• Title/Summary/Keyword: Mass Spectrometer

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Synthesis of Cyclen-Based Copper Complexes as a Potential Estrogen Receptor Ligand (에스트로젠 수용체 리간드로서 사이클렌을 기본 구조로 한 구리 착물의 합성)

  • Park, Jeong-Chan;Pandya, Darpan N.;Jeon, Hak-Rim;Lee, Sang-Woo;Ahn, Byeong-Cheol;Lee, Jae-Tae;Yoo, Jeong-Soo
    • Nuclear Medicine and Molecular Imaging
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    • v.41 no.4
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    • pp.326-334
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    • 2007
  • Purpose: The estrogen receptor (ER), which is over-expressed in ER-positive breast tumors, has been imaged by positron emission tomography (PET) using $[^{18}F]$ labeled estrogen ligands, especially $[^{18}F]FES$. However, $[^{18}F]$ has relatively short-lived half-life ($t_{1/2}$ =1.8 h) and the labeling yield of radio-fluorination is usually low compared with $^{64}Cu\;(t_{1/2}=12.7\;h)$. 1,4,7,10-tetraazacyclododecane (cyclen) is used to form stable metal complexes with copper, indium, gallium, and gadolinium. With these in mind, we prepared cyclen-based Cu complexes which mimic estradiol in aspect of two hydroxyl groups. Materials and Methods: 1.7-Protected cyclen, 1.7-bis (benzyloxycarbonyl)-cyclen was synthesized according to the reported procedure. After introducing two 4-benzyloxybenzyl groups at 4,10-positions, the benzyloxycarbonyl and benzyl groups were removed at the same time by hydrogenation on Pd/C to give 1,7-bis(4-hydroxybenzyl)-1,4,7,10-tetraazacyclododecane (1). Results: The prepared ligand 1 was fully characterized by $^1H,\;^{13}C$ NMR, and mass spectrometer. The synthesized ligand was reacted with copper chloride and copper perchlorate to give copper complexes $[Cu(1)]^{2+}2(CIO_4^-)\;and\;[Cu(1)Cl]^+Cl^-$ which were confirmed by high-resolution mass (FAB). Conclusion: We successfully synthesized a cyclen derivative of which two phenol groups are located on trans position of N-atoms. And, two Cu(ll) complexes of +2 and +1 overall charge, were prepared as a potential PET tracers for ER imaging.

Calibration of δ13C values of CO2 gas with different concentrations in the analysis with Laser Absorption Spectrometry (레이저흡광분석기(Laser Absorption Spectrometry)를 이용한 CO2가스의 탄소안정동위원소비 보정식 산출)

  • Jeong, Taeyang;Woo, Nam C.;Shin, Woo-Jin;Bong, Yeon-Sik;Choi, Seunghyun;Kim, Youn-Tae
    • Economic and Environmental Geology
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    • v.50 no.6
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    • pp.537-544
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    • 2017
  • Stable carbon isotope ratio of carbon dioxide (${\delta}^{13}C_{CO2}$) is used as an important indicator in the researches for global climate change and carbon capture and sequestration technology. The ${\delta}^{13}C$ value has been usually analyzed with Isotope Ratio Mass Spectrometer (IRMS). Recently, the use of Laser Absorption Spectrometry (LAS) is increasing because of the cost efficiency and field applicability. The purpose of this study was to suggest practical procedures to prepare laboratory reference gases for ${\delta}^{13}C_{CO2}$ analysis using LAS. $CO_2$ gas was adjusted to have the concentrations within the analytical range. Then, the concentration of $CO_2$ was assessed in a lab approved by the Korea Laboratory Accreditation Scheme and the ${\delta}^{13}C_{CO2}$ value was measured by IRMS. When the instrument ran over 12 hours, the ${\delta}^{13}C$ values were drifted up to ${\pm}10$‰ if the concentration of $CO_2$ was shifted up to 1.0% of relative standard deviation. Therefore, periodical investigation of analytical suitability and correction should be conducted. Because ${\delta}^{13}C_{CO2}$ showed the dependency on $CO_2$ concentration, we suggested the equation for calibrating the concentration effect. After calibration, ${\delta}^{13}C_{CO2}$ was well matched with the result of IRMS within ${\pm}0.52$‰.

