• Title/Summary/Keyword: MS-10

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The analysis of pharmaceuticals in drinking water by HPLC/ESI-MS/MS (HPLC/ESI-MS/MS에 의한 먹는물(정수) 중 의약물질의 분석)

  • Park, Mi-Sun;Kim, Byung-Joo;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.23 no.5
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    • pp.457-464
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    • 2010
  • The analytical method of four pharmaceuticals (virginiamycin, erythromycin, tylosin and cimetidine) in drinking water was developed. Effective simultaneous sample clean-up and extraction by solid-phase extraction (SPE) using HLB cartridge prior to LC/ESI-MS/MS analysis were performed. A linear correlation observed in the calibration curves for drinking water in the range of 0.01~2.0 ng/mL showed above $r^2$=0.995. Absolute recovery was in the range of 64.7~118.1% (except cimetidine (37.7~48.1%)). Limit of detection (LOD) and limit of quantitation (LOQ) in spiked drinking water matrix were in the range of 1.6~74.8 pg/mL and 5.5~249.7 pg/mL, respectively. The established method can be used to determine low pg/mL levels of pharmaceuticals in the drinking water.

Determination of 105 pesticide residues by GC/MS/MS (GC/MS/MS를 이용한 105종의 잔류농약 분석에 관한 연구)

  • Kim, W.S.;Do, J.A.;Lee, H.J.;Lee, J.Y.;Yang, S.J.;Lee, S.H.
    • Analytical Science and Technology
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    • v.23 no.4
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    • pp.395-404
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    • 2010
  • A multi-residual method using gas chromatography coupled with mass spectrometry (GC/MS/ MS) was developed for the analysis of 105 pesticides. This method was tested on lemons, beans and other vegetables. The pretreatment of these pesticides was performed by liquid-liquid partition followed by cleanup with solid phase extraction cartridge (SPE Florisil), after acetonitrile extraction from matrices and sodium chloride (15 g) addition. The recovery ranged from 71.1% to 126.0% except for azinphosmethyl, famoxadone, fenamidone, flufenoxuron and triadimefon in lemons and from 72.5% to 124.5% in bean. In lemon, the limit of detection (LOD) and limit of quantification (LOQ) were 0.001~150 ng/ mL and 0.004~500 ng/mL, respectively.

Simultaneous analysis and occurrences of six pharmaceuticals in surface water by LC/ESI-MS/MS (LC/ESI-MS/MS를 이용한 하천수 중 잔류 6종 의약물질의 동시분석 및 모니터링)

  • Kim, Byung-Ju;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.572-578
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    • 2010
  • The extraction/clean-up and concentrating of pharmaceuticals from surface water were performed by HLB (Hydrophilic-Lipophilic Balanced) cartridge. The method allows for the simultaneous determination of six pharmaceuticals by HPLC/ESI(+)-MS/MS. Recoveries of the pharmaceutical were between 71.1 to 92.6% (except fenbendazole) and the overall variability of the method was below 11.2% (RSD). The calibration curves for the pharmaceuticals from blank surface water showed good linearities (above $r^2$ = 0.99) in the concentration range of 0.007~1.2 ng/mL. The limit of detection (LOD) and the limit of quantification (LOQ) were 7.2~128.7 pg/mL and 23.8~429.1 pg/mL, respectively. The present analytical method can be useful for monitoring residual pharmaceuticals in surface water and other aquatic samples. High concentrations of iopromide and fenbendazole were detected in a few samples of surface water.

Quercetin Glucoside Profiling of Fresh Onion (Allium cepa) and Aged Black Onion Using HPLC-ESI/MS/MS (HPLC-ESI/MS/MS를 이용한 생양파와 흑양파의 퀘세틴 배당체 분석)

  • Chung, Dong-Min;Kwon, Sun-Hwa;Chung, Young-Chul;Chun, Hyo-Kon
    • Journal of Life Science
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    • v.21 no.3
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    • pp.464-467
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    • 2011
  • Quercetin is a major flavonoid present in onions, which acts as an antioxidant. Quercetin exists both as a free compound and conjugated with carbohydrates, primarily as glucosides in onion. Aged black onion was made through a 30 day aging process in which the onions were kept in an environment of $60^{\circ}C$ and high humidity (90% RH). Quercetin and quercetin glucosides were assayed in onion bulbs before and after the aging process, using high performance liquid chromatography-electrospray ion trap mass spectrometry (HPLC-ESI/MS/MS). Quercetin mono- and diglucosides were identified in fresh onion bulbs, whereas quercetin aglycone was the only form present in aged black onion bulbs. These findings indicate that the quercetin mono- and di-glucosides present in fresh onions undergo complete deglycosylation during the aging process. Such profiling will provide a rapid method that can be used to assess changes in the two major quercetin glycosides during the aging process of onion bulbs.

