• Title/Summary/Keyword: $MS^n$

Search Result 1,628, Processing Time 0.033 seconds

Synthesis and Structural Characterization of β-Carboline Compounds (β-카볼린 화합물의 합성 및 구조분석)

  • Byeon, Hong-Ju;Han, Min-Hui;Moon, Gi-Seong;Jung, Kyung-Hwan;Lee, Hyang-Yeol
    • Journal of the Korean Applied Science and Technology
    • /
    • v.36 no.2
    • /
    • pp.676-684
    • /
    • 2019
  • The Pictet-Spengler reactions have widely known for the organic synthesis or biosynthesis of biologically active compounds, tetrahydro-${\beta}$-carbolines. We have developed the simple and efficient synthetic method for the synthesis of ${\beta}$-carbolines in water. Their chemical structures were characterized by nmr and UPLC/MS/QTOF. Calculated masses of compound 1 ($C_{17}H_{17}N_2$ 249.1392), 2 ($C_{17}H_{23}N_2$ 255.1861), 3 ($C_{19}H_{21}N_2O_3$ 325.1552) and 4 ($C_{19}H_{19}N_2O$ 279.1497) were almost identical with the detected masses of compound 1 (249.1315), 2 (255.1789), 3 (325.1460) and 4 (279.1364) respectively. Those synthesized four compounds showed strong antibiotic activity against the common E. coli.

Determination of methamphetamine, 4-hydroxymethamphetamine, amphetamine and 4-hydroxyamphetamine in urine using dilute-and-shoot liquid chromatography-tandem mass spectrometry (시료 희석 주입 LC-MS/MS를 이용한 소변 중 메스암페타민, 4-하이드록시메스암페타민, 암페타민 및 4-하이드록시암페타민 동시 분석)

  • Heo, Bo-Reum;Kwon, NamHee;Kim, Jin Young
    • Analytical Science and Technology
    • /
    • v.31 no.4
    • /
    • pp.161-170
    • /
    • 2018
  • The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

Development of a Simultaneous Analytical Method for Determination of Trinexapac-ethyl and Trinexapac in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 식물생장조절제 Trinexapac-ethyl과 대사산물 Trinexapac의 동시분석법 개발)

  • Jang, Jin;Kim, Heejung;Ko, Ah-Young;Lee, Eun-Hyang;Ju, Yunji;Chang, Moon-Ik;Rhee, Gyu-Seek;Suh, Saejung
    • Korean Journal of Environmental Agriculture
    • /
    • v.34 no.4
    • /
    • pp.318-327
    • /
    • 2015
  • BACKGROUND: Trinexapac-ethyl is a plant growth regulator (PGR) that inhibits the biosynthesis of plant growth hormone (gibberellin). It is used for the prevention of lodging, increasing yields of cereals, and reducing mowing of turf. The experiment was conducted to establish a determination method for trinexapac-ethyl and its metabolites trinexapac in agricultural products using LC-MS/MS.METHODS AND RESULTS: Trinexapac-ethyl and trinexapac were extracted from agricultural products with methanol/ distilled water and the extract was partitioned with dichloromethane and then detected by LC-MS/MS. Limit of detection(LOD) was 0.003 mg/kg and limit of quantification(LOQ) was 0.01 mg/kg, respectively. Matrix matched calibration curves were linear over the calibration ranges (0.01-1.0 mg/L) for all the analytes into blank extract withr2> 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, 50LOQ,n=5). Recoveries of trinexapacethyl and trinexapac were within the range of 73.6-106.9%, 72.7-99.2%, respectively. The relative standard deviations (RSDs) were less than 9.0%. All values were consistent with the criteria ranges requested in the CODEX guideline(CAC/GL 40, 2003).CONCLUSION: The proposed analytical method was accurate, effective and sensitive for trinexapac-ethyl and trinexapac determination and it can be used to as an official method in Korea.

