• Title/Summary/Keyword: Selected ion monitoring

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Determination of bisphenol-A using GC/MS in Can Materials (기체크로마토그래피/질량분석법을 이용한 캔 물질에서의 bisphenol-A 분석)

  • Kim, Ki-Cheol;Kim, Yang-Hee;Choi, Ok-Kyung;Ko, Hoan-Uck;Yim, Jun-Rae;Choi, Kyo-Hong;Cho, Hyun-Woo;Kim, Hye-Young;Kim, Myungsoo;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.14 no.6
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    • pp.499-503
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    • 2001
  • A new simple, rapid and sensitive gas chromatographic technique for the determination of bisphenol-A in can materials, which is the major material of epoxy resin and polycarbonate polymer, is proposed. This method is characterised by derivatization of the bisphenol-A with a acylating reagent forming the acetate derivative to optimize the chromatographic property. The detection of bisphenol-A is performed based on GC/MS (gas chromatography/mass spectrometry). Several beverages were analyzed by the proposed method for the determination of bisphenol-A Bisphenol-A was assayed the range of $0.11{\sim}11.40{\mu}g/can$ from the can materials.

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Analytical Determination of Alkylphenols, Chlorophenols and Bisphenol A in Biota Samples using Gas Chromatography/Mass Spectrometry (기체 크로마토그래피/질량분석기를 이용한 생물시료 중 알킬 페놀류, 클로로페놀류 및 비스페놀 A의 분석법)

  • Hong, Jongki;Kim, Hyup;Baek, In-Girl;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Chung, Bong-Chul;Pyo, Hee-Soo;Kim, Kyung-Rae;Kim, Yong-Hwa
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.484-493
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    • 2000
  • The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

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Determination of Polybrominated Diphenyl Ethers(PBDEs) in Soil using Gas Chromatography/Isotope Dilution Mass Spectrometry (기체크로마토그래피/동위원소 희석 질량분석법을 이용한 토양 중 폴리브롬화 디페닐에테르의 분석법)

  • Na, Yuncheol;Chang, Yoon-Seok;Kim, Hai-Dong;Hong, Jongki
    • Analytical Science and Technology
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    • v.17 no.1
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    • pp.29-36
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    • 2004
  • An analytical method of polybrominated diphenyl ethers in soil samples by isotope dilution method using gas chromatography/mass spectrometry (GC/MS)-selected ion monitoring (SIM) was described. PBDEs in soil were extracted with soxhlet extractor and then silica and florisil solid phase extraction (SPE) methods as purification of extract were compared. After clean-up, the extractions were analyzed by GC/MS with SIM mode. Quantitation was performed isotope dilution method using four $^{13}C$ isotopically labeled PBDEs as internal standards. This developed method was validated for eight congeners of PBDEs in the concentration range 0.04~4 ng/g in soil and the average recovery of the analytes ranged 30.8~110.8% for florisil and 44.4~110.7% for silica, respectively. The method detection limits of PBDEs were 0.04~0.3 ng/g.

Ultra-fast Generic LC-MS/MS Method for High-Throughput Quantification in Drug Discovery

  • Kim, So-Hee;Yoo, Hye Hyun;Cha, Eun-Ju;Jeong, Eun Sook;Kim, Ho Jun;Kim, Dong Hyun;Lee, Jaeick
    • Mass Spectrometry Letters
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    • v.4 no.3
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    • pp.47-50
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    • 2013
  • An ultra-fast generic LC-MS/MS method was developed for high-throughput quantification of discovery pharmacokinetic (PK) samples and its reliability was verified. The method involves a simple protein precipitation for sample preparation and the analysis by ultra-fast generic LC-MS/MS with the ballistic gradient program and selected reaction monitoring (SRM) mode. Approximately 290 new chemical entities (NCEs) (over 10,000 samples) from 5 therapeutic programs were analyzed. The calibration curves showed good linearity in the concentration range of 1, 2 or 5 to 2000 ng/mL. No significant ion suppression was observed in the elution region of all the NCEs. When approximately 300 plasma samples were continuously analyzed, the peak area of internal standard was constant and reproducible. In the repeated analysis of samples, the plasma concentrations and the area under the curve (AUC) were consistent with the results from the first analysis. These results showed that the present ultra-fast generic LC-MS/MS method is reliable in terms of selectivity, sensitivity, and reproducibility and could be useful for high-throughput quantification and other bioanalysis in drug discovery.

