• 제목/요약/키워드: MsMu

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GC/MS-SIM에 의한 하수 슬러지중에 포함된 Octylphenol, Nonylphenol, Di-octylphthalate의 정량 (Analysis of Octylphenol, Nonylphenol, Di-octylphthalate in Sewage Sludge by GC/MS-SIM)

  • 김종훈
    • 분석과학
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    • 제12권3호
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    • pp.248-255
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    • 1999
  • 국내 주요 하수 슬러지(Z-1, Z-2시)에서 내분비계 장애물질로 의심 받는 여러 가지 물질 중 octylphenol(OP), nonylphenol(NP), di-octylphthalate(DOP)를 이 염화메탄을 이용하여 Soxhlet 장치로 추출한 후 GC/MS-SIM 방법으로 그들의 함량을 결정하였다. Z-1시 하수 슬러지의 경우 octylphenol, nonylphenol, di-octylphthalate의 함량이 각각 $3.25{\pm}0.07{\mu}g/g$, $1168{\pm}36{\mu}g/g$, $1172{\pm}57{\mu}g/g$이었고, Z-2 하수 슬러지는 octylphenol, nonylphenol, di-octylphthalate가 각각 $0{\mu}g/g$, $10.8{\pm}0.1{\mu}g/g$, $80{\pm}62{\mu}g/g$이 검출되었다. 특히 Z-1하수 슬러지에서 검출된 nonylphenol과 di-octylphthalate의 양은 매우 높은 값으로 생태계로 순환될 경우 매우 위험한 수준으로 평가되었으며, 또한 인간의 건강과 생식능력에 영향을 미칠 것으로 사료된다.

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낙뢰에 의해 방사된 전계와 자계 파형의 파라미터 (Waveform Parameters of the Electric and Magnetic Fields Radiated Form Lightning Return Strokes)

  • 이복희;백영환;이우철
    • 조명전기설비학회논문지
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    • 제20권5호
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    • pp.57-63
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    • 2006
  • 본 논문은 낙뢰에 의해서 방사된 전계와 자계 파형의 물리적 특성과 파라미터분석에 대한 것으로 낙뢰에 의한 전계와 자계 파형은 각각 평판형 전계센서와 루프형 자계센서로 검출되고, 측정된 신호는 12 비트의 해상도, 10[MS/s] 샘플링, 10[ms]의 기록시간을 가지는 데이터취득시스템으로 기록하였다. 낙뢰에 의해 발생한 전계와 자계 파형의 극성의존성은 거의 없었으며, 상승시간은 $13[{\mu}s]$이내이고 정 부극성의 평균값은 각각 $4.1[{\mu}s],\;4.2[{\mu}s]$이었다. 정 부각성의 영점교차시간은 각각 $65.2[{\mu}s],\;67.0[{\mu}s]$이고, 반전딥의 깊이는 38.0[%], 40.3[%]이었다.

LC-MS/MS를 이용한 곽향정기산(藿香正氣散) 추출물 중 20종 성분의 함량분석 (Quantitative Analysis of the Twenty Marker Components in Gwakhyangjeonggi-san using Ultra-Performance Liquid Chromatography with Mass Spectrometer)

  • 서창섭;신현규
    • 생약학회지
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    • 제45권2호
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    • pp.113-120
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    • 2014
  • Generally, Gwakhyangjeonggi-san has been used for treatment of diarrhea-predominant irritable bowel syndrome. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer method was established for the simultaneous quantification of marker compounds 1-20 in Gwakhyangjeonggi-san water extract. All analytes were separated by gradient elution using two mobile phases on a UPLC BEH $C_{18}$ ($100{\times}2.1mm$, $1.7{\mu}m$) column and maintained at $45^{\circ}C$. The injection volume was $2.0{\mu}L$ and the flow rate was 0.3 mL/min with detection at mass spectrometer. Regression equations of the compounds 1-20 were acquired with $r^2$ values ${\geq}0.9950$. The values of limit of detection and quantification of all analytes were 0.01-2.79 ng/mL and 0.03-8.37 ng/mL, respectively. The amounts of the compounds 1-20 in Gwakhyangjeonggi-san water extract were not detected $-3,236.67{\mu}g/g$. The established LC-MS/MS methods will be valuable to improve quality control of traditional herbal formula, Gwakhyangjeonggi-san.