Development and Validation of an Analytical Method for Fungicide Sedaxane Determination in Agricultural Products using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Sedaxane의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Park, Shin-Min;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
    • /
    • v.34 no.1
    • /
    • pp.30-39
    • /
    • 2019
  • An analytical method was developed for the determination of sedaxane in agricultural products using liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, and then purified by using silica SPE cartridges to clean up. The analytes were quantified and confirmed by using LC-MS/MS in positive ion mode using multiple reaction monitoring (MRM). The matrix-matched calibration curves were linear over the calibration ranges ($0.001-0.25{\mu}g/mL$) into a blank extract with $r^2$>0.99. For validation, recovery tests were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ, n=5) with five replicates performed at each level. The recoveries were ranged between 74.5 to 100.8% with relative standard deviations (RSDs) of less than 12.1% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for sedaxane determination in agricultural commodities.

Exosomal Protein Profiles as Novel Biomarkers in Weight Gain After Kidney Transplantation: A Pilot Study

  • Cho, Young-Eun;Lee, Hyangkyu;Kim, Hyungsuk;Yun, Sijung;Cashion, Ann
    • Journal of Korean Biological Nursing Science
    • /
    • v.22 no.2
    • /
    • pp.119-126
    • /
    • 2020
  • Purpose:Weight gain after kidney transplantation is a critical factor that can lead to poor outcomes with cardiovascular complications. Many studies have been conducted to identify predictive markers of future weight changes at the time of transplant. Recently, circulating exosomes and its contents including miRNAs and proteins have attracted attention as potential biomarkers. In this pilot study, we investigated exosomal proteins and weight change after kidney transplant. Methods: Recipients (n = 10) were classified into two groups; weight gainers (n = 5, 9.7 ± 4.4kg) and weight losers (n = 5, -6.4 ± 1.8kg) based on their weight changes at 12-months posttransplant. Based on the exosomal protein profiles obtained by the LC-MS/MS, differentially expressed proteins were identified between the groups. Results: Concentration and the mean size of exosomes significantly increased at 12-months compared to the baseline (p= .009) in the total group. Eleven exosomal proteins were found at the baseline as differentially expressed between the two groups. In the weight gain group, complement proteins including HV169, C3, C4B, and C4A, were significantly upregulated. Conclusion: Our pilot study suggests that exosomal complementary proteins are associated with weight gain after kidney transplantation. Further studies are needed to clarify the role of these exosomal proteins in the underlying mechanisms of weight changes in kidney transplant recipients.

Plant Regeneration from Embryogenic Callus of Miscanthus spp. (억새(Miscanthus spp.) 배발생 캘러스로부터 식물체 재분화)

  • Kim, Kwang-Soo;Kwon, Da-Eun;Lee, Ji-Eun;Cha, Young-Lok;Moon, Youn-Ho;Kang, Yong-Ku
    • Proceedings of the Plant Resources Society of Korea Conference
    • /
    • 2018.10a
    • /
    • pp.89-89
    • /
    • 2018
  • 우리나라, 중국 및 일본을 포함한 동북아시아가 원산이며 바이오매스량이 많은 억새(Miscanthus spp.)는 바이오에너지 생산을 위한 원료작물로서 가치가 높아, 바이오에탄올 생산용 원료작물로 주목을 받고 있다. 독일 등 유럽과 미국에서는 바이오에탄올 생산용 작물로 주로 종간 교잡 이질 3배체인 불임성 억새(M. x giganteous)를 대상으로 연구하고 있다. 이렇게 단일유전형을 갖는 품종의 재배에는 특정 병과 해충에 약하며 자연재해에도 취약성을 나타내므로 억새가 바이오에너지작물로 자리 잡기 위해서는 다양한 유전형의 억새 품종 개발이 필요하다. 본 연구는 우리나라의 자생 억새 3종을 기내배양하고 탈분화 및 재분화 시스템을 구축하여 억새 품종 육성 시 효율을 높이기 위해서 실시하였다. 억새 종자로부터 캘러스의 유도는 MS배지보다 N6배지 에서 좋았으며, 식물생장조절제로 2,4-Dichlorophenoxyacetic acid (2,4-D)와 6-Benzyl aminopurine (BA)를 조합처리한 처리구보다 2,4-D만을 단독처리하였을 때 캘러스 유도율이 더 높았다. 억새 종에 따른 캘러스 유도율은 물억새가 가장 낮고, 거대억새가 가장 높았으며, 3 ~ 5 mg/L의 2,4-D가 첨가된 N6배지에서 배발생 캘러스(embryogenic callus)가 발생하였다. 억새 신초 및 줄기의 절간에서의 캘러스 유도율은 전반적으로 종자에 비하여 낮았으며, 미성숙화기로부터의 캘러스 유도는 억새 종에 따른 차이가 없었으며, 5mg/L의 2,4-D가 첨가된 배지에서 캘러스 유도율이 가장 높게(90 ~ 95%) 나타났다. 형성된 배발생 캘러스로부터 식물체의 재분화는 N6배지에서는 재분화 식물체가 발생하지 않았고, 1 ~ 3mg/L의 BA와 0.1ml/L의 1-Naphthaleneacetic acid (NAA)가 첨가된 MS배지에서만 식물체가 재분화되였다.

