• 제목/요약/키워드: liquid chromatography-mass spectrometry (LC-MS)

검색결과 459건 처리시간 0.032초

Optimization of Solid Phase Extraction Method for Quantitative Analysis of Perfluorooctanoic Acid in Serum using Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Hyun-Seok;Yim, Yong-Hyeon
    • Mass Spectrometry Letters
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    • 제5권1호
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    • pp.30-33
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    • 2014
  • A solid phase extraction (SPE) method was optimized for the quantitative analysis of perfluorooctanoic acid (PFOA) in serum using hydrophilic-lipophilic balance SPE and LC-MS/MS. Fetal bovine serums spiked with $^{13}C_8$-PFOA before or after SPE were used as test samples for evaluation of the SPE efficiency. Simultaneous evaluation of matrix effects and absolute SPE recovery for $^{13}C_8$-PFOA in serum using different sample pre-treatments and SPE conditions allowed optimization of SPE process efficiency with minimal matrix effect and decent SPE recovery. Introduction of protein precipitation as a sample pre-treatment procedure for serum samples before SPE generally decreased matrix effect in LC-MS/MS analysis and provided more stable recovery of PFOA.

Simple and Robust Measurement of Blood Plasma Lysophospholipids Using Liquid Chromatography Mass Spectrometry

  • Ji, Dong Yoon;Lee, Chang-Wan;Park, Se Hee;Lee, Eun Jig;Lee, Do Yup
    • Mass Spectrometry Letters
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    • 제8권4호
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    • pp.109-113
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    • 2017
  • Single analytical procedure including extraction, liquid chromatography, and mass spectrometric analysis was evaluated for the simultaneous measurement of lysophospholipids (LPLs). LPLs, particularly, lysophosphatidic acids (LPA) and sphingosine 1-phosphate (S1P) are lipid messengers ubiquitously found in various biological matrix. The molecular species mediate important physiological roles in association with many diseases (e.g. cancer, inflammation, and neurodegenerative disease), which emphasize the significance of the simple and reliable analytical method for biomarker discovery and molecular mechanistic understanding. Thus, we developed analytical method mainly focusing on, but not limited by those lipid species S1P and LPA using reverse phase liquid chromatography-tandem mass spectrometry (RPLC-ESI-MS-MS). Extraction method was modified based on Folch method with optimally minimal level of ionization additive (ammonium formate 10 mM and formic acid). Reverse-phase liquid-chromatography was applied for chromatographical separation in combination with negative ionization mode electrospray-coupled Orbitrap mass spectrometry. The method validation was performed on human blood plasma in a non-targeted lipid profiling manner with full-scan MS mode and data-dependent MS/MS. The proposed method presented good inter-assay precision for primary targets, S1P and LPA. Subsequent analysis of other types of LPLs identified a broad range of lysophosphatidylcholines (LPCs) and lysophosphatidyl-ethanolamines (LPEs).

Putative multiple reaction monitoring strategy for the comparative pharmacokinetics of postoral administration Renshen-Yuanzhi compatibility through liquid chromatography-tandem mass spectrometry

  • Sun, Yufei;Feng, Guifang;Zheng, Yan;Liu, Shu;Zhang, Yan;Pi, Zifeng;Song, Fengrui;Liu, Zhiqiang
    • Journal of Ginseng Research
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    • 제44권1호
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    • pp.105-114
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    • 2020
  • Background: Exploring the pharmacokinetic (PK) changes of various active components of single herbs and their combinations is necessary to elucidate the compatibility mechanism. However, the lack of chemical standards and low concentrations of multiple active ingredients in the biological matrix restrict PK studies. Methods: A putative multiple reaction monitoring strategy based on liquid chromatography coupled with mass spectrometry (LC-MS) was developed to extend the PK scopes of quantification without resorting to the use of chemical standards. First, the compounds studied, including components with available reference standard (ARS) and components lacking reference standard (LRS), were preclassified to several groups according to their chemical structures. Herb decoctions were then subjected to ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry analysis with appropriate collision energy (CE) in MS2 mode. Finally, multiple reaction monitoring transitions transformed from MS2 of ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry were used for ultrahigh-performance liquid chromatography coupled with triple quadrupole mass spectrometry to obtain the mass responses of LRS components. LRS components quantification was further performed by developing an assistive group-dependent semiquantitative method. Results: The developed method was exemplified by the comparative PK process of single herbs Radix Ginseng (RG), Radix Polygala (RP), and their combinations (RG-RP). Significant changes in PK parameters were observed before and after combination. Conclusion: Results indicated that Traditional Chinese Medicine combinations can produce synergistic effects and diminish possible toxic effects, thereby reflecting the advantages of compatibility. The proposed strategy can solve the quantitative problem of LRS and extend the scopes of PK studies.

