• Mass Spectrometry Letters
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• v.14 no.4
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• pp.141-146
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• 2023

Liraglutide is a medication prescribed for the management of type 2 diabetes and chronic obesity. A simple, sensitive, and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantitative analysis of liraglutide in rat plasma. After a simple protein precipitation step, liraglutide was chromatographically separated using the ACQUITY Premier Peptide BEH C18 Column with mobile phases comprising 50% acetonitrile and 50% methanol, and water with 0.3% FA. Positive ion electrospray ionization in multiple reaction monitoring mode was used to achieve detection. Good linearity was observed in the 5-600 ng/mL concentration range (R² > 0.99). Liraglutide had intra- and inter-day precision values of 2.13%-9.86% and 4.14%-8.36%, respectively. The accuracy ranged from -2.36% to 2.58%. The recovery and matrix effect were within acceptable limits. This selective LC-MS/MS method was used to study the pharmacokinetic properties of liraglutide after subcutaneous administration in rats.

• Journal of the Institute of Electronics Engineers of Korea SD
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• v.48 no.2
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• pp.55-60
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• 2011

Most of neural network chips use an analog-type maximum selector circuit (MS). As the increase of integration level, the analog MS has difficulties in achieving sufficient resolution. Contrary, the digital-type MS is easy to get high resolution but slower than its analog counterparts. A new high-speed digital MS circuit called MSIT (Maximum Selector with Internal Trigger-signal) is presented in this paper. The MSIT has been designed to achieves both the high reliability by using trigger-signals and high speed by removing the unnecessary waiting times. The response time of MSIT is 3.4ns for 32 data with 10-bit resolution in the simulation with 1.2V, $0.13{\mu}m$-process model parameters, which is much faster than its analog counterparts. It shows that digital MS circuits like MSIT can achieve higher speed as well as higher resolution than analog MS circuits.

• Journal of Korean Society on Water Environment
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• v.32 no.5
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• pp.410-418
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• 2016

This study was conducted to improve the analysis method used for N-nitrosamines and to investigate the occurrences of N-nitrosamines in tributaries of the Han-river, intake stations, water treatment plants and tap water used within the city of Seoul. The samples were pretreated through a solid phase extraction and analyzed using a gas chromatography tandem mass spectrometer (GC-MS/MS). The GC-MS/MS in CI mode was compared with the GC-MS/MS in EI mode by the method detection limits (MDLs). MDLs by GC-CI/MS/MS and GC-EI/MS/MS were 0.2 ~ 1.1 ng/L and 0.2 ~ 1.4 ng/L, respectively. Samples were collected from ten tributaries of the Han-river (T1 ~ T10), six intake stations (I1 ~ I6), six water treatment plants (P1 ~ P6) and 25 taps in Seoul city. The maximum levels of N-nitrosodimethylamine (NDMA) were 0.013 μg/L, 0.008 μg/L, 0.006 μg/L and 0.002 μg/L in tributary water, raw water, finished water and tap water samples, respectively. Detected levels were much lower than 0.1 μg/L corresponding to the guideline value of WHO.

• Food Science of Animal Resources
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• v.34 no.5
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• pp.656-664
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• 2014

The purpose of this study was to analyze myosin heavy chain (MHC) isoforms in bovine longissimus thoracis (LT) muscle by liquid chromatography (LC) and mass spectrometry (MS). LT muscles taken from Hanwoo (Korean native cattle) steer (n=3) used to separate myosin bands by sodium dodecyl sulfate-polyacrylamide gel electrophoresis. The peptide queries were obtained from the myosin bands by LC-MS/MS analysis following in-gel digestion with trypsin. A total of 33 and 43 queries were identified as common and unique peptides, respectively, of MHC isoforms (individual ions scores >43 indicate identity or extensive homology, p<0.05). MHC-1 (IIx), -2 (IIa), -4 (IIb), and -7 (slow/I) were identified based on the Mowse score (5118, 3951, 2526, and 2541 for MHC-1, -2, -4, and -7, respectively). However, more analysis is needed to confirm the expression of MHC-4 in bovine LT muscle because any query identified as a unique peptide of MHC-4 was not found. The queries that were identified as unique peptides could be used as peptide markers to confirm MHC-1 (14 queries), -2 (8 queries), and -7 (21 queries) in bovine LT muscle; no query identified as a unique peptide of MHC-4 was found. LC-MS/MS analysis is a useful approach to study MHC isoforms at the protein level.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.6 no.2
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• pp.134-143
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• 2005