  • PDF

Optimal Conditions and Substrate Specificity for Trehalose Production by Resting Cells of Arthrobacter crystallopoietes N-08

  • Seo, Yi-Seul;Shin, Kwang-Soon
    • Preventive Nutrition and Food Science
    • /
    • v.16 no.4
    • /
    • pp.357-363
    • /
    • 2011
  • Recently, we found that Arthrobacter crystallopoietes N-08 isolated from soil directly produces trehalose from maltose by a resting cell reaction. In this study, the optimal set of conditions and substrate specificity for the trehalose production using resting cells was investigated. Optimum temperature and pH of the resting cell reaction were $55^{\circ}C$ and pH 5.5, respectively, and the reaction was stable for two hours at $37{\sim}55^{\circ}C$ and for one hour at the wide pH ranges of 3~9. Various disaccharide substrates with different glycosidic linkages, such as maltose, isomaltose, cellobiose, nigerose, sophorose, and laminaribiose, were converted into trehalose-like spots in thin layer chromatography (TLC). These results indicated broad substrate specificity of this reaction and the possibility that cellobiose could be converted into other trehalose anomers such as ${\alpha},{\beta}$- and ${\beta},{\beta}$-trehalose. Therefore, the product after the resting cell reaction with cellobiose was purified by ${\beta}$-glucosidase treatment and Dowex-1 ($OH^-$) column chromatography and its structure was analyzed. Component sugar and methylation analyses indicated that this cellobiose-conversion product was composed of only non-reducing terminal glucopyranoside. MALDI-TOF and ESI-MS/MS analyses suggested that this oligosaccharide contained a non-reducing disaccharide unit with a 1,1-glucosidic linkage. When this disaccharide was analyzed by $^1H$-NMR and $^{13}C$-NMR, it gave the same signals with ${\alpha}$-D-glucopyranosyl-(1,1)-${\alpha}$-D-glucopyranoside. These results suggest that cellobiose can be converted to ${\alpha},{\alpha}$-trehalose by the resting cells of A. crystallopoietes N-08.

Search for Novel Stress-responsive Protein Components Using a Yeast Mutant Lacking Two Cytosolic Hsp70 Genes, SSA1 and SSA2

