• 제목/요약/키워드: Column-switching technique

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$\mu$-HPLC의 Column-Switching 기술을 이용한 식품중 비타민 $B_{12}$의 분석 (Determination of Vitamin $B_{12}$ in Foods Using Column-Switching Technique in $\mu$-HPLC)

  • 박성진;김혜경;함태식;김병용
    • 한국식품영양과학회지
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    • 제28권6호
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    • pp.1208-1211
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    • 1999
  • Semi HPLC using a column switching technique was used to determine the trace content of vitamin B12 in various foods. Total analytical time required less than 20 mins per sample and the recovery ratio was 99.9, 99.6, 100.1 and 99.8% for 1.0, 10.0, 100.0 and 1,000 g/kg, respectively. The content of vitamin B12 in various foods obtained using column switching method showed higher levels compared to labels in dried milk(0.5 g/100g) and in grain products(0.51~34.36 g/100g). Thus, this column switching method was more sensitive, effective and precise than the microbiological analysis currently used to determine the trace compounds like a vitamin B12.

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On-line Trace Enrichment for the Determination of Insulin in Biological Samples Using Reversed-Phase High Performance Liquid Chromatography with Column Switching

  • Lee, Jung-Sook;Lee, Heeyong;Lee, Hye-Suk;Lee, Kang-Choon
    • Archives of Pharmacal Research
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    • 제17권5호
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    • pp.360-363
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    • 1994
  • Column--swtiching technique with a reversed-phase high performance liquid chromatographic method has been developed for the routine analysis of radioiodinated insulin and its degadation products in biological fluids. The diluted biological samples were loaded onto a precolumn packed with LiChrosorb RP-8 $(25-40{\;}{\mu}m)$ using 0.1% trifuoroacetic acid (TFA) in water as a washing solvent. After valve switching, the concentrated insulins were eluted in the back-flush mode and separated by a W-Porex $C_{18}$ column with a gradient of 0.1% TFA in water and 0.1% TFA in acetonitrile as the mobile phase. The method showed good precision, accuracy and speed with the detection limit of 20 pg/ml. Total analysis time per sample was about 40 min and the coefficients of variation were less than 8, 2%.

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Simple and Sensitive Determination of Baclofen in Human Plasma by Column-Switching and Semi-Micro High-Performance Liquid Chromatography

  • Ban, Eun-Mi;Ko, Hye-Ran;Kim, Chong-Kook
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.284.2-284.2
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    • 2003
  • Using a column-switching technique. highly sensitive and selective semi-micro high-performance liquid chromatographic (HPLC) method has been developed for the determination of baclofen in human plasma. Following precipitation of plasma sample containing baclofen with zinc sulfate-acetonitrile, samples were directly injected on to the system. (omitted)

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Determination of Vitamin B12 (Cyanocobalamin) in Fortified Foods by HPLC

  • Park, Youn-Ju;Jang, Jae-Hee;Park, Hye-Kyung;Koo, Yong-Eui;Hwang, In-Kyeong;Kim, Dai-Byung
    • Preventive Nutrition and Food Science
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    • 제8권4호
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    • pp.301-305
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    • 2003
  • This study was conducted to develop an HPLC method for determining vitamin B$_{12}$ in fortified foods which has typically been determined by microbiological assays according to AOAC and Korean Food Code approved methods. Vitamin B$_{12}$ (cyanocobalamin) was determined by reversed-phase HPLC with a triple column and UV/VIS dectector (550 nm) using the column switching technique after extraction with 5 mM potassium phosphate solution by sonication without a clean-up procedure. The recovery of spiked samples and limit of detection (LOD) by HPLC were 78.6 ∼107.5 % and 2 ppb ($\mu\textrm{g}$/kg), respectively. The LOD of the microbiological assay (MBA) was much lower than that of HPLC. The concentrations of vitamin B$_{12}$ analyzed in all tested samples (n=12) confirmed compliance with declared label claims. The range of recovery ratio by the HPLC method when compared to the microbiological assay was 76.2 ∼140.0 %. There was not significant difference between the HPLC and MBA methods (p < 0.01) with r=0.9791 and linear regression y=0.9923x-0.04. The HPLC method for determining vitamin B$_{12}$ using the column-switching technique appears to be suitable for determining vitamin B$_{12}$ concentrations above 1 $\mu\textrm{g}$/100 g in fortified foods.ied foods.