Collagen is the important structural proteins in mammals with various peptide composition and cross-linkings. The direct analysis of collagen protein was not suitable because of its structural complexity and diversity. In this study, we suggest the simple way of collagen analysis by introducing matrix-assisted laser desorption/ionization time-of flight mass spectrometry (MALDI-TOF MS) to identify the collagen and its trypsin-digested fragments, and by subsequent time-of-flight tandem mass spectrometry(Q-TOF MS/MS) to analyze the amino acid sequences of identified fragments. Using the collagen samples extracted from the tail of mouse, 10 separated bands were found in SDS-PAGE, and the masses of most bands could be more finely determined by MALDI-TOF MS. When each 10 separated proteins was tryptic digested and introduced to MALDI-TOF, the Gly1056-Arg1073 fragment from $\alpha_1$-chain was identified in four bands, and the Gly1056-Arg1073 fragment from $\alpha_2$-chain was identified in five bands, both in type I collagen. Although few fragments were found because of the cross-linkings left in digested collagen sample, it could be determined that the type I collagen existed at least in 7 separated bands. When the amino acid sequences of two identified fragments were analyzed by Q-TOF MS/MS, both sequences were identical with those determined by MALDI-TOF MS. It suggested that the two peaks in MALDI-TOF MS caused by the fragments identified in this work could be used as the fingerprint to simply identify type I collagen in protein samples.

• Analytical Science and Technology
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• v.25 no.1
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• pp.83-90
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• 2012

The objective of the study was to estimate the measurement uncertainty associated with determination of creatinine (Cr) in urine samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Centrifuged urine samples (10 ${\mu}L$) were diluted with 390 ${\mu}L$ of distilled water. To 20 ${\mu}L$ aliquots of diluted urine samples, 30 ${\mu}L$ of internal standard solution (Cr-$d_3$, 5 ${\mu}g/mL$) and 10 ${\mu}L$ of acetonitrile were added and filtered. The samples (1 ${\mu}L$) were introduced into LC-MS/MS with no further pretreatment. Cr was separated on a multi-mode ODS column (Scherzo SM-C18, 75 ${\times}$ 2.0 mm I.D., 3 ${\mu}m$) and quantified by LC-MS/MS operating in MRM mode (Cr, m/z 114.0${\rightarrow}$ 86.0; Cr-$d_3$, m/z 117.0${\rightarrow}$ 89.1). The four factors that contribute uncertainty to the final result were extracted and evaluated. The principal factors of contribution to combined standard uncertainty were sample dilution, calibration curve and repeatability, while the preparation of standard solution was only a minor factor. Relative extended uncertainty of the measured concentration was 14.2% in a real urine sample.

• YAKHAK HOEJI
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• v.52 no.5
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• pp.407-411
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• 2008

Phosphorylation plays the most important role in cell signaling mechanism. Various methods to identify the phosphorylation sites of proteins using tandem mass spectrometry (MS/MS) have been reported recently. Furthermore, the enrichment strategy such as Titanium dioxide ($TiO_2$) method should be combined with MS/MS analysis to effectively identify phosphorylation sites. It is necessary to optimize phosphopeptide-enrichment strategy, $TiO_2$ method in this study, due to the low amount of phosphorylated form followed by analyzing them by MS/MS. To evaluate the several conditions to enrich phosphopeptides using $TiO_2$ method, we used ${\apha}$-casein as a standard phosphoprotein and analyzed a representative phosphopeptide (VPQLEIVPNpSAEER) peak of MS spectrum. Batch is better than column method for binding and 300 g/l DHB in loading buffer is better than lower concentration of DHB. 3% TFA and pH 10.5 shows high efficiency of phosphopeptide-enrichment for washing and elution steps, respectively. Finally we identified various efficient conditions of phosphopeptide-enrichment method using $TiO_2$. This optimized method would assist in reliable identifying thousands of phosphorylation sites existed in low abundance from various complex proteins.

