• Title/Summary/Keyword: $MS^n$

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Design, Synthesis and Spectral Characterization of Novel 2-morpholino-N-(4,6-diarylpyrimidin-2-yl)acetamides (새로운 2-morpholino-N-(4,6-diarylpyrimidin-2-yl)acetamides의 합성과 분광학적 특성의 연구)

  • Kanagarajan, Vijayakumar;Thanusu, Jayaraman;Gopalakrishnan, Mannathusamy
    • Journal of the Korean Chemical Society
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    • v.54 no.1
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    • pp.49-54
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    • 2010
  • A new series of novel 2-morpholino-N-(4,6-diarylpyrimidin-2-yl)acetamides 34-42 is synthesized by the condensation of 2-chloro-N-(4,6-diarylpyrimidin-2-yl)acetamides 25-33 with morpholine in the presence of anhydrous potassium carbonate. The synthesized compounds have been characterized by melting point, elemental analysis, MS, FT-IR, one-dimensional NMR ($^1H$ & $^{13}C$) spectroscopic data.

Effect of Electroacupuncture Stimulation on Activity of Neuronal NOS in Rats (흰쥐의 neuronal NOS 신경세포의 activity에 대한 전침자극 효과)

  • Kim, Hoo-Dong;Nam, Sang-Soo;Kim, Chang-Hwan
    • Journal of Acupuncture Research
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    • v.23 no.5
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    • pp.199-206
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    • 2006
  • Objectives : The aim of this study was to investigate the effect of various electroacupuncture stimulation on neuronal nitric oxide synthase(nNOS) in cerebral cortex, brain stem, cerebellum of spontaneously hypertensive rats. Methods : We evaluated the changes of nNOS-positive neurons using a immunohistochemical method. The staining intensity of nNOS positive neurons was assessed in a quantitative fashion using a microdensitometrical method based on optical density by means of an image analyzer. Results : The average optical density of nNOS-positive neurons of 100 Hz (bipolar square wave 0.2 ms duration and 100 Hz frequency) electroacupuncture treatment group significantly decreased in most cortical areas comparison between the manual acupuncture and 2 Hz (bipolar square wave 0.2 ms duration and 2 Hz frequency) electroacupuncture groups. In the brain stem, the optical density of nNOS-positive neuron at superficial gray layer of the superior colliculus area, dorsolateral periaqueductal gray area and paralemniscal nucleus were same as cerebral cortex. Conclusion : We conclude that the morphological evidence for nNOS-positive neurons may be have regional change in cerebral cortex brain stem and cerebellum according to various electroacupuncture stimulations.

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Potential of Fuel Stratification for Reducing Pressure Rise Rate in HCCI Engines (HCCI 기관에 있어서의 층상 흡기를 통한 압력 상승률 저감에 대한 연구)

  • Lim, Ock-Taeck
    • Journal of the Korean Institute of Gas
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    • v.14 no.6
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    • pp.7-14
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    • 2010
  • This study investigated the effect on reducing the pressure rise rate(PRR) in HCCI Engine by the variation of mixing ratio in the pre-mixture of DME and n-Butane that has different auto-ignition characteristics. In addition to measure of gas pressure in the engine cylinder, chemiluminescence image using the optical accessible engine and numerical analysis with multi-zones model were used to assess the combustion at each local area in the combustion chamber. The maximum PRR changes depending on mixing condition of DME and n-Butane. When DME is stratified and n-Butane is distributed uniformly, maximum PRR becomes lowest which is about 0.25MPa/ms and it corresponds to 5deg. retarding of CA50.

Effects of Slow-Release Nitrogen Fertilizers, Latex Coated Urea and Meister10, on Direct Seeded Rice in Dry Soil (벼 건답직파재배시 완효성질소비료의 시용 효과)

  • Back, Jun-Ho;Jang, Myung-Hwan;Lee, Seung-Ho;Lee, Sang-Jo;Lim, Jun-Young;Kim, Bok-Jin
    • Korean Journal of Soil Science and Fertilizer
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    • v.34 no.6
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    • pp.407-412
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    • 2001
  • This study was conducted to find out the effect of slow-release nitrogen fertilizer, such as latex coated urea(LCU) and Meister10(MS10) on direct seeded rice in dry soil(DS). Junghwabyeo, and early maturity rice cultivar was grown on the plots which were treated with None-nitrogen. urea. LCU and MS10 plot. Growth characteristic, yield and yield components were investigated. Nitrogen uptake-efficiency and physico-chemical properties of soil before-after experiment were analyzed. Plant height and number of tillers $m^{-2}$ in LCU and MS10 plot at early grow stages were higher than those in urea plot. Plant height and number of tillers $m^{-2}$ grown on the plot of Ms10 plot were higher than those of LCU plot. The number of seedling $m^{-2}$ were no significant differences among None-N, urea, and MS10 plot in DS. Heading date and leaf color were higher with Urea than LCU and MS10 plot. Culm length in LCU and MS10 plot were longer compared with urea plot, but panicle length was similar among with Urea, LCU and MS10 plot. Number of panicles $m^{-2}$ was greater in order of MS10 > LCU > Urea plot. Yield were greater in order of MS10 > LCU > Urea plot. Nitrogen uptake and nitrogen efficiency were greater in order of MS10 > LCU > urea plot. After the experiment, total content of nitrogen in soil was not changed at all treatments, but pH, P and Si of soil were lower than those of before experiment at all treatments.