A Study on the Characteristics of PM1.0 Chemical Components Using a Real-time Aerosol Mass Spectrometer (실시간 에어로졸 질량분석기를 이용한 PM1.0의 화학적성분의 특성에 관한 연구)

  • Park, Jinsoo;Choi, Jinsoo;Kim, Hyunjae;Oh, Jun;Sung, Minyoung;Ahn, Joonyoung;Lee, Sangbo;Kim, Jeongho
    • Journal of the Korean Society of Urban Environment
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    • v.18 no.4
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    • pp.485-494
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    • 2018
  • This study aims to identify the characteristics of oxidation and chemical composition of PM in winter season, 2017 at Incheon area. The mean concentration of air pollutants were $46{\pm}22{\mu}g/m^3-PM_{10}$, $29{\pm}18{\mu}g/m^3/-PM_{2.5}$, $5{\pm}3ppb-SO_2$, $0.56{\pm}0.24ppm-CO$, $21{\pm}13ppb-O_3$ and $28{\pm}17ppb-NO_2$, respectively. The dominant ion of the $PM_{1.0}$ chemical component were organic with $3.2{\mu}g/m^3$ and nitrate with $1.9{\mu}g/m^3$. The day and night variation of the $PM_{1.0}$ chemical components was higher in nighttime than those of daytime. The averaged nitrate oxidation rate (SOR) was 0.06 and sulfate oxidation rate was 0.11 during the field campaign. In the high mass loading period, nitrate oxidation rate (NOR) was up to 0.6 and also the nitrate in $PM_{1.0}$ was increased. The averaged ratio of $NO_x/SO_2$ was 8.7 and nitrate/sulfate was 3.1, respectively. In this results, the nitrate component in $PM_{1.0}$ was influenced by NOx from the stationary source as power plant and the mobile source around the measurement site.

Investigation of Heavy Metal Migration from Food Contact Materials used for Food Delivery Using an Inductively Coupled Plasma-Mass Spectrometer

  • Chae-Yeon Hwang;Young-Jun Kim
    • Journal of Food Hygiene and Safety
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    • v.38 no.2
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    • pp.37-45
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    • 2023
  • The surge in food delivery systems during the coronavirus 2019 pandemic necessitated this study of heavy metal migration from food contact materials (FCMs). A total of 104 samples of FCMs, comprising 51 polypropylene (PP), 21 polyethylene (PE), and 32 polystyrene (PS) samples of six different types of FCMs (containers, covers, table utensils, cups, pouches, and wrappers) used for food delivery distributed in Korea, were collected and investigated for migration of three heavy metals (Pb, Cd, and As) using inductively coupled plasma-mass spectrometry (ICP-MS) to determine whether they complied with Korea's Standards and Specifications for Utensils, Containers, and Packages. Acetic acid (4%, v/v) was used as the food simulant, and tests were performed at 100℃ (in harsh conditions) for 30 min. Linearity of Pb, Cd, and As showed acceptable results with a coefficient of determination (R2) value of 0.9999. Limit of detection (LOD) and limit of quantification (LOQ) of Pb, Cd, and As were 0.001, 0.001, and 0.001 ㎍/L and 0.002, 0.003, and 0.003 ㎍/L, respectively. Accuracy and precision results complied with the criteria presented in the European Commission Joint Research Centre guidelines. The average concentration of Pb, Cd, and As migration detected in a total of 104 samples was 0.009-0.260 ㎍/L, which was very low compared with the migration specification set in the Standards and Specifications for Utensils, Containers, and Packages. The maximum level of Pb corresponded to 0.23% of the migration limit. There were no samples exceeding the limit. Thus, this study confirmed that the heavy metal contents of FCMs used for delivery food distributed in Korea were safely managed. The data from this study represent an invaluable source for science-based safety management of hazardous heavy metals migrating from FCMs used in the food delivery industry.

