• Title/Summary/Keyword: $MS^n$

Search Result 1,628, Processing Time 0.031 seconds

Facile Synthesis of 2',5'-Dideoxy-, 2',3'-Dideoxy- and 3'-Deoxy-1, N6-ethenoadenosine Nucleosides

  • Chae, Whi-Gun
    • Biotechnology and Bioprocess Engineering:BBE
    • /
    • v.4 no.1
    • /
    • pp.17-20
    • /
    • 1999
  • Facile synthetic methods of 2',5'-dideoxy-, 2',3'-dideoxy- and 3'-deoxy-1, N6-ethenoadenosine nucleosides by either an enzymatic dideoxyribosyl transfer reaction or a simple chemical reaction were proposed. The synthesis products were isolated and purified by preparative HPLC and their structures were confirmed by 1H NMR (500 MHz) and FAB-MS including high resolution mass measurement. These modified nucleoside analogs have not been reported yet. Therefore, these modified nucleoside analogs are of potential value to be studied further for biological activity such as anticancer or antiviral.

  • PDF

Mass Spectrometry in the Determination of Glycosylation Site and N-Glycan Structures of Human Placental Alkaline Phosphatase

  • Solakyildirim, Kemal;Li, Lingyun;Linhardt, Robert J.
    • Mass Spectrometry Letters
    • /
    • v.9 no.3
    • /
    • pp.67-72
    • /
    • 2018
  • Alkaline phosphatase (AP) is a membrane-bound glycoprotein that is widely distributed in the plasma membrane of cells of various organs and also found in many organisms from bacteria to humans. The complete amino acid sequence and three-dimensional structure of human placental alkaline phosphatase have been reported. Based on the literature data, AP consists of two presumptive glycosylation sites, at Asn-144 and Asn-271. However, it only contains a single occupied N-linked glycosylation site and no occupied O-linked glycosylation sites. Hydrophilic interaction chromatography (HILIC) has been primarily employed for the characterization of the glycan structures derived from glycoproteins. N-glycan structures from human placental alkaline phosphatase (PLAP) were investigated using HILIC-Orbitrap MS, and subsequent data processing and glycan assignment software. 16 structures including 10 sialylated N-glycans were identified from PLAP.

Programming characteristics of single-poly EEPROM (Single-poly EEPROM 의 프로그램 특성)

  • 한재천;나기열;이성철;김영석
    • Journal of the Korean Institute of Telematics and Electronics A
    • /
    • v.33A no.2
    • /
    • pp.131-139
    • /
    • 1996
  • Inthis apper wa analyzed the channel-hot-electron programming characteristics of the single-poly EEPROM with different control gate and drain structures. The single-poly EEPROM uses the p$^{+}$/n$^{+}$-diffusion in the n-well as a control gate instead of the second poly-silicon. The program and erase characteristics of the single-poly EEPROM were verified using the two-dimensional device simulator, MEDICI. The single-poly EEPROM was fabricated using 0.8$\mu$m ASIC CMOS process, and its CHE programming characteristics were measured using HP4155 parameteric analyzer and HP8110 pulse gnerator. Especially we investigated the CHE programming characteristics of the single-poly EEPROM with the p$^{+}$-diffusion or n$^{+}$-diffusion in the n-well as a control gate and the LDD or single-drain structure. The single-poly EEPROM with p$^{+}$-diffusion in the n-well as a control gate and single-drain structure was programmed to about VT$\thickapprox$5V with VDS=6V, VCG=12V(1ms pulse width).th).

  • PDF

A new sensitive determination method of propylene oxide-hemoglobin adducts by EI-GC-MS (SIM)

  • Shin, Ho-Sang;Lee, Jin-Heon;Ahn, Hye-Sil
    • Proceedings of the Korean Environmental Health Society Conference
    • /
    • 2004.06a
    • /
    • pp.169-172
    • /
    • 2004
  • A gas chromatography/mass spectrometric assay method was developed for the determination of propylene oxide adduct, N-(3-hydroxypropyl)valine. Adduct was released from hemoglobin by alkaline hydrolysis and extract at pH 8 with ethyl ether. The dried extract was completely derivatized with N-Methyl-N-(trimethylsilyl) trifluoroacetamide (MSTFA)/TMS-I (100:3). The detection limits of the assay were 0.08 ng/g for N-(3-hydroxypropyl)valine based upon assayed hemoglobin of 0.1 g. The method was applied to the determination of propylene oxide adduct formed in young female Sprague-Dawley rats after treatment for 1, 2 and 3 weeks with 0.008 % propylene oxide via the drinking water. An adduct was detected by proposed procedure. The structure of the adduct could be assigned to N-(3-hydroxypropyl)valine.

