• 한국작물학회:학술대회논문집
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• 한국작물학회 2020년도 춘계학술대회
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• pp.183-183
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• 2020

• 분석과학
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• 제20권2호
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• pp.115-123
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• 2007

헤테로싸이클릭 아민류(heterocyclic amines, HAs)는 소고기, 돼지고기, 닭고기 그리고 생선과 같은 근육질의 육류를 조리 할 때 생겨나는 돌연변이원성/발암성 화학물질로 잘 알려져 있다. 식품으로부터 HAs의 분석에 있어 가장 큰 어려움은 HAs가 식품 중에 극히 미량(수 ng/g)으로 존재한다는 것과 많은 방해물질이 존재한다는 것이다. 식품으로부터 HAs를 추출하고 정제하기 위해 고체-상 추출(solid-phase extraction, SPE)이 많이 사용되고 있다. HAs 분석을 위해 여러 단계의 SPE 과정을 수행하였다. HAs의 회수율은 표준물질이 녹여져 있는 메탄올 수용액과 조리되지 않은 돼지고기에 표준용액을 스파이크하여 서로를 비교하여 얻었다. 회수율은 25.0 ng/g에서 25.3~93.0%의 값을 얻을 수 있었다. 확립된 감도 좋고 재현성있는 시료전처리방법을 통해서 ${\mu}$-LC/ESI-MS에 주입함으로써 조리된 육류로부터 HAs를 분석하는데 응용될 수 있을 것이다. 다른 방법으로는 freezing filtration 방법으로써 보다 좋은 추출 효율과 재현성을 나타내었다.

• 한국자기공명학회논문지
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• 제22권2호
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• pp.26-33
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• 2018

Xanthium sibiricum is used as a traditional folk medicine for the treatment of cancer, fever, headache, nasal sinusitis, and skin pruritus. This study aimed to identify components from Xanthium sibiricum extracts using an SPE-800MHz NMR-MS hyphenated system. The simultaneous acquisition of MS and NMR spectra from the same chromatographic peaks significantly increases the depth of information acquired for the compound and allows the elucidation of structures that would not be possible using MS or NMR data alone. LC -NMR analysis was conducted using a HPLC separation system coupled to 800 MHz spectrometer equipped with a cryoprobe, and a SPE unit was used to automatically trap chromatographic peaks using a HPLC pump. LC-MS analysis was conducted with a Q-TOF MS instrument using ESI ionization in the negative ion mode. Using the hyphenated analysis, several secondary metabolites were identified, such as 3',5'-O-dicaffeoylquinic acid, 1',5'-O-dicaffeoyl- quinic acid, and ethyl caffeate. These results demonstrate that the SPE-800MHz NMR-MS hyphenated system can be used to identify metabolites within natural products that have complex mixtures.

• 약학회지
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• 제55권3호
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• pp.203-212
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• 2011

Adipocytes have been known to secrete a number of important proteins called adipokines with roles in energy metabolism, reproduction, cardiovascular function and immunity. In this study we have attempted to identify intensively secretory proteins from 3T3-L1 adipocytes. 3T3-L1 preadipocytes were differentiated into mature adipocytes and then the cells were left in serum-free medium. The supernatant was filtrated and dialyzed. Lyophilized secretome was fractionated by two different methods, 1-D SDS PAGE and RP-FPLC. The tryptic peptides from the gel slices and the FPLC fractions were analyzed by nanoLC/ESI-MS/MS. We identified a total of 303 identical proteins from two methods, 251 proteins from 1-D gel and 184 proteins from RP-FPLC. 86 of them were listed as a secretory protein Finally, we identified many known or unknown secreted proteins existed in the low level including adiponectin, angiotensinogen, bone morphogenetic protein-1 (BMP-1), macrophage migration inhibitory factor (MIF), insulin like growth factor-II (IGF-II), interleukin-6 (IL-6), follistatin-related protein-1, minecan, and resistin. The existence of some of secreted proteins has been confirmed in RNA level. This proteomic experiment is useful for the intensive screening of secretory proteins in many kinds of other cells.

• Molecules and Cells
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• 제27권5호
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• pp.601-608
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• 2009

The 2-deoxystreptamine and paromamine are two key intermediates in kanamycin biosynthesis. In the present study, pSK-2 and pSK-7 recombinant plasmids were constructed with two combinations of genes: kanABK, and kanABKF and kacA respectively from kanamycin producer Streptomyces kanamyceticus ATCC12853. These plasmids were heterologously expressed into Streptomyces lividans TK24 independently and generated two recombinant strains named S. lividans SK-2/SL and S. lividans SK-7/SL, respectively. ESI/ MS and ESI-LC/MS analysis of the metabolite from S. lividans SK-2/SL showed that the compound had a molecular mass of 163 $[M+H]^+$, which corresponds to that of 2-deoxystreptamine. ESI/MS and MS/MS analysis of metabolites from S. lividans SK-7/SL demonstrated the production of paromamine with a molecular mass of $324[M+H]^+$. In this study, we report the production of paromamine in a heterologous host for the first time. This study will evoke to explore complete biosynthetic pathways of kanamycin and related aminoglycoside antibiotics.

