• Mass Spectrometry Letters
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• 제4권4호
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• pp.79-82
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• 2013

Various types of alkaloids observed in several herbal medicines were analyzed by electrospray ionization tandem mass spectrometry in positive ion mode. In the present study, MS/MS spectralpatterns were investigated for eight-types of alkaloids (aporpine, protoberberine, tetrahydroprotoberberine, benzylisoquinoline, protopine, phthalide, morpine, and bisbenzylisoquinoline). For aporpine- and protoberberine-type alkaloids, main fragmentations occurred at substituted groups on rigid ring structures, not showing ring fusion. Interesting fragmentations due to iminolization and retro-Diels-Alder (RDA) reaction were observed in MS/MS spectra of protopine- and tetrahydroprotobereberine-type alkaloids. Also, several types of fragmentations such as inductive cleavage and ${\alpha}$-cleavage, or bond cleavage between two ring structures were observed depending on their structural characteristics. These fragmentation patterns are expected to allow instant classification of the specific alkaloid type in various MS/MS spectra of alkaloids.

• Bulletin of the Korean Chemical Society
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• 제33권10호
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• pp.3298-3302
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• 2012

Although offline enrichment of phosphorylated peptides is widely used, enrichment for phosphopeptides using $TiO_2$ is often performed manually, which is labor-intensive and can lead to irreproducible results. To address the problems associated with offline enrichment and to improve the effectiveness of phosphopeptide detection, we developed an automated online enrichment system for phosphopeptide analysis. A standard protein mixture comprising BSA, fetuin, crystalline, ${\alpha}$-casein and ${\beta}$-casein, and ovalbumin was assessed using our new system. Our multidimensional system has four main parts: a sample pump, a 20-mm $TiO_2$-based column, a weak anion-exchange, and a strong cation-exchange (2:1 WAX:SCX) separation column with LC/MS. Phosphorylated peptides were successfully detected using the $TiO_2$-based online system with little interference from nonphosphorylated peptides. Our results confirmed that our online enrichment system is a simple and efficient method for detecting phosphorylated peptides.

• Food Science and Biotechnology
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• 제18권1호
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• pp.113-117
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• 2009

A method was developed using enhanced liquid chromatography coupled with electrospray ionization mass spectrometry for the analysis and quantitation of 2 main potato glycoalkaloids, $\alpha$-chaconine, and $\alpha$-solanine, without any pre-concentration or derivatisation steps. Calibration curves generated by this technique exhibited a linear dynamic range from 0.025 to $50{\mu}g/mL$ and from 0.05 to $50{\mu}g/mL$ for $\alpha$-chaconine and $\alpha$-solanine, respectively. Matrix effects were evaluated by comparing calibration curves measured in matrix-matched and solvent-based systems. Ion suppression due to matrix effects was weak and extraction recoveries of 88 to 114% were obtained in different sample matrices spiked with analyte concentrations ranging from 15 to $35{\mu}g/mL$. Potatoes that had been genetically modified to tolerate glufosinate contained the same glycoalkaloid levels as their non-transgenic counterpart. We suggest complementing compositional comparison assessment strategy by validating quantitative analytical methods for the toxic glycoalkaloids in potato plants.

• 분석과학
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• 제18권1호
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• pp.5-12
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• 2005

고정밀 전자소자의 오동작의 한 원인인 soft error는 원료물질에 함유된 U, Th과 같은 알파방출 불순물로 알려져 있으며 전자소자의 소형화, 고집적화에 따라서 이들 불순물의 규제함량은 기존의 분석법으로는 불가능할 정도로 낮아지고 있다. 연구의 목적은 다양한 전자소자의 밀봉소재로 사용되는 EMC (epoxy molding compound)의 주 원료인 고순도 실리카에 함유되어 있는 U, Th을 고감도 (ng/g이하)로 분석할 수 있는 방사화분석법과 감마선분광분석법의 개발이다. 지금까지 방사화분석법에 이용하던 PTS (pneumatic transfer system) 중성자 조사 설비로는 산업계에서 요구하는 분석 감도를 충족시킬 수 없기 때문에 의약용 혹은 산업용 RI 생산에 주로 사용되고 있는 HTS (Hydraulic transfer system) 중성자 조사 설비를 이용한 방사화분석 조건을 확립하였다. 또한, 공기중 라돈 ($^{222}Rn$)과 자핵종 (progenies)에 의한 불안정한 바탕방사능은 분석의 감도는 물론 정확도를 저하시키는 주 요인으로 작용하므로 질소가스 유입시스템을 제작하여 라돈에 의한 바탕방사능을 소멸 혹은 안정화시켰다. 그 결과 U과 Th의 분석한계를 각각 0.1 ng/g, 0.01 ng/g까지 낮출 수 있었다.