Keratanase II Digestion Accompanied with a Liquid Chromatography/Tandem Mass Spectrometry for Urinary Keratan Sulfate Quantitative Analysis

  • Chuang, Chih-Kuang;Lin, Hsiang-Yu;Wang, Tuen-Jen;Huang, Sung-Fa;Lin, Shuan-Pei
    • Journal of mucopolysaccharidosis and rare diseases
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    • 제3권1호
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    • pp.20-27
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    • 2017
  • Purpose: Mucopolysaccharidosis IV (MPS IV) is a disease characterized by deficient activity of N-acetylgalactosamine-6-sulfatase (GALNS) causing excessive lysosomal storage of keratan sulfate (KS). The identification of the relevant disaccharide units of KS after keratanase II digestion followed by liquid chromatography/tandem mass spectrometry detection (LC-MS/MS) is validated and applicable for the preliminary diagnosis of MPS IV. Methods: A total of 67 urine samples were collected and analyzed from 11 MPS IV patients comprising 10 MPS IVA and one MPS IVB patients, and 56 normal controls. Urinary glycosaminoglycan was first precipitated by the Alcian blue method followed by a digestion of keratanase II. The protonated species of the digested disaccharide products were detected by using multiple reaction monitoring experiment. Results: One particular disaccharide of KS was selected. The transition mass-to-charge (m/z) of the parent ion and its daughter ion after collision was $462.0{\rightarrow}97.0$, whereas the chondrosine used as an internal standard in this assay was m/z $353.9{\rightarrow}73.0$. The results corresponded well with the two-dimensional electrophoresis method. The quantities of urinary KS were significantly raised in confirmed MPS IV patients when comparing with those of normal controls ($170.2{\pm}81.1$ vs. $4.06{\pm}1.92{\mu}g/mL$). Conclusion: The LC-MS/MS method for MPS IVA determination is specific, sensitive, validated, and applicable for urinary KS quantification. This method can be used not only as a first-line biochemistry examination of MPS IVA, but also as an outcome survey after enzyme replacement therapy.

LC/MS에 의한 원료생강 및 생강 페이스트 중의 Gingerol 화합물 분석 (Analysis of Gingerol Compounds of Raw Ginger (Zingiber officinale Roscoe) and Its Paste by High Performance Liquid Chromatograph-Mass Spectrometry (LC/MS))

  • 조길석
    • 한국식품영양과학회지
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    • 제29권5호
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    • pp.747-751
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    • 2000
  • 본 연구에서는 생각의 매운맛을 주요성분인 gingerol 화합물의 분석방법을 개선할 목적으로, 원료 생각을 아세톤으로 추출한 후 그 추출물을 TLC 및 LiChrosorb RP-18 column으로 장착된 HPLC를 사용하여 3가지 gingerol 동족체 화합물을 분리하였고, LC/MS 및 NMR로 확인한 결과 생강의 동족체 화합물은 [6]-, [8]-, [10]-gingerol로 확인되었다. 본 방법으로 추출한 gingerol 표준품을 사용하여 시판 원료생강 및 생각 페이스트 중의 gingerol 함량을 측정한 결과, 전자의 경우 [6]-, [8]-, [10]-gingerol 함량은 635.5 mg%, 206.6 mg%, 145.7 mg%이었고, 후자의 경우는 418.2 mg%, 142.6 mg%, 103.3 mg%로 각각 구성되어 있었다.