  • Matsumoto, Rena;Rakwal, Randeep;Agrawal, Ganesh Kumar;Jung, Young-Ho;Jwa, Nam-Soo;Yonekura, Masami;Iwahashi, Hitoshi;Akama, Kuniko
    • Molecules and Cells
    • /
    • v.21 no.3
    • /
    • pp.381-388
    • /
    • 2006
  • Heat shock proteins (Hsp) 70 are a ubiquitous family of molecular chaperones involved in many cellular processes. A yeast strain, ssa1/2, with two functionally redundant cytosolic Hsp70s (SSA1 and SSA2) deleted shows thermotolerance comparable to mildly heatshocked wild type yeast, as well as increased protein synthesis and ubiquitin-proteasome protein degradation. Since mRNA abundance does not always correlate well with protein expression levels it is essential to study proteins directly. We used a gel-based approach to identify stress-responsive proteins in the ssa1/2 mutant and identified 43 differentially expressed spots. These were trypsin-digested and analyzed by nano electrospray ionization liquid chromatography tandem mass spectrometry (nESI-LC-MS/MS). A total of 22 non-redundant proteins were identified, 11 of which were confirmed by N-terminal sequencing. Nine proteins, most of which were up-regulated (2-fold or more) in the ssa1/2 mutant, proved to be stress-inducible proteins such as molecular chaperones and anti-oxidant proteins, or proteins related to carbohydrate metabolism. Interestingly, a translational factor Hyp2p up-regulated in the mutant was also found to be highly phosphorylated. These results indicate that the cytosolic Hsp70s, Ssa1p and Ssa2p, regulate an abundance of proteins mainly involved in stress responses and protein synthesis.

Plant regeneration from callus of Iris odaesanensis Y. N. Lee native to Korea via organogenesis

  • Bae, Kee-Hwa;Yoo, Kyoung-Hwa;Lee, Mi-Hyun;Jeong, Jae-Hun;Choi, Yong-Eui;Yoon, Eui-Soo
    • Journal of Plant Biotechnology
    • /
    • v.40 no.3
    • /
    • pp.163-168
    • /
    • 2013
  • Iris odaesanensis Y. N. Lee. is an important endangered and native plant belonging to the family Iridaceae in Korea. This study describes a method for rapid micropropagation of this species via from leaf, rhizome and root explants derived calli. Leaf, rhizome and root explants were cultured on Murashige and Skoog (MS) medium supplemented with 2,4-dichlorophenoxy acetic acid (2,4-D) for callus induction. Rhizome explants yielded calli at a frequency of 72% when cultured at 1.0 mg/l 2,4-D. Calli were maintained at 1.0 mg/l 2,4-D. These calli were transferred to MS medium supplemented with 0, 0.5, 1.0, and 2.0 mg/l 2,4-D in combination with 0, 0.5, 1.0, and 3.0 mg/l BA for adventitious shoot induction. The highest number of adventitious shoot (228.9 per petri-dish) were formed at 1.0 mg/l 2,4-D and 1.0 mg/l BA. WPM medium was the best to convert calli into plantlets, where up to 98.2% of calli were regenerated into plantlets. This in vitro propagation protocol should be useful for conservation of this endangered plant.

Volatile Flavor Components of Cultivated Radish (Raphanus sativus L.) Sprout (재배한 무순의 향미성분)

  • 송미란
    • The Korean Journal of Food And Nutrition
    • /
    • v.14 no.1
    • /
    • pp.20-27
    • /
    • 2001
  • The consumption of radish ( Rhaphanus sativus L.) sprout, which is Cruciferae family, is increasing because of its pungent flavor and taste. Its volatile components were analyzed by SDE (simultaneous steam distillation & extraction) method and P&T(purge & cryogenic trapping) method. As a solvent, diethyl ether and diethyl ether : pentane mixture(2:1, v/v) were used in SDE method, and diethyl ether in P&T method. Analyzing by GC and GC-MS, the major component was sulfur compounds (19 species, peak area 76.6%) with diethyl ether, sulfur compounds(15. 44.0%) and hydrocarbons(23, 23.8%) with diethyl ether-pentane mixture in SDE method. Also, hydrocarbons(25, 84.1% ) was major component in P& T method. The major volatile component of fresh radish sprout were n-heptane, methyl pentane and that of boiled radish sprout were 4-methylthio-3-butenyl isothiocyanate, methyl mercaptane, 2,3-dimethyl disulfide. Low molecular volatile components were detected more by P& T method, but types and relative quantities of volatile components were measured less comparing to SDE method.

  • PDF