Study on production process of graphite for biological applications of ¹⁴C-accelerator mass spectrometry

Ha, Yeong Su,Kim, Kye-Ryung,Cho, Yong-Sub,Choe, Kyumin,Kang, Chaewon 대한방사성의약품학회 2020 Journal of radiopharmaceuticals and molecular prob Vol.6 No.1

Accelerator mass spectrometry (AMS) is a powerful detection technique with the exquisite sensitivity and high precision compared with other traditional analytical techniques. Accelerator mass spectrometry can be widely applied in the technique of radiocarbon dating in the fields of archeology, geology and oceanography. The ability of accelerator mass spectrometry to measure rare ¹⁴C concentrations in microgram and even sub-microgram amounts suggests that extension of ¹⁴C-accelerator mass spectrometry to biomedical field is a natural and attractive application of the technology. Drug development processes are costly, risky, and time consuming. However, the use of ¹⁴C-accelerator mass spectrometry allows absorption, distribution, metabolism and excretion (ADME) studies easier to understand pharmacokinetics of drug candidates. Over the last few decades, accelerator mass spectrometry and its applications to preclinical/clinical trials have significantly increased. For accelerator mass spectrometry analysis of biological samples, graphitization processes of samples are important. In this paper, we present a detailed sample preparation procedure to apply to graphitization of biological samples for accelerator mass spectrometry.

Study on production process of graphite for biological applications of 14C-accelerator mass spectrometry

하영수,김계령,Yong-Sub Cho,최규민,Chaewon Kang 대한방사성의약품학회 2020 Journal of radiopharmaceuticals and molecular prob Vol.6 No.1

Accelerator mass spectrometry (AMS) is a powerful detection technique with the exquisite sensitivity and high precision compared with other traditional analytical techniques. Accelerator mass spectrometry can be widely applied in the technique of radiocarbon dating in the fields of archeology, geology and oceanography. The ability of accelerator mass spectrometry to measure rare 14C concentrations in microgram and even sub-microgram amounts suggests that extension of 14C-accelerator mass spectrometry to biomedical field is a natural and attractive application of the technology. Drug development processes are costly, risky, and time consuming. However, the use of 14C-accelerator mass spectrometry allows absorption, distribution, metabolism and excretion (ADME) studies easier to understand pharmacokinetics of drug candidates. Over the last few decades, accelerator mass spectrometry and its applications to preclinical/clinical trials have significantly increased. For accelerator mass spectrometry analysis of biological samples, graphitization processes of samples are important. In this paper, we present a detailed sample preparation procedure to apply to graphitization of biological samples for accelerator mass spectrometry.

Advances in Ion Mobility Spectrometry-Mass Spectrometry (IMS-MS)-Based Techniques for Elucidating Higher-Order Protein Structures

( Jongcheol Seo ) 한국질량분석학회 2020 Mass spectrometry letters Vol.11 No.4

Despite its great success in the field of proteomics, mass spectrometry has limited use for determining structural details of peptides, proteins, and their assemblies. Emerging ion mobility spectrometry-mass spectrometry has enabled us to explore the conformational space of protein ions in the gas phase, and further combinations with the gas-phase ion spectroscopy and the collision-induced unfolding have extended its abilities to elucidating the secondary structure and local details of conformational transitions. This review will provide a brief introduction to the combined approaches of IMS-MS with gas-phase ion infrared spectroscopy or collision-induced unfolding and their most recent results that successfully revealed higher-order structural details.

