• 제목/요약/키워드: High-performance liquid chromatography-tandem mass spectrometry

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High-Performance liquid Chrmatogrphic and Tandem Mass Spectrometric Quantitation of N7-Methyldeoxyguanosin in Methylated Calf Thymus DNA

  • Chae, Whi-Gun
    • Biotechnology and Bioprocess Engineering:BBE
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    • 제5권3호
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    • pp.191-195
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    • 2000
  • Quantitation of N7-methyldeoxyguanosine (N7-MedG) produced in the in vitro N-methly-N-nitrosuourea (NMU) action on thymus DNA has been achieved by enzymatic degradation, liquid chromatoraphic separaphic separation and desorption chemical ionization tandem mass spectrometry. In conjunction with the resolving power HPLC in the separation of isomers, desorprion chemical ionization tandem mass spectrometry has utilized in determining modified nucleosides at low levels using a stable-isotope labled compound as an internal reforence. The quantitative estimation of N7-methyldeoxyguanosine was previously established by an independent HPLC analysis of methylated calf thymus DNA. A sensitive and specific methodogy for the quantitation of N7-MedG at the picomole level using HPLC combined with tandem mass spectrometry without radioisotope labeling process is presented. The potential of the liquid chromatoraphic tandem mass exposure to methlation agents in vitro.

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Identification of Ceftiofur Oxidation Products by High-Performance Liquid Chromatography/Electrospray Ionization/Tandem Mass Spectrometry

  • Lim, Young-Hee;Park, Deok-Hie;Youn, Yeu-Young;Kim, Kyung-Hoon;Cho, Hye-Sung
    • Mass Spectrometry Letters
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    • 제2권1호
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    • pp.16-19
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    • 2011
  • Oxidation products of ceftiofur were formed in hydrogen peroxide solution. The structures of the ceftiofur oxidation products were characterized by high-performance liquid chromatography/electrospray ionization/tandem mass spectrometry (HPLC/ESI/MS/MS). The products were identified as compounds oxidized at the sulfur of a cephem ring. For further analysis, experiments were performed using $O^{18}$-labeled hydrogen peroxide. In addition, density-functional calculations were carried out for six possible oxidation products to support the experimental results.

Establishment of analytical methods for allergenic compounds in mouthwashes and sanitary napkins by ultra-high-performance liquid chromatography with tandem mass spectrometry

  • Hee-Jung Sim;Hee-Jin Jeong;Yeong-In Lee;Yu-Jin Cho;Seung-Hoon Baek;Jong-Hwan Kim
    • 분석과학
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    • 제36권2호
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    • pp.89-98
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    • 2023
  • Analytical methods for detecting atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes were developed using ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). UHPLC-MS/MS conditions were optimized for rapid, sensitive, and simultaneous analysis of the five allergenic compounds. The methods were validated by assessing their specificity, matrix effects, limit of detection (LOD), limit of quantification (LOQ), linearity, accuracy, and precision. Good linearity was achieved with a determination coefficient of ≥0.99. The LOD and LOQ were 2.1-9.8 and 6.4-29.6 ng/g for sanitary napkins and 0.29-0.48 and 0.87-1.45 ng/mL for mouthwashes, respectively. The accuracy and precision were within an acceptable range according to the criteria reported in the European SANTE/11813/2017 guidelines (70-120 % recovery, <20 % relative standard deviation). Therefore, these methods can be used to analyze atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes.

Multiclass Method for the Determination of Anthelmintic and Antiprotozoal Drugs in Livestock Products by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

  • Hyunjin Park;Eunjung Kim;Tae Ho Lee;Sihyun Park;Jang-Duck Choi;Guiim Moon
    • 한국축산식품학회지
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    • 제43권5호
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    • pp.914-937
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    • 2023
  • The objective of this study was to establish a multi-residue quantitative method for the analysis of anthelmintic and antiprotozoal drugs in various livestock products (beef, pork, and chicken) using ultra-high-performance liquid chromatography-tandem mass spectrometry. Each compound performed validation at three different levels i.e., 0.5, 1, and 2× the maximum residue limit according to the CODEX guidelines (CAC/GL 71-2009). This study was conducted according to the modified quick, easy, cheap, effective, rugged, and safe procedure. The matrix-matched calibrations gave correlation coefficients >0.98, and the obtained recoveries were in the range of 60.2%-119.9%, with coefficients of variation ≤32.0%. Furthermore, the detection and quantification limits of the method were in the ranges of 0.03-3.2 and 0.1-9.7 ㎍/kg, respectively. Moreover, a survey of residual anthelmintic and antiprotozoal drugs was also carried out in 30 samples of beef, pork, and chicken collected in Korea. Toltrazuril sulfone was detected in all three samples. Thus, our results indicated that the developed method is suitable for determining the anthelmintic and antiprotozoal drug contents in livestock products.

