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Investigation of Angiotensin Glycosylation by MALDI-TOF and ESI Tandem Mass Spectrometry
Park, Soo-Jin,Park, Deok-Hie,Sul, Soo-Hwan,Oh, Sung-Hwan F.,Park, In-Sook,Chung, Doo-Soo,Kim, Hie-Joon,Kim, Min-Sik,Lee, Sang-Won Korean Chemical Society 2004 Bulletin of the Korean Chemical Society Vol.25 No.12
Angiotensin I, a model decapeptide, was glycosylated and partially hydrolyzed with HCl (6 N, 80 $^{\circ}C$, 4 h), aminopeptidase, and carboxypeptidase Y. A single peptide mass map obtained from truncated peptides in the partial acid hydrolysate of angiotensin and its glycosylation product mixture by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry enabled sequencing of angiotensin by a combinatorial procedure. MALDI-TOF and electrospray ionization (ESI) tandem mass spectrometric results indicate that both the N-terminal amino group of aspartic acid and the guanidinium group of the second residue arginine are glycosylated.
( Deok-hie Park ),( Yeu Young Youn ),( Jaewon Choi ),( Young-hee Lim ),( Hye-sung Choa ) 한국질량분석학회 2011 Mass spectrometry letters Vol.2 No.1
The Korean government has regulated emission of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in waste water of manufacturing facilities producing chlorinated compounds since 2009. As this regulation is expected to be reinforced in 2013 to 50 pg I-TEQ/L, a large sample volume is required for the analysis of trace amounts of PCDD/Fs in waste water. Liquid-liquid extraction (LLE) is used to extract PCDD/Fs from aqueous samples; however, its low efficiency makes it inadequate for analyzing large sample volumes. Herein, we present a disk-type solid-phase extraction (SPE) method for the analysis of dioxin at a part per quadrillion level in waste water. This SPE system contains airtight glass covers with a decompression pump, which enables continuous semi-automated extraction. Small (0.5 L) and large (7 L) samples were extracted using LLE and SPE methods, respectively. The method detection limits (MDLs) were 0.001-0.25 and 0.015-4.1 pg I-TEQ/L for the SPE and LLE methods, respectively. The concentrations of detected congeners with both methods were similar. However, the concentrations of several congeners that were not detected with the LLE method were quantified using the SPE method.
Park, Deok-Hie,Youn, Yeu-Young,Choi, Jae-Won,Lim, Young-Hee,Cho, Hye-Sung Korean Society for Mass Spectrometry 2011 Mass spectrometry letters Vol.2 No.1
The Korean government has regulated emission of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in waste water of manufacturing facilities producing chlorinated compounds since 2009. As this regulation is expected to be reinforced in 2013 to 50 pg I-TEQ/L, a large sample volume is required for the analysis of trace amounts of PCDD/Fs in waste water. Liquid-liquid extraction (LLE) is used to extract PCDD/Fs from aqueous samples; however, its low efficiency makes it inadequate for analyzing large sample volumes. Herein, we present a disk-type solid-phase extraction (SPE) method for the analysis of dioxin at a part per quadrillion level in waste water. This SPE system contains airtight glass covers with a decompression pump, which enables continuous semi-automated extraction. Small (0.5 L) and large (7 L) samples were extracted using LLE and SPE methods, respectively. The method detection limits (MDLs) were 0.001.0.25 and 0.015.4.1 pg I-TEQ/L for the SPE and LLE methods, respectively. The concentrations of detected congeners with both methods were similar. However, the concentrations of several congeners that were not detected with the LLE method were quantified using the SPE method.
Investigation of Angiotensin Glycosylation by MALDI-TOF and ESI Tandem Mass Spectrometry
박수진,Deok-Hie Park,설수환,오성환,박인숙,정두수,김희준,김민식,이상원 대한화학회 2004 Bulletin of the Korean Chemical Society Vol.25 No.12
Angiotensin I, a model decapeptide, was glycosylated and partially hydrolyzed with HCl (6 N, 80 oC, 4 h), aminopeptidase, and carboxypeptidase Y. A single peptide mass map obtained from truncated peptides in the partial acid hydrolysate of angiotensin and its glycosylation product mixture by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry enabled sequencing of angiotensin by a combinatorial procedure. MALDI-TOF and electrospray ionization (ESI) tandem mass spectrometric results indicate that both the N-terminal amino group of aspartic acid and the guanidinium group of the second residue arginine are glycosylated.
( Young-hee Lim ),( Deok-hie Park ),( Yeu Young Youn ),( Kyung Hoon Kim ),( Hye-sung Cho ) 한국질량분석학회 2011 Mass spectrometry letters Vol.2 No.1
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 O18-labeled hydrogen peroxide. In addition, density-functional calculations were carried out for six possible oxidation products to support the experimental results.
Lim, Young-Hee,Park, Deok-Hie,Youn, Yeu-Young,Kim, Kyung-Hoon,Cho, Hye-Sung Korean Society for Mass Spectrometry 2011 Mass spectrometry letters Vol.2 No.1
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.