A mass spectrometry-based multiplex SNP genotyping by utilizing allele-specific ligation and strand displacement amplification

Park, Jung Hun,Jang, Hyowon,Jung, Yun Kyung,Jung, Ye Lim,Shin, Inkyung,Cho, Dae-Yeon,Park, Hyun Gyu Elsevier 2017 Biosensors & Bioelectronics Vol.91 No.-

<P><B>Abstract</B></P> <P>We herein describe a new mass spectrometry-based method for multiplex SNP genotyping by utilizing allele-specific ligation and strand displacement amplification (SDA) reaction. In this method, allele-specific ligation is first performed to discriminate base sequence variations at the SNP site within the PCR-amplified target DNA. The primary ligation probe is extended by a universal primer annealing site while the secondary ligation probe has base sequences as an overhang with a nicking enzyme recognition site and complementary mass marker sequence. The ligation probe pairs are ligated by DNA ligase only at specific allele in the target DNA and the resulting ligated product serves as a template to promote the SDA reaction using a universal primer. This process isothermally amplifies short DNA fragments, called mass markers, to be analyzed by mass spectrometry. By varying the sizes of the mass markers, we successfully demonstrated the multiplex SNP genotyping capability of this method by reliably identifying several BRCA mutations in a multiplex manner with mass spectrometry.</P> <P><B>Highlights</B></P> <P> <UL> <LI> A new mass spectrometry-based method for multiplex SNP genotyping was developed in label-free manner. </LI> <LI> Multiple SNP sites were simultaneously genotyped based on the peak positions by designing mass markers with different sizes. </LI> <LI> The interpretation of the mass spectrum is simple to analyze the multiple polymorphic sites. </LI> <LI> Several BRCA mutations was genotyped in a multiplex manner for the real clinical patient samples. </LI> </UL> </P>

나노물질을 이용한 질량분석 기술 개발동향

박종민(Jong-Min Park),노주윤(Joo-Yoon Noh),김문주(Moon-Ju Kim),변재철(Jae-Chul Pyun) 한국세라믹학회 2018 세라미스트 Vol.21 No.3

In conventional MALDI-TOF mass spectrometry, analyte molecules are known to be ionized by mixing with organic matrix molecules. As the organic matrix molecules are made into small fragments, they generate unreproducible mass peaks such that MALDI-TOF mass spectrometry is nearly impossible in the low mass-to-charge (m/z) range (< 1000). Additionally, the dried sample mixed with matrix were made as inhomogeneous crystal on metal plate. When the laser radiation was made on the sample crystal, the amount of generated sample ion was observed to be quite different according to the radiation point. Therefore, the quantitative analysis was very difficult even for the sample spots at the same concentration for the conventional MALDI-TOF mass spectrometry. In this work, we present laser desorption/ionization (LDI) mass spectrometry based on solid-matrices for the quantitative analysis of small molecules in the low m/z range by using MALDI-TOF mass spectrometry: (1) Carbon based nanostructures; (2) Semiconductor based nanomaterials; (3) Metal based nanostructures.

Comparison Study of Sensitivity Factors of Elements in Glow Discharge- & Inductively Coupled Plasma- Mass Spectrometry

김영상,M. Plotnikov,Volker Hoffmann 대한화학회 2005 Bulletin of the Korean Chemical Society Vol.26 No.12

Sensitivity factors of elements by a glow discharge mass spectrometry (GD-MS) were intensively investigated and compared with a laser ablation inductively coupled plasma-mass spectrometry (ICP-MS). In case of copper matrix, the sensitivity factor by GD-MS generally decreases with the increase of the mass number of element. The details are a little different between each data measured by Faraday and multiplier detectors. The factor by a multiplier detector drastically decreases with the mass increase in the region of low mass as in Faraday detector’s case, but slowly in the high mass region. On the contrast, the sensitivity factor of solution standard by a conventional ICP-MS slowly increases with the increase of elemental mass number even though there are some exceptions such as gold and also the sensitivity factor by a laser ablation ICP-MS generally increases with mass number of element in the specimen of glass type. In case of steel matrix, any definite trends could not be shown in the relationship between the GD-MS’s sensitivity factor and elemental mass.