Profiling Analysis of Sphingolipids in HL-60 Cells by High-Performance Liquid Chromatography-Tandem Mass Spectrometry in combination with Multiple Reaction Monitoring

  • Son, Jung-Hyun;Lee, Jae-Ick;Yang, Ryung;Kim, Dong-Hyun
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.288.3-289
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    • 2003
  • Sphingolipid species are important second messengers due to their role in the mitogenesis, differentiation and apoptosis. We developed a new column liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) in combination with multiple reaction monitoring (MRM) method for the rapid, simultaneous and quantitative determination of unambiguous detecting sphingolipids in cell culture of human cancer cells (HL-60). (omitted)

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Determination of N-nitrosodimethylamine in zidovudine using high performance liquid chromatography-tandem mass spectrometry

  • Yujin Lim;Aelim Kim;Yong-Moon Lee;Hwangeui Cho
    • 분석과학
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    • 제36권6호
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    • pp.281-290
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    • 2023
  • Zidovudine is an antiretroviral agent prescribed for the prevention and treatment of human immunodeficiency virus/acquired immune deficiency syndrome (HIV/AIDS). It is typically recommended to be used in combination with other antiretroviral drugs. Zidovudine has the potential to generate N-nitrosodimethylamine (NDMA) in the presence of dimethylamine and nitrite salt under acidic reaction conditions during the drug manufacturing process. NDMA is a potent human carcinogen that may be detected in drug substances or drug products. An analytical method was developed to determine NDMA in pharmaceuticals including zidovudine using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The analysis involved reversed-phase chromatography on a Kinetex F5 column with a mobile phase comprising water-acetonitrile mixtures. The detection of positively charged ions was conducted using atmospheric pressure chemical ionization (APCI). The calibration curve demonstrated excellent linearity (r = 0.9997) across the range of 1-50 ng/mL with a highly sensitive limit of detection (LOD) at 0.3 ng/mL. The developed method underwent thorough validation for specificity, linearity, accuracy, precision, robustness, and system suitability. This sensitive and specific analytical method was applied for detecting NDMA in zidovudine drug substance and its formulation currently available in the market, indicating its suitability for drug quality management purposes.

Application of Fast Atom Bombardment Collision-induced Dissociation Tandem Mass Spectrometry for Structural identification of Glycerolipids Isolated From Marine Sponge

  • Lee, Sun-Young;Hong, Joo-Yeon;Jung, Jee-H.;Hong, Jong-Ki
    • Mass Spectrometry Letters
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    • 제2권1호
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    • pp.8-11
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    • 2011
  • Two types of glycerolipids [monoacylglycerols (MAG) and cyclitols] were isolated by reversed phase high-performance liquid chromatography from the methanol extracts of a marine sponge, and analyzed by fast atom bombardment mass spectrometry (FAB-MS) in positive-ion mode. FAB mass spectra of these compounds yielded protonated molecules $[M + H]^+$ and abundant sodiated molecules $[M + Na]^+$ from a mixture of 3-nitrobenzyl alcohol and NaI. The structures of these compounds were elucidated by FAB-collisional-induced dissociation (CID)-tandem mass spectrometry. We carried out collision-indused dissociation (CID) of these lipids in B/E-linked scan mode. The CID B/E-linked scan of $[M + H]^+$ and $[M + Na]^+$ precursor ions resulted in the formation of numerous characteristic product ions through a series of dissociative processes. The product ions formed by charge-remote fragmentation (CRF) provided important information for the identification of the acyl chain structure substituted at the glycerol backbone. Some of the product the ions were diagnostic for the presence of a glycerol backbone or acyl chain structure.

High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

  • Choi, Young-Wook;Nam, Dae-young;Kang, Kyoung-Hoon;Ha, Kyung-Wook;Han, In-Hee;Chang, Byung-Kon;Yoon, Mi-kyeong;Lee, Jae-hwi
    • Bulletin of the Korean Chemical Society
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    • 제27권2호
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    • pp.291-294
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    • 2006
  • A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC $C_{18}$ column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole.

Determination of Polar Secondary Metabolomes in Arabidopsis thaliana using High Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

  • Cho, Young-Ah;Park, Se-min;Bae, Dong-Won;Seo, On-Nuri;Lee, Ji-Eun;Jeong, Sung-Woo;Kwon, Young-Sang;Cha, Jae-Yul;Bae, Han-Hong;Shin, Sung-Chul
    • 농업생명과학연구
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    • 제46권6호
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    • pp.165-171
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    • 2012
  • As a preceding study for investigating the influence of sound wave stimulus on Arabidopsis thaliana metabolomics, the polar secondary metabolomes of the plant were determined using high performance liquid chromatography coupled with tandem mass spectrometry. A total of 10 polar secondary metabolomes were characterized and quantified. Among them, 4 metabolomes, p-coumaroylagmatine isomer (7 and 8), p-coumaroylagmatine isomer (9 and 10) were identified in the plant for the first time. The validation was conducted in terms of linearity, recovery, precision, limit of detection (LOD) and limit of quantification (LOQ). The validated method was applied to the simultaneous quantification of the 10 polar secondary metabolomes.

액체크로마토그래프-탠덤질량분석기(LC-MS/MS)를 이용한 소변 내 D-, L- Lactate 분리 및 정량 (Simultaneous Quantification of Urinary L-, and D-Lactate by Reversed-Phase Liquid Chromatography Tandem Mass Spectrometry)

  • 문철진;양송현
    • 대한유전성대사질환학회지
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    • 제15권2호
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    • pp.59-64
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    • 2015
  • 사람의 신체내에서 주로 존재하는 lactate는 L-lactate로서 몇몇 선천성대사이상과 관련하여 증가된다. 최근 2형 당뇨병(type 2 diabetes)과 만성적인 염증성 위장질환(inflammatory bowel disease)과 관련하여 증가되는 D-lactate를 L-lactate와 분리해야 하는 요구도가 높아졌다. 이에 액체크로마토그래프-탠덤질량 분석기를 사용하여 소변 내 D-, L-lactate를 분리하는 방법을 확립하였으며, 분석시간과 정밀성, 정확성, 특이성 등에서 신뢰성 있는 방법임을 확인하였다.