Planting Conditions of Korean Cannabis Derived from Stable Isotope Ratio & Tetrahydrocannabinol Contents (안정동위원소 비율 및 테트라하이드로칸나비놀 함량 분석을 통한 한국산 대마의 재배 환경 추론)

  • Lee, Jae-Sin;Park, Yong-Hoon;Rhee, Jong-Sook;Jeong, Jin-Il;Lim, Mi-Ae;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.52 no.3
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    • pp.172-175
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    • 2008
  • Stable isotope ratio of carbon and nitrogen ($\delta^{13}C$ & $\delta^{15}N$), and $\Delta^{9}$-tetrahydrocannabinol (THC) contents were measured on 37 Korean cannabis and 10 commercial grade marijuana seized in Korea. Factors influencing on the measured values and their variations were investigated. $\delta^{13}C$ value of cannabis is specified mainly by water availability. Korean cannabis showed relatively low $\delta^{13}C$ values ranging -33.29$\sim$-27.01% (mean=-31.01%), which reflect geographic conditions of Korea where is rainy, especially during summer. $\delta^{15}N$ values, which reflect individual planting conditions, were relatively high up to -0.5$\sim$18.0% (mean=6.44%). It reflects characteristics of Korean cannabis growing wild in forest or cultivated in fertile soil. Tetrahydrocannabinol is the major hallucinogenic compound of cannabis. Ethanol extracts of cannabis leaves were derivatized by N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA), and the derivatives were analyzed by GC-MS in selected ion monitoring (SIM) mode. THC contents of Korean cannabis ranged 0.11$\sim$4.34% (mean=1.47%), which were relatively low compared with commercial grade marijuana.

COMS Electrical Power Subsystem Preliminary Design (통신해양기상위성 전력계 예비설계)

  • Gu, Ja-Chun;Kim, Ui-Chan
    • Journal of Satellite, Information and Communications
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    • v.1 no.2
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    • pp.95-100
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    • 2006
  • The COMS(Communication, Ocean and Meteorological Satellite) EPS(Electrical Power Subsystem) is derived from an enhanced Eurostar 3000 version. Eurostar 3000 EpS is fully autonomous operation in nominal conditions or in the event of a failure and provides a high level of reconfigure capability. This paper introduces the COMS EPS preliminary design result. COMS EPS consists of a battery, a solar arrat wing, a PSR(Power Supply Regulator), a PRU(Pyrotechnic Unit), a SDAM(Solar Array Drive Mechanism) and relay and fuse brackets. COMS EPS can offer a bus power capability of 3 kW. The solar array is made of a deployable wing with two panels. One type fo solar cells is selected ad GaAs/Ge triple junction cells. Li-ion battery is base lined with ten series cell module of five cells in parallel. PSR associated to battery and solar array wing generates a power bus fully regulated at 50 V. Power bus os centralized protection and distribution by relay and fuse brackets. PRU provides power for firing actuarors devices. The solar array wing is rotated by the SADM under control of the attitude orbit control subsystem. The control and monitoring of the EPS, especially of the battery, is performed by the PSR in combination with the on-board software.

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Evaluation of Denitrification Efficiency and Functional Gene Change According to Carbon(Fumarate) Concentration and Addition of Nitrate Contaminated-soil in Batch System (회분식반응조 실험을 통한 탄소원(Fumarate) 주입조건에 따른 지하수 중 탈질율 및 탈질 관련 기능성 유전자 분석)