Improvement of DS System using Transversal Filter for Advanced Duty Rate on Meteor Burst Channel (유성 버스트 채널 도통율 향상을 위해 Transversal Filter를 적용한 DS시스템의 개선)

  • Kwon Hyeog-Soong
    • The Journal of Korean Institute of Communications and Information Sciences
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    • v.31 no.6A
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    • pp.627-633
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    • 2006
  • In spite of many advantages of Meteor Burst Communications(MBC) on its transmission channel, the fact that its duty rate is less than 10 percents is a considerable deficiency of MBC. To overcome with this deficiency without paying large cost, we use a direct sequence(DS) simple reception system. This method doesn't need to add the components for acquisition or tracking the signal so that it keeps the cost efficiency of the MBC. But it has a disadvantage that its duty rate shows a large decline by noise. For this problem we adopt the proposed system applying a transversal filter circuit. The improvement by this method is more significant when the received signal is weak Simulation results show as t1 is 100ms, then the burst length would be increased by 35% when the initial value of the received signal power increases by 3 dB, t2 is 135ms. If the power increases by 6dB the burst length would be 170ms thus increased by 70%, which shows a great enhancement. Suppose now that t1 is 50ms and the power is increased by 3dB, then t2 would be increased by 70% to 85ms, and increasing the power by 6dB it would be increased by 130% to 115ms.

Development of Isotope Dilution-Liquid Chromatography/Tandem Mass Spectrometry as a Candidate Reference Method for the Determination of Acrylamide in Potato Chips

  • Park, Sun-Young;Kim, Byung-Joo;So, Hun-Young;Kim, Yeong-Joon;Kim, Jeong-Kwon
    • Bulletin of the Korean Chemical Society
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    • v.28 no.5
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    • pp.737-744
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    • 2007
  • An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of acrylamide in potato chips, starch-rich foodstuff cooked at high temperature. Sample was spiked with 13C3-acrylamide and then extracted with water. The extract was further cleaned up with an Oasis HLB solid-phase extraction (SPE) cartridge and an Oasis mixed-phase cation exchange (MCX) SPE cartridge. The extract was analyzed by using LC/ESI/Tandem MS in positive ion mode. LC with a medium reversed-phase (C4) column was optimized to obtain adequate chromatographic retention and separation of acrylamide. MS was operated to selectively monitor [M+H]+ ions of the analyte and its isotope analogue at m/z 72 and m/z 75, respectively. Sample was also analyzed by the LC/MS with selectively monitoring the collisionally induced dissociation channels of m/z 72 → m/z 55 and m/z 75 → 58. Compared to the LC/MS chromatograms, the LC/MS/MS chromatograms showed substantially reduced background chemical noises coming from solvent clusters formed during ESI spray processes and interferences from sample matrix. Repeatability and reproducibility studies showed that the LC/MS/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0% while the LC/MS results are influenced by chemical interferences.

Analysis of Phoxim Residue in Animal Food Production (Cattle and Pig) by LC/ESI-MS/MS (LC/ESI-MS/MS를 이용한 식육(소, 돼지)중 잔류 phoxim 분석)

