• 제목/요약/키워드: Analytical Chromatography

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Simple and Robust Measurement of Blood Plasma Lysophospholipids Using Liquid Chromatography Mass Spectrometry

  • Ji, Dong Yoon;Lee, Chang-Wan;Park, Se Hee;Lee, Eun Jig;Lee, Do Yup
    • Mass Spectrometry Letters
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    • 제8권4호
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    • pp.109-113
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    • 2017
  • Single analytical procedure including extraction, liquid chromatography, and mass spectrometric analysis was evaluated for the simultaneous measurement of lysophospholipids (LPLs). LPLs, particularly, lysophosphatidic acids (LPA) and sphingosine 1-phosphate (S1P) are lipid messengers ubiquitously found in various biological matrix. The molecular species mediate important physiological roles in association with many diseases (e.g. cancer, inflammation, and neurodegenerative disease), which emphasize the significance of the simple and reliable analytical method for biomarker discovery and molecular mechanistic understanding. Thus, we developed analytical method mainly focusing on, but not limited by those lipid species S1P and LPA using reverse phase liquid chromatography-tandem mass spectrometry (RPLC-ESI-MS-MS). Extraction method was modified based on Folch method with optimally minimal level of ionization additive (ammonium formate 10 mM and formic acid). Reverse-phase liquid-chromatography was applied for chromatographical separation in combination with negative ionization mode electrospray-coupled Orbitrap mass spectrometry. The method validation was performed on human blood plasma in a non-targeted lipid profiling manner with full-scan MS mode and data-dependent MS/MS. The proposed method presented good inter-assay precision for primary targets, S1P and LPA. Subsequent analysis of other types of LPLs identified a broad range of lysophosphatidylcholines (LPCs) and lysophosphatidyl-ethanolamines (LPEs).

우리나라의 해상유출물질 감식.분석기법 연구 (Introduction of Korea Oil Identification System(KOIS))

  • 이완섭;이상진;김차수;오현정;김한규
    • 해양환경안전학회:학술대회논문집
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    • 해양환경안전학회 2006년도 춘계학술발표회
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    • pp.85-92
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    • 2006
  • 모든 원유(crude oil) 와 연료유(refined petroleum) 는 서로 구별되는 개별 탄화수소 특성을 가지고 있다. 원유의 경우 산지별로 고유한 특성을 지니고 있으며, 연료유의 경우 같은 유종이라 할지라도 그 원료가 되는 원유의 특성, 또는 생산공정, 생산시기 등에서 차이점이 발생하고 생산시기가 동일한 통일유종의 기름이더라도 선박의 연료탱크 내에 남아있는 잔류물과의 혼합 등에 의해 구별될 수 있는 특징을 가지게 된다. 유지문기법(oil fingerprint method)은 이러한 특성을 이용하여 해상유출유의 오염원을 밝히기 위한 감식 분석기법을 말한다. 현재의 유용한 유지문기법으로는 기체크로마토그래피 (GC)를 이용한 포화탄화수소류 방향족탄화수소류 황화합물 패턴분석방법과 적외선분광광도계(IR)를 이용한 적외선스펙트럼 측정방법 그리고 형광분광광도계(FL)를 이용한 방향족탄화수소류 스펙트럽분석방법 둥이 있으며 GC/MS를 이용한 EICs(Extracted Ion Chromatograms) 패턴분석방법이 있다.

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GC/MS를 이용한 뇨 중 환경 에스트로겐들의 동시 프로필 (Profiling of Urinary Environmental Estrogens by Gas Chromatography/Mass Spectrometry)