• Nuclear Engineering and Technology
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• 제45권3호
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• pp.415-420
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• 2013

A determination method for $^{237}Np$ in spent nuclear fuel samples was developed using an isotope dilution method with $^{239}Np$ as a spike. In this method, inductively coupled plasma mass spectrometry (ICP-MS) was taken for the $^{237}Np$ instead of the previously used alpha spectrometry. $^{237}Np$ and $^{239}Np$ were measured by ICP-MS and gamma spectrometry, respectively. The recovery yield of $^{237}Np$ in synthetic samples was $95.9{\pm}9.7$% (1S, n=4). The $^{237}Np$ contents in the spent fuel samples were 0.15, 0.25, and $1.06{\mu}g/mgU$ and these values were compared with those from ORIGEN-2 code. A fairly good agreement between the measurements (m) and calculations (c) was obtained, giving ratios (m/c) of 0.93, 1.12 and 1.25 for the three PWR spent fuel samples with burnups of 16.7, 19.0, and 55.9 GWd/MtU, respectively.

• Mass Spectrometry Letters
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• 제13권4호
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• pp.95-105
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• 2022

Amatoxin-induced mushroom poisoning starts with nonspecific symptoms of toxicity but hepatic damage may follow, resulting in the rapid development of liver insufficiency and, ultimately, coma and death. Accurate detection of amatoxins, such as α-, β-, and γ-amanitin, within the first few hours after presentation is necessary to improve the therapeutic outcomes of patients. Therefore, analytical methods for the identification and quantification of α-, β-, and γ-amanitin in biological samples are necessary for clinical and forensic toxicology. This study presents a literature review of the analytical techniques available for amatoxin detection in biological matrices, and established an inventory of liquid chromatography (LC) techniques with mass spectrometry (MS), ultraviolet (UV) detection, and electrochemical detection (ECD). LC-MS methods using quadrupole tandem mass spectrometry, time-of-flight mass spectrometry, and orbitrap MS are powerful analytical techniques for the identification and determination of amatoxins in plasma, urine, serum, and tissue samples, with high sensitivity, specificity, and reproducibility compared to LC with UV and ECD, enzyme-linked immunoassay, and capillary electrophoresis methods.

• 한국발생생물학회지:발생과생식
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• 제12권1호
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• pp.107-112
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• 2008

점망둑의 난모세포 성숙과정에서 생성되는 주요 성 스테로이드 호르몬, $C_{21}$-스테로이드를 분석하고자 전구물질 $^3H-17{\alpha}hydroxyprogesterone$ ($^3H-17{\alpha}OHP$)를 성숙기 난모세포(난경 $0.74{\sim}0.97\;mm$) 배양초기에 첨가하여 24시간 배양하였다. 스테로이드 대사물질 분석과 동정은 thin layer chromatography와 gaschromatography-mass spectrometry로 이루어졌다. $^3H-17{\alpha}20{\alpha}P$로부터 생성된 주요 성 스테로이드 대사물질은 $17{\alpha}$-hydroxy, $20{\alpha}$-dihydroprogesterone ($17{\alpha}20{\alpha}P$)와 $17{\alpha}$-hydroxy, $20{\beta}$-dihydroprogesterone ($17{\alpha}20{\beta}P$)로 확인되었다. 이들 대사물질은 난경 0.80 mm 이상에서 관찰되었으며, GVBD (germinal vesicle breakdown) 유도 효능 테스트에서 점망둑의 난모세포는 $17{\alpha}20{\beta}P$에 더 민감하게 반응하였다. 이러한 결과는 점망둑의 난소성숙 과정에 $17{\alpha}20{\alpha}P$와 $17{\alpha}20{\beta}P$이 모두 관여하나, MIS (maturation inducing steroid)로서의 가능성은 $17{\alpha}20{\beta}P$이 더 큰 것으로 관찰되었다.