  • Park, Mi-Sun;Lee, Jin-Joo;Myung, Seung-Woon
    • Journal of the Korean Chemical Society
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    • v.55 no.4
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    • pp.626-632
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    • 2011
  • Phoxim, which is one of veterinary drugs, is a well-known antiparasitic agent in wide use. In this paper, phoxim was extracted from cattle and pig tissue using solid-phase extraction (SPE) employing a silica cartridge with acetonitrile. Liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) for the analysis of phoxim from animal tissue was presented. Phoxim was detected on a $C_{18}$ column ($2.1{\times}100\;mm$, $3.5\;{\mu}m$) using a mobile phase of 0.1% formic acid in water and acetonitrile. A linear correlation observed in the calibration curves for cattle (0.0048~2.0 mg/kg) and pig (0.0055~2.0 mg/kg) showed above $r^2$=0.995. Accuracy measured at concentrations ranging from 0.0048 to 0.2 mg/kg was the range of 68.2~106.9%. Limit of detection (LOD) and limit of quantitation (LOQ) were the range of 0.0014~0.0017 mg/kg and 0.0048~0.0055 mg/kg, respectively. The precision (RSD%) was below 11.2%.

Improved Data Concealing and Detecting Methods for OOXML Document (OOXML 문서에 대한 향상된 데이터 은닉 및 탐지 방법)

  • Hong, Kiwon;Cho, Jaehyung;Kim, Soram;Kim, Jongsung
    • Journal of the Korea Institute of Information Security & Cryptology
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    • v.27 no.3
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    • pp.489-499
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    • 2017
  • MS office is a office software which is widely used in the world. The OOXML format has been applied to the document structure from MS office 2007 to the newest version. In this regard, the method of data concealing, which is a representative anti-forensic act has been researched and developed, so the method of detecting concealed data is very important to the digital forensic investigation. In this paper, we present an improved data concealing method bypassing the previewers detecting methods for OOXML formatted MS office documents. In addition, we show concealment of the internal data like sheets and slides for MS office 2013 Excel and PowerPoint, and suggest an improved detecting algorithm against this data concealing.

Sensitive Determination of Pinaverium Bromide in Human Plasma by LC-ESI-MS/MS : Applicability to Oral Bioavailability Determination (LC-ESI-MS/MS를 이용한 생체시료 중 브롬화피나베리움의 고감도 분석 및 이를 이용한 생체이용률 평가)

  • Park, Seok;Lee, Ye-Rie;Kim, Ho-Hyun;Lee, Hee-Joo;Kim, Yoon-Gyoon;Youm, Jeong-Rok;Han, Sang-Beom
    • Journal of Pharmaceutical Investigation
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    • v.34 no.6
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    • pp.513-519
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    • 2004
  • A sensitive method for quantification of pinaverium bromide in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS/MS). Glimepiride was used as internal standard. Pinaverium bromide and internal standard in plasma sample were extracted using tert-butylmethylether(TBME). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of acetonitrile-5 mM ammonium formate (80/20, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS with multiple reaction monitoring (MRM) mode, pinaverium and glimepirde were detected without severe interference from human plasma matrix. Pinaverium produced a protonated precursor ion $([M+H]^+)$ at m/z 510.3 and a corresponding product ion at m/z 228.9. Internal standard produced a protonated precursor ion $([M+H]^+)$ at m/z 491.5 and a corresponding product ion at m/z 352.0. Detection of pinaverium bromide in human plasma was accurate and precise, with limit of quantitation at 0.5 ng/ml. The method has been successfully applied to bioavailability study of pinaverium bromide tablet in Korean healthy male volunteers. Pharmacokinetic parameters such as $AUC_t,\;C_{max},\;T_{max},\;K_{el}\;and\;t_{1/2}$ were calculated.

A Study on Edit Order of Text Cells on the MS Excel Files (MS 엑셀 파일의 텍스트 셀 입력 순서에 관한 연구)

  • Lee, Yoonmi;Chung, Hyunji;Lee, Sangjin
    • Journal of the Korea Institute of Information Security & Cryptology
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    • v.24 no.2
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    • pp.319-325
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    • 2014
  • Since smart phones or tablet PCs have been widely used recently, the users can create and edit documents anywhere in real time. If the input and edit flows of documents can be traced, it can be used as evidence in digital forensic investigation. The typical document application is the MS(Microsoft) Office. As the MS Office applications consist of two file formats that Compound Document File Format which had been used from version 97 to 2003 and OOXML(Office Open XML) File Format which has been used from version 2007 to now. The studies on MS Office files were for making a decision whether the file has been tampered or not through detection of concealed items or analysis of documents properties so far. This paper analyzed the input order of text cells on MS Excel files and shows how to figure out what cell is the last edited in digital forensic perspective.