The progress in NF3 destruction efficiencies of electrically heated scrubbers (전기가열방식 스크러버의 NF3 제거 효율)

  • Moon, Dong Min;Lee, Jin Bok;Lee, Jee-Yon;Kim, Dong Hyun;Lee, Suk Hyun;Lee, Myung Gyu;Kim, Jin Seog
    • Analytical Science and Technology
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    • v.19 no.6
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    • pp.535-543
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    • 2006
  • Being used widely in semiconductor and display manufacturing, $NF_3$ is internationally considered as one of the regulated compounds in emission. Numerous companies have been continuously trying to reduce the emissions of $NF_3$ to comply with the global environmental regulation. This work is made to report the destruction and removal efficiency (DRE) of electrically heated scrubbers and the use rate in process chambers installed in three main LCD manufacturing companies in Korea. As the measurement techniques for $NF_3$ emission, mass flow controlled helium gas was continuously supplied into the equipment by which scrubber efficiency is being measured. The partial pressures of $NF_3$ and helium were accurately measured for each sample using a mass spectrometer, as it is emitted from inlet and outlet of the scrubber system. The results show that the DRE value for electrically heated scrubbers installed before 2004 is less than 52 %, while that for the new scrubbers modified based on measurement by scrubber manufacturer has been sigificentely improved upto more than 95 %. In additon, we have confirmed the efficiency depends on such variables as the inlet gas flow rate, water content, heater temperature, and preventative management period. The use rates of $NF_3$ in process chambers were also affected by the process type. The use rate of radio frequency source chambers, built in the $1^{st}$ and $2^{nd}$ generation process lines, was determined to be less than 75 %. In addition, that of remote plasma source chambers for the $3^{rd}$ generation was measured to be aboove 95 %. Therefore, the combined application of improved scrubber and the RPSC process chamber to the semiconductor and display process can reduce $NF_3$ emmision by 99.95 %. It is optimistic that the mission for the reduction of greenhouse gas emission can be realized in these LCD manufacturing companies in Korea.

Development and Validation of an Official Analytical Method for Determination of Ipfencarbazone in Agricultural Products using GC-ECD (GC-ECD를 이용한 농산물 중 Ipfencarbazone의 신규분석법 개발 및 검증)

  • Jang, Jin;Kim, Heejung;Lee, Eun-Hyang;Ko, Ah-Young;Ju, Yunji;Kim, Sooyeon;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.210-217
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    • 2015
  • Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.

Isolation of Isoflavones and Soyasaponins from the Germ of Soybean (콩 배아로 부터 Isoflavone과 Soyasaponin의 동시 분리)