• 한국연초학회지
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• 제4권1호
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• pp.67-71
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• 1982

4, 8, 13-Duvatriene-1, 3-viols have been identified in the cuticular lipid of fresh Sohyang (aromatic cultivar) tobacco leaves. Their $\alpha, \beta$-isomers were directly separated by SE-54 glass capillary column and identified by mass spectrometry. Gas chromatographic analysis revealed that the duvatrienediols are major components in the culticular lipid of Nicotiana Tabacum.

• 한국산학기술학회논문지
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• 제6권2호
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• pp.134-143
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• 2005

포유동물에서 중요한 구조단백질인 콜라겐은 다양한 조직내 단백질 조성과 사슬간 복잡한 가교결합의 존재로 인해 그 구조가 복잡하고 다양하여, 직접적으로 분석할 적당한 방법이 없었다. 본 연구에서는 간단한 전처리만으로 다수의 생체분자 시료에 대해 정확한 분자량 측정이 가능한 매트릭스 보조 레이저 탈착/이온화 비행시간 질량분석법(MALDI-TOF MS)을 이용하여 콜라겐과 조각화된 콜라겐을 분석하고 이의 아미노산 서열을 사중극자-비행시간 직렬 질량분석법(Q-TOF MS/MS)으로 확인하여, 시료 중의 콜라겐의 종류에 대한 정보를 확인하여, MALDI-TOF 질량분석을 이용한 콜라겐 분석에서 콜라겐의 종류를 쉽게 예측할 수 있는 방법을 제시하고자 하였다. 쥐의 꼬리에서 분리한 콜라겐을 SDS-PAGE로 분리한 결과 10개의 band를 얻을 수 있었는데, 같은 시료를 MALDI-TOF MS로 확인하여 각 band의 정확한 분자량을 결정할 수 있었다. SDS-PACE상의 10개의 분리된 band에 대해 각각 tryptic digestion후 MALDI-TOF 질량분석을 수행한 결과 4개의 band에서 type I 콜라겐의 $\alpha_1$-chain내의 fragment인 Gly1056-Arg1073을 확인할 수 있었고, 5개의 band에서 type I 콜라겐의 $\alpha_2$-chain내의 fragment인 Gly985-Arg1002을 확인하였다. 잔재한 콜라겐의 가교결합으로 인해 예상되는 fragment중 둘만이 확인되었지만, 확인된 fragment를 통해 적어도 7개의 band에서는 type I콜라겐이 존재함을 확인할 수 있었다. 확인된 두 콜라겐 flagment의 아미노산 서열을 Q-TOF MS/MS로 분석한 결과 MALDI-TOF MS에서의 예측과 일치함을 확인할 수 있었으며, 이를 통해 확인된 두 fragment에 의한 peak을 지문으로 하여 MALDI-TOF MS측정시에 시료내의 type I 콜라겐의 존재를 쉽게 확인할 수 있음을 볼 수 있었다.

• Nuclear Engineering and Technology
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• 제38권5호
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• pp.423-426
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• 2006

A developed neutron activation analysis(NAA) and gamma-spectrometry were applied to improve the analytical sensitivity and precision of impurities in electronic-circuit raw materials. It is well known that soft errors in high precision electronic circuits can be induced by alpha particles emitted from naturally occurring radioactive impurities such as U and Th. As electronic circuits have recently become smaller in dimension and higher in density, these alpha-particle emitting radioactive impurities must be strictly controlled. Therefore, new NAA methods have been established using a HTS(Hydraulic Transfer System) irradiation facility and a background reduction method. For eliminating or stabilizing fluctuated background caused by Rn-222 and its progeny nuclides in air, a nitrogen purging system is used. Using the developed NAA and gamma-spectrometry, ultra trace amounts of U(0.1ng/g) and Th(0.01ng/g) in an alumina ball and high purity silica used for an epoxy molding compound (EMC) could be determined.