액체크로마토그래프/질량분석기를 이용한 수중 남조독소물질 동시분석법 (Method for Simultaneous Determination of Cyanotoxins in Water by LC-MS/MS)

  • 김정희;윤미애;김학철
    • 한국물환경학회지
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    • 제25권4호
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    • pp.597-605
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    • 2009
  • Algae bloom occurred in reservoir in summer can cause taste and odor in water and disturb the flocculation and sedimentation processes in water treatment plant and cause sand filter plugging. It was also reported that microcystins, anatoxin and saxitoxin released from cyanobacteria had acute toxic effects on liver and nervous system. For these reasons, many advanced countries inclusive of WHO set the guideline for these toxins and cyanotoxins have been managed with regular monitoring in Korea as well. However, complex sample preparation steps such as a solid phase extraction (SPE) and derivatization are required with an existing analysis method with HPLC. We needed to improve an analysis method for low extraction efficiency and long sample preparation time. In this study, we have established a new LC/MS/MS method which can simultaneously determine 6 cyanotoxins (Microcystins-LR, Microcystins-RR, Microcystins-YR, Anatoxin-a, Saxitoxin, Neosaxitoxin) with only simple filtration step. When $75{\mu}L$ filterated sample was injected onto the LC-MS/MS, the recovery ranged from 86% to 112% and the MDL was $0.025{\sim}0.581{\mu}g/L$. We can make the MDL be lower than the guideline ($1{\sim}3{\mu}g/L$) of advanced countries with simple preparation.

Simultaneous Determination of Methylphenidate, Amphetamine and their Metabolites in Urine using Direct Injection Liquid Chromatography-Tandem Mass Spectrometry

  • Kwon, Woonyong;Suh, SungIll;In, Moon Kyo;Kim, Jin Young
    • Mass Spectrometry Letters
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    • 제5권4호
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    • pp.104-109
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    • 2014
  • Nonmedical use of prescription stimulants such as methylphenidate (MPH) and amphetamine (AP) by normal persons has been increased to improve cognitive functions. Due to high potential for their abuse, reliable analytical methods were required to detect these prescription stimulants in biological samples. A direct injection liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed and implemented for simultaneous determination of MPH, AP and their metabolites ritalinic acid (RA) and 4-hydroxyamphetamine (HAP) in human urine. Urine sample was centrifuged and the upper layer ($100{\mu}L$) was mixed with $800{\mu}L$ of distilled water and $100{\mu}L$ of internal standards ($0.2{\mu}g/mL$ in methanol). The mixture was then directly injected into the LC-MS/MS system. The mobile phase was composed of 0.2% formic acid in distilled water (A) and acetonitrile (B). Chromatographic separation was performed by using a Capcell Pak MG-II C18 ($150mm{\times}2.0mm$ i.d., $5{\mu}m$, Shiseido) column and all analytes were eluted within 5 min. Linear least-squares regression with a 1/x weighting factor was used to generate a calibration curve and the assay was linear from 20 to 1500 ng/mL (HAP), 40-3000 ng/mL (AP and RA) and 2-150 ng/mL (MPH). The intra- and inter-day precisions were within 16.4%. The intra- and inter-day accuracies ranged from -15.6% to 10.8%. The limits of detection for all the analytes were less than 4.7 ng/mL. The suitability of the method was examined by analyzing urine samples from drug abusers.