  • 양윤정;이선화;정봉철
    • 분석과학
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    • 제12권4호
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    • pp.265-272
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    • 1999
  • 에스트로겐처럼 행동하여 호르몬 수용체와 결합하거나 세포의 신호전달 과정에 영향을 미침으로서 내분비계를 교란시킬 수 있는 환경 에스트로겐 19종 (phytoestrogen: 12종, mycoestrogen: 5종, synthetic estrogen: 2종)의 동시 프로필 분석을 시도하였다. Gas Chromatography/Mass Spectrometry (GC/MS)의 selected ion monitoring (SIM) 방법을 기본으로 하였으며, 액체-고체 추출, 효소 기수분해, 액체-액체 추출 그리고 trimethylsilyl (TMS)-ether 형태의 유도체화를 거치는 비교적 간편한 전처리 방법으로 47.6~99.5%의 회수율과 0.66~9.33%, 1.66~16.14%의 within-a-day 및 day-to-day 분석의 RSD 값을 얻었다. 이 방법을 적용하여 정상 성인 여성과 남성의 뇨 시료에 존재하는 대상 물질들의 농도범위를 결정함으로서 환경 에스트로겐의 영향을 평가하는데 기준이 될 수 있는 한국인 정상인 참고치를 설정하였다.

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대기 유기질소화합물의 분석방법 및 농도 (Review on the Analytical Methods and Ambient Concentrations of Organic Nitrogenous Compounds in the Atmosphere)

  • 최나래;김용표
    • 한국대기환경학회지
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    • 제34권1호
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    • pp.120-143
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    • 2018
  • The analytical methods and their ambient levels of organic nitrogenous compounds such as nitrosamines, nitramines (nitroamines), imines, amides and nitro-polycyclic aromatic hydrocarbons (nitro-PAHs) in the atmosphere are summarized and discussed. Sampling for the analysis of organic nitrogenous compounds was mostly conducted using high volume air sampler. The direct liquid extraction (DLE) using sonification and the pressurized liquid extraction (PLE) using the accelerated solvent extraction (ASE) have been frequently employed for the extraction of organic nitrogenous compounds in the atmospheric samples. After extraction, clean-up via filtration and the solid phase extraction (SPE) and concentrations using nitrogen and rotary evaporator have been generally conducted but in some studies the clean-up and concentration steps have been omitted to prevent the loss of analyte and improve the recovery rate of the analytical procedure. Instrumental analysis was mainly carried out using gas chromatography (GC) or the high performance liquid chromatography (HPLC) coupled with the single quadrupole mass spectrometer or tandem mass spectrometer in the electron ionization (EI), positive chemical ionization (PCI) and negative chemical ionization (NCI) mode and analysis sensitivity of nitrosamines and nitramines were higher in NCI mode. Desirable sampling and analysis methods for analyzing particulate organic nitrogenous compounds are suggested.

Establishment of analytical methods for allergenic compounds in mouthwashes and sanitary napkins by ultra-high-performance liquid chromatography with tandem mass spectrometry

  • Hee-Jung Sim;Hee-Jin Jeong;Yeong-In Lee;Yu-Jin Cho;Seung-Hoon Baek;Jong-Hwan Kim
    • 분석과학
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    • 제36권2호
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    • pp.89-98
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    • 2023
  • Analytical methods for detecting atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes were developed using ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). UHPLC-MS/MS conditions were optimized for rapid, sensitive, and simultaneous analysis of the five allergenic compounds. The methods were validated by assessing their specificity, matrix effects, limit of detection (LOD), limit of quantification (LOQ), linearity, accuracy, and precision. Good linearity was achieved with a determination coefficient of ≥0.99. The LOD and LOQ were 2.1-9.8 and 6.4-29.6 ng/g for sanitary napkins and 0.29-0.48 and 0.87-1.45 ng/mL for mouthwashes, respectively. The accuracy and precision were within an acceptable range according to the criteria reported in the European SANTE/11813/2017 guidelines (70-120 % recovery, <20 % relative standard deviation). Therefore, these methods can be used to analyze atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes.