  • Park, Sunhwa;Kim, Hyun-Koo;Kim, Moon-su;Lee, Gyeong-Mi;Jeon, Sang-Ho;Song, Dahee;Kim, Deok-hyun;Kim, Young;Kim, Tae-seung
    • Journal of Soil and Groundwater Environment
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    • v.20 no.7
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    • pp.80-89
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    • 2015
  • Nitrate is on the most seriou pollutant encountered in shallow groundwater aquifer in agricultural area. There are various remediation technologies such as ion exchange, reverse osmosis, and biological denitrification to recover from nitrate contamination. Biological denitrification by indigenous microorganism of the technologies has been reviewed and applied on nitrate contaminated groundwater. In this work, we selected the site where the annual nitrate (NO3) concentration is over 105 mg/L and evaluated denitrification process with sampled soil and groundwater from 3 monitoring wells (MW4, 5, 6). In the results, the nitrate degradation rate in each well (MW 4, 5, and 6) was 25 NO3 mg/L/day, 6 NO3 mg/L/day, and 3.4 NO3 mg/L/day, respectively. Nitrate degradation rate was higher in batch system treated with 2 times higher fumarate as carbon source than control batch system (0.42M fumrate/1M NO3), comparing with batch system with soil sample. This result indicates that increase of carbon source is more efficient to enhance denitrification rate than addition of soil sample to increase microbial dynamics. In this work, we also confirmed that monitoring method of functional genes (nirK and nosZ) involved in denitrification process can be applied to evaluated denitrifcation process possibility before application of field process such as in-situ denitrification by push-pull test.

The study on the measurement of formaldehyde in saliva and urine by GC-MS (가스크로마토그래프-질량분석기에 의한 타액 및 뇨 중 포름알데하이드 분석법 연구)

  • Shin, Ho-Sang;Ahn, Hye-Sil
    • Analytical Science and Technology
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    • v.19 no.2
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    • pp.149-154
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    • 2006
  • A gas chromatography-mass spectrometric method was developed for the determination of formaldehyde in urine and saliva. In a 20 mL glass tube, 0.2 mL of urine or saliva was taken. Further, 1.8 mL of 0.1 M HCl, 0.1 mL of 2,000 mg/L 2,4-dinitrophenyl hydrazine and $20{\mu}l$ of 500 mg/L acetone-$d_6$ as internal standard were added in the tube and sealed tightly with cap. The solution was shaken for 20 min at room temperature and extracted using 4 mL of toluene. The extract was concentrated and redissolved with $100{\mu}l$ of acetonitrile, and then measured by gas chromatography-mass spectrometer (selected ion monitoring). The detection limit was 2.0 ng/mL and 0.5 ng/mL in saliva and urine, respectively. The calibration curves showed good linearity with r = 0.997 and 0.998 for saliva and urine, respectively. The method was used to analyze formaldehyde in rat urine after oral exposure. The developed method may be use ful to the monitoring for formaldehyde exposure in human.

Determination of Quintozene Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Quintozene의 잔류분석)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.195-203
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    • 2015
  • Quintozene, pentachloronitrobenzene (PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930's as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea on 1969. However, now it was banned to use due to its high residue levels in selected harvest products. Also, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of quintozene in agricultural commodities.

Analysis of 1,3-dichloro-2-propanol and 3-chloro-1,2-propanediol by Solid Phase Extraction (고체상 추출에 의한 1,3-dichloro-2-propanol과 3-chloro-1,2-propanediol의 분석)

  • Chae, Hee-Jeong;In, Man-Jin;Kim, Min-Hong;Han, Keum-Soo
    • Korean Journal of Food Science and Technology
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    • v.29 no.1
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    • pp.183-187
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    • 1997
  • The analytical conditions of 1,3-dichloro-2-propanol (DCP) and 3-chloro-1,2-propanediol (MCPD) by solid phase extraction were optimized to improve recovery. Selected-ion monitoring technique which was used for GC-MS analysis of both compounds gave substantially higher sensitivity. The detection limits of DCP and MCPD were 25 and 50 ppb, respectively. The effects of extraction column type, elution solvent and salt concentration on recovery were examined. A normal phase column was better than a reverse phase column in solid phase extraction of DCP and MCPD. It was explained in terms of polarity relationship of solvent-solute-solid phase. A maximum recovery was obtained at the salt concentration of 20% (w/v). Water-immiscible and chloropropanol-soluble solvents such as chloroform, diethyl ether, hexane and ethyl acetate were tested for elution solvent. Hexane and ethyl acetate were the most suitable solvents for the extraction of DCP and MCPD, respectively. High recovery better than 95% was obtained with the selected solvents.

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