• Title/Summary/Keyword: liquid chromatography mass spectrometry

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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
    • Proceedings of the PSK Conference
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    • 2003.04a
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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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Simultaneous quantitation of enalapril and enalaprilat in human plasma by high-throughput solid phase extraction and liquid chromatography/tandem mass spectrometry

  • Son, Jung-Hyun;Lee, Jae-Ick;Kim, Dong-Hyun
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.401.3-402
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    • 2002
  • Enalapril (ENP) maleate is effective drug for the treatment of renivascular hypertension and heart failure. ENP acts as inhibitor of the enzyme angiotensin-convertase (ACE-inhibitor) and metabolized to enalaprilat (ENPT), which is the active metabolite that is really responsible for the therapeutic action. In the present study, a sensitive and rapid liquid chromatography/ electrospray ion trap tandem mass spectrometry (LC/MS/MS) method combined with high-throughput solid phase extraction (SPE) has been developed and validated for the simultaneous quantitative determination of ENP and ENPT in human plasma. (omitted)

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Determination of lisinopril in human plasma by liquid chromatography tendem mass spectrometry and its application to human bioavailibility study

  • Shim, Hee-Ok;Kim, Dong-Chul
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.239.1-239.1
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    • 2003
  • This study was to develop a quantification method of lisinopril using liquid chromatography tendem mass spectrometry in human plasma. Quntitation of lisinopril by MRM(multiple reaction monitoring) in the electrospray positive mode was validated according to FDA guideline. Extraction of lisinopril and enalapril as internal standard from plasma was perfomed by means solide phase extraction. The calibration curve of lisinopril showed a good linerarity in the concentration range 2∼200ng/ml. The coefficients of variations for the inter-day and intra-day precision was less than 15%, and the inter-day and intra-day accuracy was 97.6∼101.0%. (omitted)

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Isolation and Structural Characterization of an Oligosaccharide Produced by Bacillus subtilis in a Maltose-Containing Medium

  • Shin, Kwang-Soon
    • Preventive Nutrition and Food Science
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    • v.21 no.2
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    • pp.124-131
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    • 2016
  • Among 116 bacterial strains isolated from Korean fermented foods, one strain (SS-76) was selected for producing new oligosaccharides in a basal medium containing maltose as the sole source of carbon. Upon morphological characterization using scanning electron microscopy, the cells of strain SS-76 appeared rod-shaped; subsequent 16S rRNA gene sequence analysis revealed that strain SS-76 was phylogenetically close to Bacillus subtilis. The main oligosaccharide fraction B extracted from the culture supernatant of B. subtilis SS-76 was purified by high performance liquid chromatography. Subsequent structural analysis revealed that this oligosaccharide consisted only of glucose, and methylation analysis indicated similar proportions of glucopyranosides in the 6-linkage, 4-linkage, and non-reducing terminal positions. Matrix-assisted laser-induced/ionization time-of-flight/mass spectrometry and electrospray ionization-based liquid chromatography-mass spectrometry/mass spectrometry analyses suggested that this oligosaccharide consisted of a trisaccharide unit with 1,6- and 1,4-glycosidic linkages. The anomeric signals in the $^1H$-nuclear magnetic resonance spectrum corresponded to ${\alpha}$-anomeric configurations, and the trisaccharide was finally identified as panose (${\alpha}$-D-glucopyranosyl-1,6-${\alpha}$-D-glucopyranosyl-1,4-D-glucose). These results suggest that B. subtilis SS-76 converts maltose into panose; strain SS-76 may thus find industrial application in the production of panose.

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
    • Analytical Science and Technology
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    • v.36 no.2
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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.

High Purity Extraction and Simultaneous High-performance Liquid Chromatography Analysis of Curcuminoids in Turmeric (강황에서 curcuminoids의 고순도 추출 및 고성능 액체 크로마토그래피 동시분석)

  • Lee, Kwang-Jin;Ma, Jin-Yeul;Kim, Young-Sik;Kim, Dong-Seon;Jin, Yinzhe
    • Journal of Applied Biological Chemistry
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    • v.55 no.1
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    • pp.61-65
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    • 2012
  • Three major curcuminoids in turmeric (Curcuma longa), curcumin, demethoxycurcumin, and bisdemethoxycurcumin, were efficiently extracted by optimizing extraction condition and simultaneously analyzed and identified using reverse phase high-performance liquid chromatography, thin-layer chromatography, and liquid chromatography-mass spectrometry method. The highest yield of extraction amount 0.279 g, 9.30% was obtained by dipping method with extraction time of 7 h.

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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    • v.66
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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.

In Vitro and in Vivo Metabolism of Salsolinol, on Endogenous Isoquinoline Neurotoxin, in Rats

  • Rhee, Hee-Kyung;Kwon, Oh-Seung;Ryu, Jae-Chun
    • Environmental Mutagens and Carcinogens
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    • v.21 no.1
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    • pp.30-33
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    • 2001
  • Salsolinol (1-methyl-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline, SAL), a dopaminergic isoquinoline neurotoxin, has been implicated to contribute the etiology of Parkinson's disease and neuropathology of chronic alcoholism. In our previous results, SAL was reported to have the mutagenicity and clastogenicity not in bacteria but in mammalian cells, and its genotoxic potential was known to be potentiated in the presence of rat liver S-9 fraction. This may indicate that some metabolite(s) of SAL was involved in the mutagenic potentials. To investigate the SAL metabolites, the metabolism studies of SAL were conducted in vitro rat liver S-9 fraction and in vivo using rats by high performance liquid chromatography and gas chromatography/mass spectrometry. The methylated metabolite of SAL was found in urine of rats, while the same methylating form of metabolite was not produced from the in vitro metabolism system using rat liver S-9 fraction.

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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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    • v.43 no.11
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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.