• 분석과학
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• 제23권2호
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• pp.119-127
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• 2010

환경 시료중에 잔류하는 베타-락탐계 항생제를 동시에 추출하는 방법을 확립하였다. pH 2 에서 HLB 고체상을 사용하여 추출 및 정제한 후, 7종의 베타-락탐계 항생제(amoxicillin, ampicillin, penicillin G, cefaclor, cefadroxil, cefatrizine 및 cephradine)를 LC/ESI-MS/MS를 사용하여 동시에 분석하였다. 새롭게 확립된 분석법은 하천수중에서 베타-락탐계 항생제의 농도가 0.01~1.0 ng/mL일 때 정량을 위한 검정곡선의 상관계수($r^2$)가 0.9911~0.9995 범위로써 우수한 직선성을 나타내었다. 바탕하천수로부터 구한 검출한계(LOD)와 정량한계(LOQ)는 각각 0.0003~0.0234 ng/mL 와 0.0046~0.0778 ng/mL이었다. 이 분석방법은 물 환경중에 잔류하는 베타-락탐계 항생제를 정성 정량하는데 빠르고 신뢰할 만한 방법이 될 것이다.

• 분석과학
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• 제20권2호
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• pp.164-169
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• 2007

고속액체크로마토그라피/질량분석기를 이용하여 가공 식품 중 아크릴아마이드를 분석하였다. 대상 식품은 감자칩 (6종), 프렌치후라이 (11종)으로 총 17종이었다. 시료를 균질화하여 3차 증류수로 추출하고 C18 및 혼합이온교환수지 카트리지를 이용하여 정제한 후 LC/MS/MS으로 분석하였다. 이동상으로는 0.1% 초산과 0.5% 메탄올을 함유하는 수용액을 사용하였으며, 대상물질의 특이이온을 ESI 질량분석기로 확인 및 정량하였다. 평균 회수율은 91~101%이었으며, 정량한계는 $10{\mu}g/kg$이었다. 대상식품의 유형에 따라 검출 수준에 차이를 나타냈으며, 평균 검출수준은 감자칩은 0.71 mg/kg, 프렌치후라이는 0.34 mg/kg이었다.

• 생약학회지
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• 제47권4호
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• pp.381-388
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• 2016

Hyangso-san is a traditional herbal medicine that consists of the seven herbal medicines, Cyperi Rhizoma, Perillae Folium, Atractylodis Rhizoma, Citri Unshius Pericarpium, Glycyrrhizae Radix et Rhizoma, Zingiberis Rhizoma Crudus, and Allii Fistulosi Bulbus. Hyangso-san has long been clinically used to treat the influenza, including headache, ferver, chills, and pantalgia. In this study, we were performed the simultaneous analysis of the 15 marker compounds (liquiritin apioside, liquiritin, ferulic acid, naringin, hesperidin, rosmarinic acid, liquiritigenin, kaempferol, glycyrrhizin, nobiletin, 6-gingerol, elemicin, atractylenolide III, nootkatone, and atractylenolide I) in Hyangso-san using liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS/MS). Column for the separation of the 15 ingredients was used a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ by using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient condition. Identifications of all analytes were performed using a Waters ACQUITY TQD LC-MS/MS system. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$, respectively. Correlation coefficient of the calibration curve was ${\geq}0.9958$. The values of limits of detection and quantification of the 15 components were 0.002-4.29 and 0.01-12.88 ng/mL, respectively. The result of an analysis using the established LC-MS/MS method, kaempferol and atractylenolide I were not detected, while other 13 compounds were 0.08-56.87 mg/g in lyophilized Hyangso-san sample.

• Journal of Microbiology and Biotechnology
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• 제19권1호
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• pp.51-54
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• 2009

Myxobacteria, Gram-negative soil bacteria, are a well-known producer of bioactive secondary metabolites. Therefore, this study presents a methodological approach for the high-throughput screening of secondary metabolites from 4 wild-type Myxococcus xanthus strains. First, electrospray ionization mass spectrometry (ESI-MS) was performed using extracellular crude extracts. As a result, 22 metabolite peaks were detected, and the metabolite profiling was then conducted using the m/z value, retention time, and MS/MS fragmentation pattern analyses. Among the peaks, one unknown compound peak was identified as analogous to the myxalamid A, B, and C series. An analysis of the tandem mass spectrometric fragmentation patterns and HR-MS identified myxalamid K as a new compound derived from M. xanthus. In conclusion, LC-MS/MS-based chemical screening of diverse secondary metabolites would appear to be an effective approach for discovering unknown microbial secondary metabolites.

• 대한약학회:학술대회논문집
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• 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2-2
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• pp.217.3-217.3
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• 2003

Acetyl-L-carnitine, a physiological component of the L-carnitine family, has been proposed for treating Alzheimer's disease in pharmacological doses. Acetyl-L-carnitine and d3-acetylcarnitine (internal standard) were analyzed by electrospray ionization / tandem mass spectrometry (ESI/MS/MS) after derivatization to their butylesters through treatment with butanolic hydrogen chloride. Acetyl-L-carnitine produced a protonated precursor ion at m/z 260 and a corresponding product ion of m/z 85. Analytes were separated on a Capcell Pak C18 (2.0${\times}$150mm, 5 mm). (omitted)