In situ mass spectrometry of glucose decomposition under hydrothermal reactions

Pattasuda Duangkaew,Shuhei Inoue,Tsunehiro Aki,Yutaka Nakashimada,Yoshiko Okamura,Takahisa Tajima,Yukihiko Matsumura 한국화학공학회 2017 Korean Journal of Chemical Engineering Vol.34 No.5

We designed an in situ mass spectrometry (in situ MS) analysis method and developed to identify the products of glucose decomposition under hydrothermal condition for the first time. The in situ MS analysis was performed by coupling a tubular batch reactor with a quadrupole mass analyzer via custom-built connection fittings. The products of glucose decomposition were investigated by in situ MS, mass spectrometry of cold effluent, and high-performance liquid chromatography (HPLC) analysis of cold effluent and the results were compared. At 140 oC, in situ MS and mass spectrometry of cold effluent showed that the decomposition of glucose does not proceed; this was confirmed by comparison with the mass spectral database for glucose. At 180 oC or higher, a clear base fragmentation peak of 5-hydroxymethylfurfural (5-HMF) at position m/z 97 and that of furfural at m/z 96, formic acid (m/z=46) and levulinic acid (m/z=116) were observed by mass spectrometry. No levulinic acid or furfural was observed through conventional HPLC analysis under any condition; only glucose, formic acid, and 5-HMF could be detected. The effectiveness of in situ MS analysis is clear, compared to mass spectrometry analysis of cold effluent and HPLC analysis.

Mass spectrometry based cellular phosphoinositides profiling and phospholipid analysis: A brief review

김영준,Li-Hua Zhou,Selina Rahman Shanta,김광표 생화학분자생물학회 2010 Experimental and molecular medicine Vol.42 No.1

Phospholipids are key components of cellular membrane and signaling. Among cellular phospholipids,phosphoinositides, phosphorylated derivatives of phosphatidylinositol are important as a participant in essential metabolic processes in animals. However,due to its low abundance in cells and tissues, it is difficult to identify the composition of phosphoinositides. Recent advances in mass spectrometric techniques,combined with established separation methods, have allowed the rapid and sensitive detection and quantification of a variety of lipid species including phosphoinositides. In this mini review, we briefly introduce progress in profiling of cellular phosphoinositides using mass spectrometry. We also summarize current progress of matrices development for the analysis of cellular phospholipids using matrix-assisted laser desorption/ionization mass spectrometry. The phosphoinositides profiling and phospholipids imaging will help us to understand how they function in a biological system and will provide a powerful tool for elucidating the mechanism of diseases such as diabetes, cancer and neurodegenerative diseases. The investigation of cellular phospholipids including phosphoinositides using electrospray ionization mass spectrometry and matrix-assisted laser desorption/ionization mass spectrometry will suggest new insights on human diseases,and on clinical application through drug development of lipid related diseases.

Mass spectrometry와 NMR Spectroscopy를 이용한 1, 2-Octanediol Galactoside의 효소합성 확인

이향렬(Hyang-Yeol Lee),진홍종(Hong-Jong Jin),안승혜(Seung Hye An),이혜원(Hye Won Lee),정경환(Kyung-Hwan Jung) 한국응용과학기술학회 (구.한국유화학회) 2021 한국응용과학기술학회지 Vol.38 No.3