HPLC 분석기를 이용한 펄프용 단풍나무의 펄핑 추출액에 관한 물질수지 (Mass Balance on the Pulping Extracts of Maple Hardwood using High Performance Liquid Chromatography)

  • 엄병환
    • Journal of the Korean Wood Science and Technology
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    • 제36권4호
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    • pp.102-108
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    • 2008
  • 현재 메인 주립대학에서는 펄프용 목재 성분 중 헤미셀룰로오스 추출 기술에 관한 연구개발이 한창 진행 중이다. 펄프의 수율 향상과 용액 회수에 필요한 유기 및 무기물 사용을 줄이고 새로운 바이오 물질 생산에 필요한 도입부 추가 공정이 연구의 핵심이다. 바이오 물질 중 경제적으로 상용 가능한 에탄올 생산(pilot-scale)에 있어 전 처리되지 않은 기질, 전 처리된 기질 및 펄핑 선 추출액의 화학적 성분분석은 아주 중요한 공정이다. HPLC (High Performance Liquid Chromatography)를 이용한 펄프목재 성분분석 결과, H-column으로 분석한 총 물질수지(total analytical mass balance)는 전 처리되지 않은 칩의 경우 100.6%, 전 처리된 목재 칩은 100.3%, 그리고 펄핑 선 추출액은 81.6%의 결과를 보였다. 한편, P-column으로 분석한 결과, 전 처리되지 않은 기질, 전 처리된 기질, 그리고 선 추출액은 각각, 97.8%, 97.4%, 그리고 80.7%로 나타났다. 총 물질수지가 100%를 넘거나 부족한 수치는 분석해석 중 발생한 약간의 오류로 보인다. 펄프-바이오리파이너리(Biorefinery) 공정을 통해 생성된 기질(substrate) 각각의 정확한 성분분석 결과는 에탄올 상용화 공정에 필요한 중요한 자료가 될 것으로 기대한다.

식초의 에탄올 및 초산 함량의 동시분석 (Simultaneous Gas Chromatographic Analysis of Ethanol and Acetic Acid in Vinegar)

  • 윤희남
    • 한국식품과학회지
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    • 제30권6호
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    • pp.1247-1251
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    • 1998
  • 식초의 에탄올과 초산을 동시에 분석하고자 packed column으로 gas chromatographic analysis을 모색하였다. Tenax-GC를 충진물로 사용하여 $2\;m{\times}2\;mm$의 stainless steel column을 제조하고 식초를 여과하여 column에 직접 주입한 결과 내부 표준 물질로 사용한 isopropyl alcohol과 에탄올, 초산이 20분 이내에서 완전히 분리되었으며 정확도가 매우 높은 것으로(P<0.05)나타났다. 19종의 식초를 이용하여 적정방법으로 산도를, packed column GSC로 에탄올과 초산을, HPLC로 초산을, capillary column GLC로 에탄올과 초산을 각각 분석하여 분석치들을 상호 비교하였다.

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Determination of trace bromate in various water samples by direct-injection ion chromatography and UV/Visible detection using post-column reaction with triiodide

  • Kim, Jungrae;Sul, Hyewon;Song, Jung-Min;Kim, Geon-Yoon;Kang, Chang-Hee
    • 분석과학
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    • 제33권1호
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    • pp.42-48
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    • 2020
  • Bromate is a disinfection by-product generated mainly from the oxidation of bromide during the ozonation and disinfection process in order to remove pathogenic microorganism of drinking water, and classified as a possible human carcinogen by International Agency for Research of Cancer (IARC) and World Health Organization (WHO). For the purpose of determining the trace level concentration of bromate, several sensitive techniques are applied mostly based on suppressed conductivity detection and UV/Visible detection after postcolumn reaction (PCR). In this study, the suppressed conductivity detection method and the PCR-UV/Visible detection method through the triiodide reaction were compared to analyze the trace bromate in water samples and estimated for the availability of these analytical methods. In addtion, the state-of-the-art techniques was applied for the determination of trace level bromate in various water matrices, i.e., soft drinking water, hard drinking water, mineral water, swimming pool water, and raw water. In comparison of two analytical methods, it was found that the conductivity detection had the suitable advantage to simultaneously analyze bromate and inorganic anions, however, the bromate might not be precisely quantified due to the matrix effect especially by chloride ion. On the other hand, the trace bromate was analyzed effectively by the method of PCR-UV/Visible detection through triiodide reaction to satisfactorily minimize the matrix interference of chloride ion in various water samples, showing the good linearity and reproducibility. Furthermore, the method detection limit (MDL) and recovery were 0.161 ㎍/L and 101.0-108.1 %, respectively, with a better availability compared to conductivity detection.