Method for Simultaneous Determination of Anatoxin-a and Microcystins in Korean Water Systems by Using LC/MS/MS

  • Moon, Jeong-Suk;Kim, Hwa-Bin;Park, Hae-Kyung;Lee, Jae-Jung;Park, Jong-Hwan;Lee, Hae-Jin
    • 생태와환경
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    • 제44권1호
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    • pp.22-30
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    • 2011
  • This study was purposed to develop an effective LC/MS/MS method for simultaneously determining five pre-treated cyanotoxins (anatoxin-a, microcystins-RR, -YR, -LR and -LA) of cyanobacteria blooms. Cyanobacterial bloom samples were collected from 11 major lakes and three downstream areas of river around Korea during 2005~2009. Cyanotoxins were identified in 38 samples from the lakes. The validity of the method was evaluated and the recovery rates were found ranging from 83~87%. The MDL turned out to be $0.046\;{\mu}g\;L^{-1}$ for anatoxin-a and $0.066\;{\mu}g\;L^{-1}$ for microcystins (RR, YR, LR and LA), which indicates that the method has high sensitivity and accuracy. The most dominant genus of the cyanobacterial blooms was Microcystis, which accounted for 71% of the analysed samples. Microcystis also contained the largest amount of microcystins ($398.5\;{\mu}g\;gDW^{-1}$) among the analyzed cyanobacteria. The analysis of the five cyanotoxins showed that anatoxin-a ranged between $0{\sim}41.833\;{\mu}g\;gDW^{-1}$ and microcystins ranged between $6.311{\sim}2,148.786\;{\mu}g\;gDW^{-1}$. Among the microcystins, micocystin-RR took up 58.3%, the largest portion. Anatoxin-a was found to account for 77.8% of the samples. This study has its significance in that it allowed the establishment of toxin criteria appropriate for the Korean water systems. Further studies may be necessary to conduct for improving water treatment methods.

HPLC-FLD 및 LC-MS/MS에 의한 식품 중 총아플라톡신 오염실태 조사 (A Survey of Total Aflatoxins in Food Using High Performance Liquid Chromatography-Fluorescence Detector (HPLC-FLD) and Liquid Chromatography Tandem Mass Spectrometry(LC-MS/MS))

  • 장미란;이창희;조성혜;박준식;권은영;이은진;김소희;김대병
    • 한국식품과학회지
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    • 제39권5호
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    • pp.488-493
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    • 2007
  • 국내유통중인 곡류, 견과류 및 그 가공품 총 25품목, 393건의 시료에 대해 immunoaffinity column 정제방법을 이용하여 총아플라톡신 오염실태를 조사하였으며, 그 결과 곡류 및 곡류가공품 6건, 견과류 및 견과류 가공품 37건에서 아플라톡신 오염이 확인되었으며 오염수준은 아플라톡신 $B_1$으로서 $0.04-2.65{\mu}g/kg$, 총아플라톡신으로서 $0.04-5.51{\mu}g/kg$ 범위로 나타났다. Immunoaffinity column 정제를 거쳐 HPLC-FLD로 분석한 결과 아플라톡신이 검출된 시료에 대해서 LC-MS/MS로 확인하였으며, 그 결과 모두 아플라톡신으로 확인되었다. 본 연구결과에서 나타난 곡류 및 견과류에 대한 아플라톡신 검출빈도 및 오염수준은 국내, 외 연구 결과와 유사하거나 비교적 낮게 나타났으며 국내 아플라톡신 기준 및 미국, CODEX에서 설정된 기준규격 이하로 검출되었다.