  • Kim, Sun-Lim;Lee, Jae-Eun;Kim, Yul-Ho;Jung, Gun-Ho;Kim, Dea-Wook;Lee, Choon-Ki;Kim, Mi-Jung;Kim, Jung-Tae;Lee, Yu-Young;Hwang, Tae-Young;Lee, Kwang-Sik;Kim, Wook-Han;Kwon, Young-Up;Kim, Hong-Sig;Chung, Ill-Min
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.58 no.2
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    • pp.149-160
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    • 2013
  • The objective of present study was to simultaneously isolate of isoflavone and soyasaponin compounds from the germ of soybean seeds. Soy germ flours were defatted with hexane for 48h at room temperature, and methanolic extracts were prepared using reflux apparatus at $90^{\circ}C$ for 6h, two times. After extraction, extracts were separated with preparative RP-$C_{18}$ packing column ($125{\AA}$, $55-105{\mu}m$, $40{\times}150mm$), and collected 52 fractions were identified with TLC plate (Kieselgel 60 F-254) and HPLC, respectively. Among the identified isoflavone and soyasaponin fractions, isoflavone fractions were re-separated using a recycling HPLC with gel permeation column (Jaigel-W252, $20{\times}500mm$). Final fractions were air-dried, and the purified compounds of two isoflavones (ISF-1-1, ISF-1-2) and four soyasaponins (SAP-1, SAP-2, SAP-3, SAP-4) were obtained. Two isoflavone compounds (ISF-1-1, ISF-1-2) were acid-hydrolyzed for the identification of their aglycones, and confirmed by comparing with 12 types of isoflavone isomers. While the four kinds of soyasaponins were identified by using a micro Q-TOF mass spectrometer in the ESI positive mode with capillary voltage of 4.5kV, and dry temperature of $200^{\circ}C$. Base on the obtained results, it was conclude that ISF-1-1 is the mixture isomers of daidzin (43.4%), glycitin (47.0%), and genistin (9.6%), but ISF-1-2 is the single compound of genistin (99.8% <). On the other hand, soyasaponin SAP-1 is the mixture compounds of soyasaponin A-group (Aa, Ab, Ac, Ae, Af); SAP-2 is soyasaponin B-group (Ba, Bb, Bc) and E-group (Bd, Be); SAP-3 is soyasaponin B-group (Ba, Bb, Bc), E-group (Bd, Be), and DDMP-group (${\beta}g$); SAP-4 is soyasaponin B-group (Ba, Bb, Bc), E-group (Bd, Be), and DDMP-group (${\beta}g$, ${\beta}a$), respectively.

Physicochemical Characteristics of Cultivated Aromatic Rice Germplasm and Comparative Analysis of Flavor Components During Transplanting Time (국내 육성된 향미 품종의이앙시기별 이화학적 특성 및 향기성분 비교 분석)

  • Cho, Jun Hyun;Song, You Chun;Lee, Kwang Sik;Choi, Sik Won;Lee, Mi Ja;Jang, Ki Chang;Kim, Hyun Young;Kang, Hyeon Jung;Park, Ki Do;Seo, Woo Duck
    • Korean Journal of Environmental Agriculture
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    • v.36 no.3
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    • pp.175-183
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    • 2017
  • BACKGROUND:The Aromatic rice which is characterized by the flavor of Nurungji when cooked rice, and consumption is increasing recently. The purpose of this study was to investigate the physicochemical characteristics and aroma components of five aromatic rice cultivars according to transplanting time. METHODS AND RESULTS: Quantitative analysis of protein, fat, fatty acid and essential amino acid for five aroma rice cultivars(Hyangmibyeo 2 ho, Aromi, Mihyang, Aranghyangchal, Heughyang)and transplanting time was analyzed by crude protein analyzer, gas chromatography (GC), liquid chromatography (LC) and viscosity analysis was done by using rapid viscosity analyzer (RVA). The content of 2-acetyl-1-pyrroline (2AP) was determined by gas chromatography mass spectrometer. (GC-MS) As a result, the average protein and lipid contents were 6.5% and 2.4%, respectively. The content of essential amino acid showed the highest content at 104.4mg/g. There was no significant change in normal nutrients during the transplanting time. By RVA, cv.Hyangmibyeo 2 ho showed the highest peak and total setback viscosities and lowest breakdown viscosity in early transplantation. The content of 2AP in flavor varieties and transplanting time was quantitatively analyzed by GC-MS. Among the cultivars, Aromi showed the highest 2AP contents at $66.7{\mu}g/100gin$ normal transplanting time. CONCLUSION: cv.Aromi and Hyangmibyeo 2 ho were excellent physicochemical properties and 2AP components contents amongaromatic rice cultivars tested. Theiroptimaltime to transplant was at the beginning of June in the area of Miryang.

