• Bulletin of the Korean Chemical Society
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• 제32권12호
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• pp.4415-4418
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• 2011

• Bulletin of the Korean Chemical Society
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• 제28권5호
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• pp.840-842
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• 2007

• Mass Spectrometry Letters
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• 제7권1호
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• pp.26-29
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• 2016

Simultaneous determination of three corticosteroids (clobetasol propionate, betamethasone dipropionate, fluticasone propionate) in moisturizers was performed by using liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS). Sample preparation was conducted by the liquid-liquid extraction (LLE). Moisturizers include emulsifying agent and it forms micelles. In order to improve the extraction efficiency of corticosteroids trapped in micelle, newly developed-optimized extraction conditions which can remove the matrix effect from moisturizers was applied with various pH conditions in LLE extraction stage of sample preparation. Thus, the addition of 10 μL of 1 M HCl into moisturizers sample before extraction could improve the extraction efficiency. For the quantitative analysis, SRM table that contained specific transition of all of target corticosteroids was created. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), limit of quantization (LOQ) and recovery. Over the 0.99 r² value was obtained in calibration standard range. Effective accuracy and precision were also obtained. LODs were below 31 ng/mL and LOQs were estimated below 94 ng/mL for all corticosteroids tested.

• Mass Spectrometry Letters
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• 제2권2호
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• pp.41-44
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• 2011

Molecular compositions of two types of heavy oil were studied using positive atmospheric pressure photoionization (APPI) Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS). Vacuum gas oil (VGO) was generated from vacuum distillation of atmospheric residual oil (AR), and slurry oil (SLO) was generated from catalytic cracking of AR. These heavy oils have similar boiling point ranges in the range of 210-$650^{\circ}C$, but they showed different mass ranges and double-bond equivalent (DBE) distributions. Using DBE and carbon number distributions, aromatic ring distributions, and the extent of alkyl side chains were estimated. In addition to the main aromatic hydrocarbon compounds, those containing sulfur, nitrogen, and oxygen heteroatoms were identified using simple sample preparation and ultra-high mass resolution FT-ICR MS analysis. VGO is primarily composed of mono- and di-aromatic hydrocarbons as well as sulfur-containing hydrocarbons, whereas SLO contained mainly polyaromatic hydrocarbons and sulfur-containing hydrocarbons. Both heavy oils contain polyaromatic nitrogen components. SLO inludes shorter aromatic alkyl side chains than VGO. This study demonstrates that APPI FT-ICR MS is useful for molecular composition characterization of petroleum heavy oils obtained from different refining processes.

• Mass Spectrometry Letters
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• 제6권3호
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• pp.53-58
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• 2015

Recombinant erythropoietins (EPOs) are an important class of biotherapeutics that stimulate red blood cell production. The quality, safety, and potency of EPO variants are determined largely by their glycosylation, which makes up nearly half their mass. Thus, detailed glycomic analyses are important to assess biotherapeutic quality and establish the equivalency of biosimilar EPOs now coming to market. High-resolution mass spectrometry (MS) has recently emerged as the premier tool for glycan analysis in EPOs. Using the accurate mass measurements provided by high-resolution MS, the compositions of even large, complex glycans can easily be determined. When combined with a nano-LC separation, differentiation of structural isomers also becomes a possibility. These components, together, provide a comprehensive picture of biotherapeutic glycosylation. In this review, we provide an overview of MS-based analytical platform for glycomic characterization of EPO biotherapeutics and biosimilars.

• 분석과학
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• 제16권1호
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• pp.82-89
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• 2003

Isotope dilution mass spectrometry (IDMS) was applied to the determination of Ni, Cr, Mo in low alloy steel reference materials. The Mo isotope ratio measurement was performed by dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP/MS) using ammonia as a reaction cell gas. In the case of Ni and Cr measurement, all data were obtained at medium resolution mode (m/${\Delta}m=3000$) of double focusing sector field high resolution inductively coupled plasma mass spectrometry (HR-ICP/MS). For the method validation of the technique was assessed using the certified reference materials such as NIST SRM 361, NIST SRM 362, NIST SRM 363, NIST SRM 364, NIST SRM 36b. This method was applied to the determination of Ni, Cr and Mo in low alloy steel sample (CCQM-P25) provided by NMIJ for international comparison study.