• Korean Journal of Biological Psychiatry
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• v.18 no.1
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• pp.46-54
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• 2011

Objectives : The objective of this study is to assess the prevalence and risk factors of metabolic syndrome (MS) among inpatients with schizophrenia, and to compare with general population. Methods : Nine hundreds seventy inpatients were included to assess the prevalence of MS from two mental hospitals in Yong-in city. Assessment of MS was performed based on modified American Heart Association criteria with abdominal obesity threshold of 90cm for men, 85cm for women. Comparative analysis was performed using age- and gender matched sample from Korea Health and Nutritional Examination Survey III. For evaluating risk factors, analysis included 766 inpatients taking consistent medications at least for 30 days. Results : The prevalence of MS of inpatients with schizophrenia was 26.2%, in females it was 33.2%, compared to 20.2% in males(p < 0.001). Compared to general population, the prevalence of MS was significantly lower in male and higher in female patients. In terms of criteria prevalence, who met abdominal circumference criterion were more prevalent in patient group(p < 0.001). After multivariate analysis, female gender and old age remained as risk factors of MS. Conclusions : The prevalence of MS of inpatients with schizophrenia was 26.2% and significantly low compared to general population. Female gender and old age were risk factors of MS.

• Mass Spectrometry Letters
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• v.2 no.2
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• pp.37-40
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• 2011

Saccharin is a commonly used artificial sweetener in foodstuffs. However, for its carcinogenic dispute, it has been regulated by government bodies. In this study, isotope dilution mass spectrometry (ID-MS) was introduced for the accurate quantification of saccharin. To employ ID-LC/MS, we obtained its isotope analogue, $^{13}C_1$-sodium saccharin, by customized synthesis. Samples were spiked with $^{13}C_1$-sodium saccharin and analyzed with LC/MS in negative mode. Chromatographic conditions were optimized for the adequate chromatographic retention and separation of saccharin with a $C_{18}$ column. MS was operated with electrospray ionization by the selected ion monitoring (SIM) mode of $[M-H]^-$ for saccharin (m/z 182) and $[M-Na]^-$ for its isotope analogue (m/z 183). To validate the ID-LC/MS method for accurate measurement, we prepared a batch of a candidate material by sortifying quasi-tea-drinks with saccharin and analyzed samples gravimetrically fortified in various levels of concentration. The repeatability and reproducibility of this method was tested by analyzing the reference material. Result show that ID-LC/MS is a reliable method for the quantitative analysis of saccharin.

• Analytical Science and Technology
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• v.35 no.2
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• pp.60-68
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• 2022

In this study, we developed and validated a sensitive analytical method to quantify baphicacanthin A in mouse plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The standard calibration curves for baphicacanthin A ranged from 0.5 to 200 ng/mL and were linear, with an r² of 0.985. The inter- and intra-day accuracy and precision and the stability fell within the acceptance criteria. Besides, we investigated the pharmacokinetics of baphicacanthin A following its intravenous (5 mg/kg) and oral administration (30 mg/kg). Intravenously injected baphicacanthin A showed biphasic elimination kinetics with high clearance and volume of distribution values. Furthermore, baphicacanthin A showed a rapid absorption but low aqueous solubility (182.51±0.20 mg/mL), resulting in low plasma concentrations and low oral bioavailability (2.49 %). Thus, we successfully documented the pharmacokinetic properties of baphicacanthin A using this newly developed sensitive LC-MS/MS quantification method, which could be used in future lead optimization and biopharmaceutic studies.