• Proceedings of the SCSK Conference
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• 2003.09b
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• pp.480-507
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• 2003

A rapid and efficient method for analyzing the nonionic surfactants and silicone polymers, which control the shape and characteristics of cosmetic products and give influence on product quality, has been developed using Matrix-Assisted Laser Desorption Ionization Time of Flight Mass Spectrometry (MALDI- TOF IMS). The MALDI-TOF/MS could easily and effectively determine the molecular weight distribution and monomer units of nonionic surfactants. As a result, creating a library of mass spectrum data of surfactants used in cosmetic products using MALDI-TOF/MS and analyzing surfactants extracted from the products may become a useful method for detailed structural characterization of the surfactants. Furthermore, the MALDI-TOF/MS analysis was effective in obtaining the spectrum of silicone polymers from which the molecular weight distribution could be determined. The repetition units and structural data could also be obtained through molecular mass peaks. Additionally, the monomer ratio and terminal groups as properties of silicone copolymers could be determined

• BMB Reports
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• v.29 no.2
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• pp.122-126
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• 1996

A series of oligonucleotides were synthesized by automatic DNA synthesizer. The purity of crude products was checked and their molecular weights determined by matrix assisted laser desorption ionization mass spectrometry (MALDI-MS) with an accuracy of better than 0.05% deviation even without using an internal standard. This mass determining technology in combination with partial digestion of oligonucleotides by 5'- and 3'-exonuclease provides a straightforward and simple method to obtain sequence information of oligonucleotides. The extension of this technology to the sequencing of modified oligonucleotides and genomic DNA and RNA might become possible.

• Bulletin of the Korean Chemical Society
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• v.20 no.11
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• pp.1299-1302
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• 1999

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) was used to demonstrate cross-linking of peptides induced by transglutaminase. The presence of ε-( Υ-glutamyl)lysine isopeptide cross-link in the acid hydrolysate of the cross-linking reaction mixture was also demonstrated by MALDI-TOF-MS without prior separation. MALDI-TOF-MS quickly provided peptide mass maps after pronase digestion of the cross-linked peptide adduct, which enabled us to monitor the hydrolytic sequence. Pronase appears to preferentially hydrolyze peptide bonds distant from the cross-link before hydrolyzing peptide bonds around the cross-link. The results suggest that pronase digestion followed by MALDI-TOF-MS could be used for determination of amino acid sequence around a modification site.

• Bulletin of the Korean Chemical Society
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• v.33 no.9
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• pp.3119-3121
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• 2012

• Bulletin of the Korean Chemical Society
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• v.17 no.11
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• pp.1036-1039
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• 1996

Synthetic lipoidal peptides based on viral protein sequences have been prepared. These peptides contain an N-palmitoyl group at the N-terminal residue, which is a modified cysteine, containing a S-[2,3-bis(acyloxy)-(2-R,S)-propyl] moiety. When this residue (Pam3Cys) is at the N-terminus of a synthetic peptide, it acts as potent immunoadjuvant to enhance both IgM and IgG antibody responses to the attached peptide. Conventional analytical procedures (e.g., Edman degradation and amino acid analysis) are either not applicable due to the N-terminal modification, or do not provide confirmation of the intact structure. Chromatographic analysis is also hindered by the tendency of these lipoidal Pam3Cys peptides to form large aggregates, and in some cases to be permanently adsorbed on reversed phase columns. We have applied several mass spectrometric techniques, including fast atom bombardment (FAB), electrospray ionization (ESI) and matrix assisted laser desorption ionization (MALDI) to characterize the intact structures of a number of different Pam3Cys synthetic peptides. The MALDI-MS has been found to be the most sensitive for the analysis of the structure of Pam3Cys peptides.

• Bulletin of the Korean Chemical Society
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• v.23 no.2
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• pp.315-319
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• 2002

Visible surface-assisted desorption/ionization mass spectrometry (SALDI-MS) has been investigated for several small macromolecules deposited on the graphite plate using laser radiation at 532 nm where most of the macromolecules are transparent. The graphite surface functioned well as a photon absorbing material and an energy transfer mediator for visible light. The results show that visible SALDI is a much softer ionization technique than UV-MALDI and FAB-MS in our results with synthetic macromolecules, PPG, PPGMBE and cavitand molecules. For the SALDI of biomolecules, glycerol as a proton source was essential with the graphite plate. As in visible SALDI, the role division of the photon absorbing material and the cationization agent can provide a generality in mass spectrometric analysis of macromolecules compared with MALDI using the dual functional matrix.