An Investigation of the Sources of Nitrate Contamination in the Kyonggi Province Groundwater by Isotope Ratios Analysis of Nitrogen (질소 동위 원소 분석을 이용한 경기도 지역 지하수 중 질산태 질소 오염원 구명)

  • Yoo, Sun-Ho;Choi, Woo-Jung;Han, Gwang Hyun
    • Korean Journal of Soil Science and Fertilizer
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    • v.32 no.1
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    • pp.47-56
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    • 1999
  • $^{15}N$-Isotope concentrations of groundwater from l4 wells with different land-use types in Kyonggi Province were measured to investigate the nitrate contamination sources. Water samples were collected monthly from January to December 1997 and analyzed for pH. PC, anions (fluoride, chloride, nitrate, sulfate, inorganic phosphate, and bicarbonate), and canons (calcium, magnesium, potassium, and sodium). For the analysis of the $^{15}N/^{14}N$ ratio as ${\delta}^{15}N$, $N_2$ samples were prepared through Kjeldahl-Rittenberg method and were analyzed using an isotope ratio mass spectrometer (VG Optima IRMS). Reproducibility of the method and precision of the IRMS were below 1.0‰ and 0.1‰, respectively. The ionic composition of each groundwater sample was only slightly different according to the land-use type. The nitrate concentrations of groundwater in cropland or livestock farming areas were higher than those in the residential area. The percentages of nitrate to total anions of groundwater samples from the livestock farming area were higher than those of other areas. The ${\delta}^{15}N$ values of ammonium sulfate, urea, groundwater sample in the non-contaminated area, and water from the animal manure septic tank were -2.7, 1.4, 5.5, and 27.2‰, respectively. Based on the ${\delta}^{15}N$ values, the sources of nitrate could be classified as originated from chemical fertilizers with ${\delta}^{15}N$ values below 5% and as from animal manure or municipal waste with ${\delta}^{15}N$ values over 10‰. In most cases, contamination sources investigated from ${\delta}^{15}N$ values of groundwater samples were correlated with the specific sources according to the land-use types. However, some ${\delta}^{15}N$ values did not matched the apparent land-use types, and there were seasonal variations of ${\delta}^{15}N$ values within the same well. These results suggest that the groundwater quality was affected by two or more contamination sources and the contribution of each source to the groundwater quality varied depending on the sampling season.

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Development and Validation of Analytical Method for Determination of Fungicide Spiroxamine Residue in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Spiroxamine의 시험법 개발 및 검증)

  • Park, Shin-Min;Do, Jung-Ah;Lim, Seung-Hee;Yoon, Ji-Hye;Pak, Won-Min;Shin, Hye-Sun;Kuk, Ju-Hee;Chung, Hyung-Wook
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.296-305
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    • 2018
  • Spiroxamine, one of fungicides, is used to control powdery mildew in various crops and black yellow sigatoka in bananas. The major strength of spiroxamine is to control powdery mildew in various crops and bananas yellow sigatoka in bananas. The compound has shown a high level of activity, good persistence and crop tolerance. Besides powdery mildew, good control of rust, net blotch and Rhynchosporium diseases been indicated in cereals, together with a complementary activity against Septoria diseases. In 2017, the maximum residue limit (MRL) of spiroxamine established in Korea. According to Ministry of ood and rug afety) regulations, spiroxamine residues defined only parent compound. Thus, a analytical method is needed to estimate the residue level of the parent compound. The objective of this study was to develop and validate analytical method for spiroxamine in representative agricultural commodities. Samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interfering substances. The analyte were quantified and confirmed liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.0005{\sim}0.1{\mu}g/mL$) for the analyte in blank extract with coefficient of determination ($r^2$) > 0.99. For validation purposes, recovery studies will be carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries 70.6~104.6% with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges in the Codex guidelines (CAC/GL40, 2003) and MFDS guidelines. proposed analytical method be used as an official analytical method in the Republic of Korea.