  • PDF

Indentification of Some Metabolites of Carbinoxamine in Rat Urine (흰쥐 뇨에서의 Carbinoxamine의 대사체 확인)

  • 정병화;이선화;김태욱;정봉철;박종세
    • YAKHAK HOEJI
    • /
    • v.37 no.4
    • /
    • pp.317-324
    • /
    • 1993
  • The metabolic profile of carbinoxamine, 2-[(4-chlorophenyl)-2-pyridinyi-methoxy] N, N-dimethylethanamine, was determined in rat urine. Urinary extracts obtained with or without enzyme hydrolysis were derivatized with MSTFA/TMSCI (N-methyl-N-trimethylsilyl trifluoroacetamide/Trimethylchlorosilane) and analyzed by GC/MSD. In rat urine, which obtained after oral treatment with carbinoxamine maleate, chlorobenzolyl pyridine, (4-chlorophenyl)-2-pyridinyl methanol : carbinol, 2-[(4-chlorophenyl)-2-pyridinylmethoxy]-N-methylethanamine : norcarbinoxamine, 2-[(4-chlorophenyl)2-pyridinylmethoxy]ethanamine : bis-norcarbinoxamine and parent carbinoxamine were detected in free form. Norcarbinoxamine and bisnorcarbinoxamine were also detected in conjugated form(acetylation). These data suggest that in the rat, hydroxylation of either the benzyl or pyridinyl ring can occur during carbinoxamine elimination. O-demethylation and subsequent conjugation represents the primary pathway of carbinoxamine elimination in the rat.

  • PDF

Effect of pulse frequency and duty cycle on microstructure, residual stress and mechanical properties of ZrN coatings deposited by mid-frequency magnetron sputtering (펄스 주파수 및 듀티 사이클이 중간 주파수 마그네트론 스퍼터법으로 증착된 ZrN 코팅막의 미세구조, 잔류응력 및 기계적 특성에 미치는 영향)

  • Sung-Yong Chun
    • Journal of Surface Science and Engineering
    • /
    • v.57 no.4
    • /
    • pp.348-354
    • /
    • 2024
  • Nanocrystalline zirconium nitride (ZrN) coatings were deposited by mid-frequency direct current sputtering (mfMS) with varying pulsed plasma parameters such as pulse frequency and duty cycle to understand the effect of pulsed plasma on the microstructure, residual stress and mechanical properties. The results show that, with the increasing pulse frequency and decreasing duty cycle, the coating morphology changed from a porous columnar to a dense structure, with finer grains. Mid-frequency magnetron sputtered ZrN coatings with pulse frequency of 30 kHz showed the highest both nanoindentation hardness of 16.3 GPa, and elastic modulus of 214.4 GPa. In addition, Effect of pulse frequency on a residual stress and average crystal grain sizes was also investigated.

Development of a Microsatellite Marker Set for the Individual Identification and Parentage Verification of Korean Native Black Goats (재래흑염소 개체식별과 친자확인을 위한 Microsatellite Marker Set 개발)

  • Lee, Sang-Hoon;Kang, Ho-Chan;Lee, Sung-Soo;Lee, Jinwook;Kim, Eun-Ho;Myung, Hyun-Cheol;Kim, Kwan-Woo;Lim, Hyun-Tae
    • Journal of Life Science
    • /
    • v.30 no.10
    • /
    • pp.912-918
    • /
    • 2020
  • The Korean native black goat (Capra hircus coreanae) is the goat species to be officially registered in Korea under the Food and Agriculture Organization. The object of this study is to establish a set of microsatellite (MS) markers for the individual identification and parentage verification of goats. In this study, we analyzed alleles of MS markers in crosses between Korean native black goats and crossbred goats (n=304 animals), and, based on the diversity of alleles for each marker, we selected 11 MS markers for individual identification and parentage verification. Using these 11 MS markers, the probabilities of different individuals with the same genotype being found within random and half-sib mating populations were 5.58×10-10 and 1.15×10-7, respectively. The parentage verification accuracy was 0.999996 when information about the parents was available and 0.999833 with no information. Thus, even given the total rearing population of 576,150 animals in South Korea, we concluded that these markers could be used for the individual identification and parentage verification of goats. Moreover, by analyzing the genetic relationships between the four lines of Korean native black goats and the crossbred goats, we verified the genetic characteristics of Korean native black goats, confirming their conservation value as a unique genetic resource.