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Chemical Analysis of Cuticular Hydrocarbons in Apis mellifera L. and Apis cerana F. (동양종과 서양종 꿀벌의 표피탄화수소 성분 분석)

  • 이창주;신경우;박승찬;심재한
    • Korean journal of applied entomology
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    • v.42 no.1
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    • pp.9-13
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    • 2003
  • Cuticular hydrocarbons of antenna, legs and wings from two species of honeybee worker of Apis mellifera L. and Apis cerana F. can be analyzed directly with gas chromatograph and GC/MS without solvent extraction. The saturated hydrocarbons identified in selected part of both species were nC22, nC23, nC25-nC3O, nC32 and nC34 except nC24. Two saturated hydrocarbons, nC26 (23.0-42.6%) and nC28 (16.8-54.8%), were major compounds in both species and others were minor compounds. A. mellifera can be distinguished from A. cerana F. by having higher proportion of nC30, nC32 and nC34 by having lower proportion of nC25 from three selected part of both species.

Development of LC-MS/MS Quantitation Method for Ethoxyquin in Fishery Products (수산물 중 에톡시퀸의 LC-MS/MS 정량분석법 개발)

  • Shin, Dasom;Chae, Young-Sik;Kang, Hui-Seung;Lee, Soo-Bin;Cho, Yoon-Jae;Cheon, So-Young;Jeong, Jiyoon;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.31 no.6
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    • pp.432-438
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    • 2016
  • Ethoxyquin (EQ, 1,2-dihydro-6-ethoxy-2,2,4-trimethyl-quinoline) is quinoline-based antioxidant used in the animal feed and food industry to protect the raw materials and final products against oxidation. In recent years the use of synthetic antioxidants in fishmeal ingredients carry-over to farmed fish fillets has received increasing attention in food safety. This study was conducted to develop an analytical method to determine EQ in aquatic products. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with 1 N HCl (in case of flatfish extracted with 1 N HCl containing 10% acetonitrile). Then, solid phase extraction (SPE) was used for the cleanup. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.99, analyzed at 0.005-0.2 mg/kg concentration. The developed method was validated according to the Codex Alimentarius Commission (CAC) guideline. The limits of quantitation for EQ were 0.01 mg/kg. Average recoveries ranged from 81.3% to 107%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was below 10%. The analytical method was characterized with high accuracy and acceptable sensitivity to meet CODEX guideline requirements and would be applicable to analyze the EQ residue in aquatic products.

Survey and method validation of simultaneous quantitative analysis of T-2 and HT-2 toxins in cereals (곡류 중 T-2 및 HT-2 독소 동시 정량분석의 유효성 검증 및 실태조사)

  • Paek, Ockjin;Kang, Teabeom
    • Food Science and Preservation
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    • v.22 no.4
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    • pp.559-566
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    • 2015
  • The aim of this study was to develop an analytical method for determination of T-2 toxin and HT-2 toxin level in cereals and to survey their levels using LC-MS/MS. The T-2 and HT-2 toxins were simultaneously analyzed by electrospray ionization with a positive ion mode and multiple reaction monitoring (MRM) after filteration and immuno-affinity column clean-up. A matrix-matched standard calibration used for quantification and recoveries of T-2 and HT-3 toxins were in the range of $100.6{\pm}7.2%$ and $96.8{\pm}9.4%$, respectively. Limits of detection and quantification of T-2 and HT-2 toxins were estimated to be 0.5 and $1.5{\mu}g/kg$, respectively. Each repeatability (RSRr) of T-2 and HT-2 toxins was determined to be 0.9~6.0%, and 4.9~6.1%, respectively. Total 115 samples cereals were collected from 9 types of cereals for analysis. The positive percentages of T-2 and HT-2 toxins obtained from collected samples were found to be 72% and 80%, respectively. The contamination level of T-2 toxin and HT-2 toxin in cereals were $37.1{\mu}g/kg$, and $5.4{\mu}g/kg$, respectively. Therefore, this study suggests that the developed method could be an useful analytical method to determine the T-2 and HT-2 toxin level in cereals and the present data could be used as a reference to estimate the risk assessment.