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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
    • 분석과학
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    • 제30권2호
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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.

Identfication of Phase I and Phase II Metabolites of Hesperetin in Rat Liver Microsomes by Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry

  • Kim, Un-Yong;Han, Sang-Beom;Kwon, Oh-Seung;Yoo, Hye-Hyun
    • Mass Spectrometry Letters
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    • 제2권1호
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    • pp.20-23
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    • 2011
  • The purpose of this study is to investigate the in vitro metabolism of hesperetin, a bioflavonoid. Hesperetin was incubated with rat liver microsomes in the presence of NADPH and UDP-glucuronic acid for 30 min. The reaction mixture was analyzed by liquid chromatography-ion trap mass spectrometer and the chemical structures of hesperetin metabolites were characterzed based on their MS/MS spectra. As a result, a total of five metabolites were detected in rat liver microsomes. The metabolites were identified as a de-methylated metabolite (eriodictyol), two hesperetin glucuronides, and two eriodictyol glucuronides.

Profiling of the leaves and stems of Curcuma longa using LC-ESI-MS and HPLC analysis

  • Gia Han Tran;Hak-Dong Lee;Sun-Hyung Kim;Seok Lee;Sanghyun Lee
    • Journal of Applied Biological Chemistry
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    • 제66권
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    • pp.338-344
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    • 2023
  • Curcuma longa is a plant belonging to the genus Curcuma and is distributed across various Asian regions. This plant is widely known for its rhizomes, which possess a variety of pharmacological properties. However, although the leaves and stems of this plant also contain several health-promoting secondary metabolites, very few studies have characterized these compounds. Therefore, our study sought to quantify the secondary metabolites from the leaves and stems of Curcuma longa L. (LSCL) using liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) and high-performance liquid chromatography (HPLC). Our LC-ESI-MS analyses detected twenty-one phenolic compounds in the LSCL, among which fifteen compounds were detected via HPLC analysis. Four compounds, namely vanillic acid (0.129 mg/g), p-coumaric acid (0.431 mg/g), 4-methylcatechol (0.199 mg/g), and afzelin (0.074 mg/g) were then quantified. These findings suggest that LSCL is rich in secondary metabolites and holds potential as a valuable resource for the development of functional and nutritional supplements in the future.

Quantitative measurement of salivary testosterone in Korean adults by stable isotope-dilution liquid chromatographyelectrospray-tandem mass spectrometry

  • Lee, Sang-Hoo;Kwon, Soon-Ho;Shin, Hye-Jin;Park, Ji-Myeong;Lim, Hwan-Sub;Lee, Kyoung-Ryul;Kim, Young-Jin
    • BMB Reports
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    • 제43권11호
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    • pp.761-765
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    • 2010
  • Salivary testosterone levels in Korean adults were quantitatively measured for the first time by liquid chromatography-electrospray-tandem mass spectrometry (LC ESI MS/MS). Salivary testosterone was separated on a multiple reaction monitoring (MRM) chromatogram within 7 min. The LC ESI MS/MS assay was validated over the linearity range of 0.01-2.00 ng/ml (r=0.99987) using testosterone-$d_3$ as an internal standard. The lower limit of quantification (LOQ) was 0.01 ng/ml. The intra- and inter-assay precisions were 1.54% to 4.09% and 0.96% to 4.29%, respectively. The mean recovery was 93.32% (range 88.43-98.05%). The validated assay was then applied to measure the salivary testosterone levels of Korean adults. In men, the salivary testosterone level collected between 9:00-11:00 am was approximately 2.8 times higher than that in women (P < 0.0001). Salivary testosterone levels in both sexes negatively correlated with age. The present assay would also be useful in measuring salivary testosterone levels in clinical laboratories.