• Mass Spectrometry Letters
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• v.2 no.3
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• pp.69-72
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• 2011

Defective synthesis of the steroid hormones by the adrenal cortex has profound effects on human development and homeostasis. Due to the time-consuming chromatography procedure combined with mass spectrometry, the matrix-assisted laser desorption ionization method coupled to the linear ion-trap tandem mass spectrometry (MALDI-LTQ-MS/MS) was developed for quantitative analysis of 10 adrenal steroids in human serum. Although MALDI-MS can be introduced for its applicability as a high-throughput screening method, it has a limitation on reproducibility within and between samples, which renders poor reproducibility for quantification. For quantitative MALDI-MS/MS analysis, the stable-isotope labeled internal standards were used and the conditions of crystallization were tested. The precision and accuracy were 3.1~35.5% and 83.8~138.5%, respectively, when a mixture of 10 mg/mL ${\alpha}$-cyano-4-hydroxycinnamic acid in 0.2% TFA of 70% acetonitrile was used as the MALDI matrix. The limit of quantification ranged from 5 to 340 ng/mL, and the linearity as a correlation coefficient was higher than 0.988 for all analytes in the calibration range. Clinical applications include quantitative analyses of patients with congenital adrenal hyperplasia. The devised MALDI-MS/MS technique could be successfully applied to diagnosis of clinical samples.

• Bulletin of the Korean Chemical Society
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• v.24 no.9
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• pp.1308-1312
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• 2003

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) was used to observe folic acid and its derivatives such as tetrahydrofolate and 5-methyltetrahydrofolate in a vitamin tablet and in foods. Folic acid in a vitamin tablet was determined using angiotensin I as an internal reference. Tetrahydrofolic acid, 5-methyltetrahydrofolic acid, and an oxygenated folate were observed from a human blood sample using graphite plate. The results show that these mass spectrometric methods are useful for quickly obtaining a profile of folates.

• Bulletin of the Korean Chemical Society
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• v.31 no.8
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• pp.2293-2298
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• 2010

Focused electrospray (FES) deposition method is presented for matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. FES ion optics consists of two cylindrical focusing electrodes capped with a truncated conical electrode through which an electrospray emitter passes along the cylindrical axis. A spray of charged droplets is focused onto a sample well on a MALDI target plate under atmospheric pressure. The shape and size distributions of matrix crystals are visualized by scanning electron microscope and the mass spectra are obtained by time-of-flight mass spectrometry. Angiotensin II, bradykinin, and substance P are used as test samples, while $\alpha$-cyano-4-hydroxycinnamic acid and dihydroxybenzoic acid are employed as matrices. FES of a sample/matrix mixture produces fine crystal grains on a 1-3 mm spot and reproducibly yields the mass spectra with little shot-to-shot and spot-to-spot variations. Although FES greatly stabilizes the signals, the space charge due to matrix ions limits the detection sensitivity of peptides. To avoid the space charge problem, we adopted a dual FES/FES mode, which separately deposits matrix and sample by FES in sequence. The dual FES/FES mode reaches the detection sensitivity of 0.88 amol, enabling ultrasensitive of peptides by homogeneously depositing matrix and sample under atmospheric pressure.

• Journal of Ginseng Research
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• v.45 no.5
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• pp.539-545
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• 2021

Background: Red ginseng polysaccharides (RGPs) have been acknowledged for their outstanding immunomodulation and anti-tumor activities. However, their studies are still limited by the complexity of their structural features, the absence of purification and enrichment methods, and the rarity of the analytical instruments that apply to the analysis of such macromolecules. Thus, this study is an attempt to establish a new mass spectrometry (MS)-based analysis procedure for RGPs. Methods: Saponin pre-excluded powder of RG (RG-SPEP, 10 mg) was treated with 200 µL of distilled water and centrifuged for 5 h at 1000 rpm and 85 ℃. Ethanol-based precipitation and centrifugation were applied to obtain RGPs from the heated extracts. Further, endo-carbohydrase treatments were performed to produce specific saccharide fragments. Solid-phase extraction (SPE) processes were implemented to purify and enrich the enzyme-treated RGPs, while matrix-assisted laser desorption/ionization time-of-flight/time-of-flight (MALDI-TOF/TOF) MS was employed for the partial structural analysis of the obtained RGPs. Results: Utilizing cellulase, porous graphitized carbon (PGC), hydrophilic interaction chromatography (HILIC), and MALDI-TOF/TOF MS, the neutral and acidic RGPs were qualitatively analyzed. Hex_n and Hex_n-18 (cellulose analogs) were determined to be novel neutral RGPs. Additionally, the [Unknown + Hex_n] species were also determined as new acidic RGPs. Furthermore, HexA_n (H) was determined as another form of the acidic RGPs. Conclusion: Compared to the previous methods of analysis, these unprecedented applications of HILIC-SPE and MALDI-TOF/TOF MS to analyze RGPs proved to be fairly effective for fractionating and detecting neutral and acidic components. This new procedure exhibits great potential as a specific tool for searching and determining various polysaccharides in many herbal medicines.