Analysis of Glyphosate and Glufosinate in Animal Feeds using LC-MS/MS (LC-MS/MS를 이용한 동물 사료 내 글라이포세이트 및 글루포시네이트 분석)

  • Lee, Ji-Su;Kim, Wanseo;Yang, Heedeuk;Park, Na-Youn;Jung, Woong;Kim, Junghoan;Kho, Younglim
    • Journal of the Korean Chemical Society
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    • v.63 no.5
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    • pp.342-345
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    • 2019
  • The standards for the contents of glyphosate and glufosinate in foods are specific and well categorized. However, the standard of content in animal feeds is relatively inadequate and the classification is insufficient. There is also constant debate about the risk of glyphosate and glufosinate to human health, but the risk to animals has not been well studied. In this study, we established an analytical method in feeds that is estimated to be the path for animals to ingest glyphosate. The solvent extraction was carried out using 25% methanol. After centrifugation, samples were purified using solid phase extraction (SPE) and quantitatively analysed using LC-MS/MS after concentrated. Assessment of validation was conducted through detection limits, accuracy, and precision tests. The detection limits for the established method were 1.8 of ${\mu}g/kg$ of glufosinate and $2.4{\mu}g/kg$ of glyphosate. Accuracy was ranged from 94.4% to 103.4% and precision was range from 1.5% to 7.2%. Glufosinate was detected in one sample ($ND{\sim}8.8{\mu}g/kg$) and glyphosate was detected in all but one sample ($ND{\sim}337.0{\mu}g/kg$) by applying the analytical method to animal feeds (n=13).

Simultaneous analysis of residual glucocorticoids in egg by LC/MS/MS (LC/MS/MS를 이용한 계란 중 잔류 글루코코티코이드의 동시분석)

  • Jang, Mi-Ae;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.326-335
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    • 2009
  • A specific analytical method able to identify and quantify traces of six glucocorticoids residues in eggs were developed. The extraction and clean-up parameters for simultaneous analysis were evaluated and HPLC and spectrometric conditions were also established. For determination of glucocorticoids, 5 g of egg was transferred into a test tube, adjusted pH 5.2 with acetate buffer and was $\beta$-glucuronidase/arylsulfatase from Helix pomatia added. The mixture was centrifuged and supernatant was extracted twice with 20 mL n-hexane. The extraction was performed with HLB cartridge using methanol, followed by clean-up with silica cartridge using methanol/ethyl acetate (4/6, v/v). The analytes were determined by HPLC/ESI-MS/MS operating in the negative ion mode. Validation studies with fortified egg samples for established method were performed. The result of method validation gave good efficiency, linearity, accuracy and precision. The correlation coefficients ($r^2$) of the calibration curves appeared to be higher than 0.99 in egg, indicating excellent linearity. LOD was ranged 0.09 to $0.17{\mu}g/kg$, and recoveries for most compounds were in the range of 55.7-69.8%. This method can be used to determine ${\mu}g/kg$ levels of glucocorticoids in eggs.

Method Development and Validation of Strychnine in Blood by Gas Chromatography/Mass Spectrometry Using Solid Phase Extraction and its Application in Real Specimens (SPE 및 GC/MS에 의한 혈액중 스트리크닌의 분석법 개발 및 검출사례)

  • Rhee, Jongsook;Yum, Hyesun;Moon, Sungmin;Lee, Sangki
    • YAKHAK HOEJI
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    • v.57 no.2
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    • pp.87-94
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    • 2013
  • An analytical methodology based on solid-space extraction (SPE) with with Bond Elut Certify cartridge (Varian, 130 mg) has been developed for the qualification and quantitation of strychnine in blood. After the elution layer was evaporated, the residue was reconstituted with methanol for GC/MS. Internal standard was used 10 mg/l dextromethorphan. Strychnine is a potent central nervous stimulant and convulsant, and an alkaloid found in seeds of Strychnos nux-vomica. It was used therapeutically to improve circulation and muscle tone in oral or intramuscular doses of 0.05~8 mg. The fatal dose of strychnine for humans is 50~100 mg. A man was found dead lying curled up the corner of the large room in a roof house after the fire fighter opened a locked door inside to put out the fire. The postmortem blood and gastric contents were analyzed for toxicological testing. Strychnine and brucine were detected using GC/MS first in gastric contents extracts. The contents of strychnine was 0.083 mg/l in heart blood, 0.088 mg/l in peripheral blood and 4.0 mg/kg in gastric contents, respectively. Method validation was carried out in terms of linearity, accuracy, precision (intraday, interday) in blood. The assay is linear over 0.05~10 mg/l ($r^2$=0.999). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.02 mg/l (S/N=3) and 0.07 mg/l (S/N=10), respectively. Accuracy (bias%) of strychnine with 0.1, 1 and 10 mg/l was 12.0% (n=6), 9.3% (n=6) and 6.9% (n=6), respectively. Intraday precision (CV%) of strychnine with, 0.1, 1 and 10 mg/l were 6.4%, 10.4%, 1.2% (n=6), respectively. Interday precision (CV%) of strychnine with 0.1, 1 and 10 mg/l over three days were 24.0%, 18.5%, 13.8% (n=18), respectively. Relative recovery with 0.1, 1 and 10 mg/l (in blood) were 114.9%, 99.3% and 87.4% (n=6), respectively. The described method can be applied in forensic toxicology to determine strychnine in blood samples.