안전한 화장품용 방부제에 대한 연구를 위하여 1, 2-octanediol (OD)에 galactose 한 분자가 결합된 1, 2-octanediol galactoside (OD-gal)의 합성을 시도하였다. 이를 위하여, 재조합 대장균의 β-galactosidase (β-gal)를 이용하여 transgalactosylation 반응을 수행하였으며, OD-gal 합성을 확인 하기 위하여 mass spectrometry 분석과 NMR ( 1 H- and 13 C-) spectroscopy 분석을 실시하였다. 합성 반응물에서 m/z=331.1732의 sodium adduct ion 형태로 OD-gal 분자의 합성을 확인하였고, 정제된 OD-gal의 NMR 분석을 통하여 OD-gal의 1 H NMR 스펙트럼에서 OD에 갈락토실화가 되었음을 보여주는 다양한 피크를 확인하였다. 1 H NMR 스펙트럼의 다운필드인 δ H 4.39 ppm과 δ H 3.98~3.55 ppm에서 나타나는 다양한 피크들은 이들이 OD에 갈락토실화가 되었다는 것을 잘 암시하고 있으며, 또한 1 H NMR 스펙트럼의 업필드에서 나타나는 δ H 1.52~1.26 ppm과 0.89 ppm의 피크는 OD의 CH 2 와 CH 3 작용기로 부터 나타나는 피크로써 OD가 본 물질에 존재함을 알 수 있었다. 13 C NMR 스펙트 럼에서는 OD-gal의 알파-아노머와 베타-아노머의 구조에서 기인하는 총 24개의 탄소피크가 나타났고, 각 아노머 마다 14개의 탄소가 존재하는데 이중 δc 31.4, 29.0, 22.3 그리고 13.7 ppm에 보이는 OD 4개의 탄소는 지방족 사슬의 끝부분에 해당하며 화학적 구조의 유사성으로 인하여 탄소 피크가 겹쳐서 나타난 것으로 보인다. 따라서 총 28개의 탄소 피크 중 24개가 나타났다. 마지막으로, 합성된 OD-gal 의 β-gal을 이용한 가수분해 반응을 통하여 OD-gal에 gal이 결합되어 있다는 것을 확인하였다. 이러 한 결과를 바탕으로 세포독성이 감소된 첨가물 개발을 기대하고 있으며, 추가적인 후속연구를 진행할 예정이다. 1, 2-Octanediol galactoside (OD-gal) has been synthesized from 1, 2-octanediol (OD), as a safer cosmetic preservative, using recombinant Escherichia coli β-galactosidase (β-gal). To confirm the molecular structure of synthesized OD-gal, mass spectrometry and NMR ( 1 H- and 13 C-) spectroscopy of OD-gal were carried out. In the reaction mixture, a sodium adduct ion of OD-gal (m/z=331.1732) was identified using mass spectrometry analysis. In addition, 1 H NMR spectrum of OD-gal showed multiple peaks corresponding to the galactosyl group, which is evidence of galactosylation on OD. Downfield proton peaks at δ H 4.39 ppm and multiple peaks from δ H 3.98~3.55 ppm were indicative of galactosylation on OD. Up field proton peaks at δ H 1.52~1.26 ppm and 0.89 ppm showed the presence of CH 2 and CH 3 protons of OD. 13 C NMR spectrum revealed the presence of 24 carbons suggestive of α- and β-anomers of OD-gal. Among 14 carbon peaks from each anomer, the 4 peaks at δ C 31.4, 29.0, 22.3, and 13.7 ppm were assigned to be overlapped showing only 24 peaks out of a total of 28 peaks. The mass value from mass spectrometry analysis of OD-gal, and 1 H and 13 C NMR spectral data were in good agreement with the expecting structure of OD-gal. Finally, we identified a galactose molecule from the hydrolysate of OD-gal using β-gal. We are expecting that through future study it will eventually be able to develop a safe cosmetic preservative.

Unusual Applications of Kendrick Plots: Recalibration and Tolerance

Thierry N. J. Fouquet,Orlando Cabarcos 사단법인 한국질량분석학회 2023 Mass spectrometry letters Vol.14 No.4

Kendrick plots offer an alternative visualization of mass spectral data which reveals ion series and patterning by turn- ing a mass spectrum into a map, plotting the fractional mass (wrongly called mass defect) as a function of mass-to-charge ratios and ion abundances. Although routinely used for polymer mass spectrometry, two unreported applications of these Kendrick plots are proposed using the program “kendo2”: the graphical recalibration of a mass spectrum via the simulation of a theoretical fractional mass and a multi-segment fit; and the rapid evaluation of scan-to-scan variation of accurate mass measurements used as tolerances for the blank subtraction of UPLC-MS data files. Both applications are compatible with any type of high-resolution MS data including LC/GC-MS(/MS).