• Mass Spectrometry Letters
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• 제12권2호
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• pp.31-40
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• 2021

Probable human carcinogenic compounds nitrosamines, have been detected as by-product impurities in sartan pharmaceuticals in recent years which has drawn worries for medication safety. To provide a sensitive and effective method for the quality control of sartan pharmaceuticals, this study established a feasible gas chromatography-tandem mass spectrometry (GC-MS/MS) method for simultaneous determination of 13 nitrosamines. The target analytes were separated on a DB-WAX Ultra Inert column (30 m × 0.25 mm; i.d., 0.25 ㎛) and were then subjected to electron impact ionization in multiple reaction monitoring mode. The established method was validated and further employed to analyze authentic samples. Limits of detection (LODs) and limits of quantification (LOQs) of the 13 nitrosamines were 15-250 ng/g and 50-250 ng/g, respectively, which also exhibited intra-day and inter-day accuracies of 91.4-104.8%, thereby satisfying validation criteria. Five nitrosamines, viz., N-nitrosodiethylamine, N-nitrosodimethylamine, N-nitrosodiphenylamine, N-nitrosomorpholine, and N-nitrosopiperidine were detected at concentrations above their LODs in 68 positive samples out of 594 authentic samples from seven sartans.

• Mass Spectrometry Letters
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• 제15권3호
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• pp.149-157
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• 2024

The objective of the present study was to validate the analytical procedure for the quantitative determination of four trace metals (As, Cd, Pb, and Hg) in extracted fish lipids using Inductively Coupled Plasma-Mass Spectrometry, ICP-MS. The extracted lipids using Bligh and Dyer method were digested by means of microwave-assisted acid digestion and introduced into an optimized ICP-MS instrument. The validation of the analytical method was carried out in accordance with the international standards and guidelines outlined in the European Pharmacopeia (2022), which included specificity, selectivity, linearity, limit of detection, limit of quantification, precision, and accuracy. The linearity ranges of the calibration curves were R² > 0.999, while the relative standard deviation (%RSD) for precision was within 5%. All targeted trace metals have shown mean recoveries between 88.0%-114.9%. The obtained LOD and LOQ values for this analytical protocol indicated the ability to detect and quantify of As, Cd, Pb, and Hg at trace levels. The overall validation confirms the described analytical method was appropriate for routine analyses of As, Cd, Pb, and Hg in fish lipids.

• Mass Spectrometry Letters
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• 제15권3호
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• pp.158-165
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• 2024

Pneumonia is an acute respiratory infection that primarily affects the lungs and is caused by various microorganisms, including viruses, fungi, and bacteria. Klebsiella pneumoniae, a multidrug-resistant (MDR) and extensively drug-resistant (XDR) bacterium, is a leading cause of widespread pneumonia. This study aimed to identify endophytic bacteria from the leaves of Acalypha indica L. and evaluate their antibacterial properties through both in vitro and in silico approaches. The objectives included isolating endophytic bacteria from Acalypha indica L., testing their antibacterial activity against Klebsiella pneumoniae, identifying the selected bacterial isolates using molecular techniques, analyzing their secondary metabolites via gas chromatography-mass spectrometry (GC-MS), and performing in silico molecular docking studies. The study identified BE 4, an endophytic bacterial isolate of Bacillus pumilus, as exhibiting the most potent antibacterial activity against Klebsiella pneumoniae. GC-MS analysis of the ethyl acetate extract of this isolate revealed 1,2-benzenedicarboxylic acid, bis(2-methylpropyl) ester as the primary metabolite component. Furthermore, molecular docking analysis identified two natural compound ligands, 1,2-benzenedicarboxylic acid, diethyl ester (-6.5 kcal/mol), and lilial (-6.2 kcal/mol), as having potential efficacy against drugresistant bacteria responsible for pneumonia. These findings suggest that endophytic bacteria and their bioactive compounds could serve as promising candidates for the development of new treatments against drug-resistant pneumonia.

• Food Science and Biotechnology
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• 제17권3호
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• pp.508-513
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• 2008

Erythromycin has been used to treat Streptococosis, Edwardsiel1osis, Vibriosis, Bacterial enteritis in the cultured fish. In this study, a rapid and effective erythromycin analysis method with new sample treatment protocol and liquid chromatography/tandem mass spectrometry (LC/MS/MS) system for fish products was developed. For the erythromycin extraction from fish muscle, the solvent mixture composed of 0.2% meta-phosphoric acid and methanol (6:4) showed good recovery rate, and the optimum extraction solvent volume was 20 mL. Erythromycin detection using LC/MS/MS were carried out under electro spray ionization (ESI) positive condition and erythromycin mass value 576.2 and 157.9. And the detection limit of the established method was 0.005 mg/kg in fish products. The recovery rate of the developed method applied to the fish species were as following, olive flounder, $87.6{\pm}5.0%$; black rockfish, $87.2{\pm}6.4%$; eel, $85.2{\pm}4.8%$; and rainbow trout, $86.0{\pm}6.2%$. In the established method in this study, the correlation of coefficient values ($R^2$) of erythromycin calibration curve (n=11) was 0.9998.