In vitro propagation of Bambusa nutans Wall. ex Munro through axillary shoot proliferation

  • Negi, Divya;Saxena, Sanjay
    • Plant Biotechnology Reports
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    • 제5권1호
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    • pp.35-43
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    • 2011
  • This communication describes for the first time an efficient and reproducible protocol for large-scale multiplication of Bambusa nutans. Nodal segments collected from field-grown clumps and cultured on Murashige and Skoog (MS) medium supplemented with $4.4{\mu}M$ benzylaminopurine (BA) and $2.32{\mu}M$ kinetin (Kin) gelled with 0.2% gelrite yielded 80% aseptic cultures with 100% bud-break. The in vitro-formed shoots obtained after bud-break were successfully multiplied in MS liquid medium supplemented with $13.2{\mu}M$ BA, $2.32{\mu}M$ Kin, and $0.98{\mu}M$ indole-3-butyric acid (IBA). Sub-culturing of shoots every 3 weeks on fresh multiplication medium yielded a consistent proliferation rate of 3.5-fold. Shoot clusters containing three to five shoots were successfully rooted with 100% success on half-strength MS liquid medium supplemented with $9.8{\mu}M$ IBA, $2.85{\mu}M$ indole-3-acetic acid (IAA), $2.68{\mu}M$ naphthaleneacetic acid (NAA), and 3% sucrose. Plantlets grown in vitro were acclimatized and subsequently transferred to the field. Inter-simple sequence repeat analysis has confirmed the genetic uniformity of the tissue-cultured plants up to 27 passages.

ICP/MS를 이용한 축산물의 유해중금속 분석방법 및 숙련도 검증 (Method and proficiency test for analysis of toxic metals in livestock products by ICP/MS)

  • 장정희;김동규;권현정;임채미;손성완;김미경
    • 대한수의학회지
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    • 제52권2호
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    • pp.69-74
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    • 2012
  • The analytical method of trace toxic metals in livestock products was confirmed and validated through certified reference material (CRM) and the international proficiency tests. There are some difficulties to determine low levels of toxic metals in livestock products because of interferences due to the matrix. The recoveries of CRM (NIST 1577c) ranged from 73.9 to 119% for lead and from 86.4 to 111% for cadmium in bovine liver. The international proficiency tests were carried out with the milk powder and cocoa powder samples including metals provided by Food Analysis Performance Assessment Scheme (FAPAS$^{(R)}$, UK). The test samples were prepared by microwave digestion using solution of $HNO_3:H_2O_2:H_2O$ (v/v/v = 5 : 2 : 4) and analyzed by ICP/MS. The analytical result of cadmium in milk powder was $121{\mu}g/kg$ with -0.3 of the z-score compared to the assigned value of $131{\mu}g/kg$ by FAPAS$^{(R)}$. The analytical results of lead and cadmium in cocoa powder were $29.2{\mu}g/kg$ and $97.6{\mu}g/kg$, respectively, which satisfied the assigned values of $34.2{\mu}g/kg$ for lead and $126{\mu}g/kg$ for cadmium by FAPAS$^{(R)}$. It is verified that the analytical method is accurate and reliable to determine trace lead and cadmium in livestock products by microwave digestion and ICP/MS.

SPME/GC-MS를 이용한 혈액중의 호모시스테인, 메치오닌 및 시스테인의 분석 (Determination of Homocysteine, Methionine, Cysteine in Human Plasma with SPME/GC-MS)

  • 유은아;김정수;명승운
    • 분석과학
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    • 제13권6호
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    • pp.736-742
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    • 2000
  • SPME/GC-MS 방법을 이용하여 호모시스테인, 메치오닌 및 시스테인의 혈액중의 함량을 측정하고 관상동맥질환과 호모시스테인의 함량과의 관계를 조사하였다. 혈액중의 호모시스테인, 메치오닌 및 시스테인은 관상동맥질환의 위해성에 대한 생체표식인자로 알려지고 있다. 관상동맥질환자들에 대한 이들의 함량분포는 호모시스테인의 경우 $18.47-33.38{\mu}mol/L$,메치오닌피 경우는 $30.16-55.72{\mu}mol/L$ 그리고 시스테인의 경우는 $183.16-387.32{\mu}mol/L$ 범위의 함량을 보였다. 이 방법은 시간과 노력이 절약되고 또한 용매의 제한 사용으로 훨씬 환경 친화적인 방법임을 시사하였다.

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