Development of Individual Residue Analysis Method for Cyanazine in Agricultural Commodities as an Unregistered Herbicide in Korea (국내 미등록 제초제 cyanazine의 농산물 중 개별 잔류분석법 개발)

  • Choung, Myoung-Gun;Im, Moo-Hyeog
    • Journal of the Korean Society of International Agriculture
    • /
    • v.30 no.4
    • /
    • pp.339-346
    • /
    • 2018
  • Cyanazine is a member of the triazine family of herbicides. Cyanazine is used as a pre- and post-emergence herbicide for the control of annual grasses and broadleaf weeds. This experiment was conducted to establish a determination method for cyanazine, as domestic unregistered pesticide, residue in major agricultural commodities using HPLC-DAD/MS. Cyanazine was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and partitioned to dichloromethane for remove polar extractive in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized florisil column chromatography. On a $C_{18}$ column in HPLC, cyanazine was successfully separated from co-extractives of sample, and sensitively quantitated by diode array detection at 220 nm. Accuracy and precision of the proposed method was validated by the recovery experiment on every major agricultural commodity samples fortified with cyanazine at 3 concentration levels per agricultural commodity in each triplication. Mean recoveries were ranged from 83.6 to 93.3% in five major representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring(SIM) technique was also provided to clearly identify the suspected residue.

Development and Validation of an Analytical Method for β-Agonists in Livestock and Fishery Products Using LC-MS/MS (LC-MS/MS를 이용한 축·수산물 중 β-agonist계 시험법 개발 및 검증)

  • Lee, Tae Ho;Kim, Yu Ra;Park, Su Jeong;Kim, Ji Young;Choi, Jang Duck;Moon, Gui Im
    • Korean Journal of Environmental Agriculture
    • /
    • v.41 no.2
    • /
    • pp.135-151
    • /
    • 2022
  • BACKGROUND: The β-agonists known as phenyl ethanolamine derivatives have a conjugated aromatic ring with amino group. They are used as tocolytic agents and bronchodilator to human and animal generally, and some of them are used as growth promoters to livestock. METHODS AND RESULTS: β-agonists in samples were extracted by 0.4 N perchloric acid and ethyl acetate. The target compounds were analyzed by liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS). Validation of method was performed according to CODEX guidelines (CAC/GL-71). The matrix matched calibration gave correlation coefficients>0.98, and the obtained recoveries were in the range of 62.0-109.8%, with relative standard deviation ≤ 20.1%. In addition, a survey was performed to inspect any residual β-agonist from 100 samples of livestock and fishery products and ractopamine was detected in one of the 100 samples. CONCLUSION(S): In this study, we established the analytical method for β-agonists through using the expanded target compounds and samples. And we anticipate that the established method would be used for analysis to determine veterinary drug residues in livestock and fishery products.

Simultaneous Determination of Cholesterol, Bile Acids and Sterols in Human Bile Juices and Gallstones Using GC/MS (GC/MS에 의한 담석과 담즙내의 Cholesterol, Bile Acids 및 Sterols의 동시 Profiling)

  • Yang, Yoon Jung;Lee, Seon Hwa;Kim, Hyun Joo;Chung, Bong Chul
    • Journal of the Korean Chemical Society
    • /
    • v.42 no.3
    • /
    • pp.266-276
    • /
    • 1998
  • Cholesterol supersaturation in bile, which causes gallstone formation, is the result of low bile acid secretion or high cholesterol secretion. The quantitative analysis of cholesterol, bile acids and sterols which are precursors of cholesterol have been used to examine the changes in bile component. We described a simple, sensitive and reproducible method for simultaneous determination of cholesterol, five bile acids and seven sterols in human bile juices and gallstones by capillary column gas chromatography-mass spectrometry (GC/MS). Clinical samples were hydrolyzed by alcoholic KOH, extracted twice (pH 14 and 1) and derivatized to trimethylsilyl (TMS) ether with $MSTFA/NH_4I$ (N-methyl-N-trimethylsilyltrifluoroacetamide/ammonium iodide) mixture in order to be detected on the GC/MS. The good quality control data were obtained through within-a-day and day-to-day test (RSD values were 1.72-13.79, 0.68-14.10, respectively) and the recovery range of them was 73.56-96. 95 Using this method, biliary and gallstone compositions in the patients with intrahepatic stones were analyzed. The amounts and its relative distribution of cholesterol, bile acids and sterols showed different pattern in bile juices and gallstones.

  • PDF