Chemistry)

  • 김재웅
    • 한국식품영양학회지
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    • 제14권4호
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    • pp.360-366
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    • 2001
  • This brief review is organized to integrate methodology of carotenoids chemistry from the author's experimental conceps. The majors include classification of carotenoids. extraction·phase separation, purification. crystalyzation, identification, quantitation, spectroscopic properties, organic reactions, and analytical methods of carotenoproteins. The goal is not write a important conceps of carotenoid but to provide a technical methods that may be useful to researchers of natural products chemistry.

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Quantitation of Hepatitis C Viral RNA Using Direct CRT-PCR

  • Park, Young-Suk;Lee, Kyung-Ok;Oh, Moon-Ju;Chai, Young-Gyu
    • BMB Reports
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    • 제30권3호
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    • pp.234-236
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    • 1997
  • Chronic hepatitis C virus (HCV) infection is associated with the rapid development of cirrhosis and hepatocellular carcinoma. It has been reported that the amount of HCV RNA may be correlated with the progression of hepatitis and may be a prognostic marker for treatment of HCV patients. The direct detection of HCV RNA by reverse transcription-polymerase chain reaction (RT-PCR) is widely used to determine the presence of circulating virions. The most relevant limit of this approach is the lack of quantitative information about the viral titer. In the present study, we developed the method for HCV quantitation using competitive reverse transcription (CRT)-PCR using the deleted HCV standard. The serially diluted standard was added in titrated amounts to the target HCV RNA. The mixture was then reverse transcribed and amplified in the same reaction tube. The methods were evaluated using over 110 HCV-PCR positive samples in Koreans. About 59% of the samples were judged to contain $10^{5}-10^{6}$ copies of HCV RNA in 1 ml of serum.

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식육중의 잔류 항생.항균제의 검정에 관한 연구(III) Macrolide계 항생물질인 Erythromycin과 Tylosin의 Gas Chromatography/Mass Spectrometry 동시분석 (A study on the determination of residual Antibiotics and Synthetic Antibacterial Agents in Meat(III) Simultaneous Gas Chromatography/Mass Spectrometry Analysis of Erythromycin and Tylosin)

  • 류재천;송윤선;양종순;서지원;김명수;박종세
    • 한국식품위생안전성학회지
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    • 제8권1호
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    • pp.17-23
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    • 1993
  • In an attempt to quantitate and qualitate residual antibiotics and antibacterial agents n meat simultaneously, we studied a gas chromatogrphy-mass spectrometry (GC/MS) analysis. For a simultaneous analysis of macrolide antibiotics such as erythromycin and tylosin in meat, the homogenization with MeOH, defatting with n-hexane, extraction with CHCl3, elution with CHCl3 : MeOH=2:1 from Sep-Pak silica cartridge, acid gydrolysis, back extraction with CHCl3, and quantitation by selected ion monitoring(SIM) mode after trimethylsilyl derivatization were performed. The recoveries of erythromycin and tylosin (CV,%) at 10 ppm fortification level were 90.59(4.89) and 45.91(0.20) , and the detection limits of those were 0.02 and 2.0 $\mu\textrm{g}$/g beef, respectively. From these results, the developed analytical method using GC/MS-SIM mode allows excellent detection and quantitation of residual macrolide antibiotics in meats, using complementary method with bio-assay.

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SENSITIVE DETERMINATION OF ELEVEN PHENOLIC ENDOCRINE-DISRUPTING CHEMICALS IN HUMAN URINE USING GAS CHROMATOGRAPHY/MASS SPECTROMETRY -SELECTED ION MONITORING

  • Kim, Hyub;Jang, Cheol-Hyeon
    • Environmental Engineering Research
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    • 제12권3호
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    • pp.93-100
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    • 2007
  • I improved an analytical method for determining trace amounts of eleven phenolic endocrine-disrupting chemicals (11 phenolic EOCs) in human urine. The 11 phenolic EOCs were subjected to hydrolysis and then to solid phase extraction with a XAD-4 column. Alkylphenols, chlorophenols, and bisphenol A in XAD-4 column were eluted with acetonitrile, and the eluate was concentrated under a nitrogen stream, and then tert-butyldimethylsilylation. Separation and determination were done by gas chromatography, using mass spectrometry operating in the selective ion monitoring mode for quantitation. For tert-butyldimethylsily (TBDMS) derivatization the recoveries were $91.2{\sim}125.9%$, the limits of quantitation (LOQ) for the 11 phenolic EOCs in the nanogram-per-milliliter range ($0.025{\sim}1.000\;ng/mL$) were thus achieved by using 1 mL of urine, and the SIM responses were linear with the correlation coefficient varying by $0.9300{\sim}0.9943$. Based on the results for urine samples from unexposed individuals, 4-tert-octylphenol and pentachlorophenol were detected in hydrolysed urine sample. Other alkylphenols, chlorophenols and bisphenol A were not detected.

Picomolar Scale Determination of Carbohydrates Covalently Immobilized on Activated Beads Using Hydroxyl Functionality

  • Yu, Jae-Hoon;Chun, Sung-Min;Park, Ho-Koon;Park, Yong-Keun;Jeong, Sun-Joo
    • BMB Reports
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    • 제32권1호
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    • pp.98-102
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    • 1999
  • Since carbohydrates are major mediators in cell-to-cell adhesion and communication, the development of specific and strong binders against them could generate promising therapeutics. As the first step towards that goal, sugar molecules have to be immobilized to be used as an affinity matrix. The amino functionality in sugar is the most active nucleophile for the immobilization, if the amino group is available. An alternative and general method is to use the hydroxyl group as a direct nucleophile, but the quantitation of immobilized hydroxyl groups is not easily done. To overcome this limitation, we have developed a method to immobilize various isomers of monosaccharides with p-nitrophenyl groups to the beads by using their hydroxyl groups. It was found that the amount of immobilized sugar was independent of the structure of the sugar, but was dependent on the number of hydroxyl groups. We also developed a sensitive method to quantify the amount of immobilized sugar at the picomolar scale by utilizing commercially available glycosidases to release a sensitive reporter molecule, p-nitrophenol, and detect it by HPLC. This new technique would allow a facile quantitation method for immobilized sugar molecules, which could be used as the affinity matrix to develop strong binders against biologically important sugars.

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