Micro-HPLC를 이용한 조제분유 중 비타민 A.E 동시분석법 개발 (Development of simultaneous determination of vitamin A and E in infant formula by micro-HPLC)

  • 윤이란;최유정;이민권;정명호;김병훈
    • 한국동물위생학회지
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    • 제29권3호
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    • pp.339-346
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    • 2006
  • Semi-micro-HPLC using a column-switching technique was developed for simultaneous determination of vitamin A and E contents in infant formula. Vitamin A and E were extracted by PDA - HPLC with reversed phase column using organic solvent and their contents in Certified Reference Material (CRM) and infant formula were determined and compared with hydrolysis method and rapid extraction. Developed method has many advantages of simple and rapid sample preparation and simultaneous determination of vitamin A and E by micro-HPLC using reversed phase column.

후세척-이온크로마토그래피를 이용한 형석 광산 폐수 중 플루오라이드 정량 (Determination of fluoride in fluorite mine wastewater by ion chromatography with post-wash technique)

  • 송경선;음철헌;김상연
    • 분석과학
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    • 제19권5호
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    • pp.383-388
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    • 2006
  • 간단한 후세척의 이온 크로마토그래피를 이용하여 형석 광화대 지역의 광산 폐수에서 플루오라이드 이온을 빠르고 정확하게 정량하는 방법을 확립하였다. 시료중의 높은 농도의 황산 이온은 전치 컬럼(pre-column)에 머물러있고 머무름 시간이 적은 플루오라이드 이온은 제시된 이온 크로마토그래프 시스템과 스위칭 기술을 이용하여 분리 시스템에 주입되었다. 사전 농축(pre-concentration) 컬럼은 다량의 황산 이온을 보유할 수 있는 이온 교환 용량이 큰 분석용 컬럼(AS 9 HC)을 사용하였다. 분리용 컬럼은 플루오라이드 이온의 감도를 증가시키기 위하여 틈새 부피(void volumn)와 시스템 압력을 감소시킬 수 있도록 보호 컬럼(AG 14)을 사용하였다. 첫 번째 전기전도도 검출기로는 플루오라이드 이온의 회수율을, 두 번째 전기전도도 검출기로는 제거되는 황산 이온 피크를 관찰함으로써 결정된 최적의 10-포트주입기의 스위칭 시간은 4.3 분 이었다. 시료 주입량이 $25{\mu}L$ 일때, $500mg\;L^{-1}$ 의 높은 황산 이온이 포함된 용액에서 플루오라이드 이온의 검출한계(S/N = 3)는 $2.4{\mu}g/L$였다.

온라인 시료주입과 UPLC-Orbitrap 질량분석법을 이용한 수질 조류독소의 고속분석방법 개발 및 환경시료적용 (Fast and Accurate Determination of Algal Toxins in Water using Online Preconcentration and UPLC-Orbitrap Mass Spectrometry)

  • 장제헌;김윤석;최재원
    • 한국물환경학회지
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    • 제28권6호
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    • pp.843-850
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    • 2012
  • Due to the fast response to algae bloom issue in drinking water treatment plant, very fast determination methodology for algal toxin is required. In this study, column switching technique based online preconcentration method was combined with high resolution full scan mass spectrometer to save sample preparation time and to obtain fast and accurate result. After parameter optimization of online preconcentration, 1mL filtered sample was directly injected to trap column with switching valve system. Next, target toxins are eluted by 98% acetonitrile and analysed with 150 - 1,100 amu scan range at 50,000 resolving power. Method detection limit (MDL) for microcystin-LR, the most toxic isomer, was 0.1 ng/mL and others such as microcystin-YR, microcystin-RR and nodularin were 0.08, 0.03 and 0.04 ng/mL, respectively. This is the best improved sensitivities with 1mL volume in the literature. Furthermore, due to the use of ultra pressure HPLC (UPLC), the whole method run was completed in 4 min. Real sample applications for 173 sample including 55 surface water and 118 treatment plant samples for raw and treated water could be done within 16 hours. In our calculation, this methodology is roughly 80% faster than the previous manual solid-phase extraction with LC-MS/MS method.

Cefamandole nafate 함유 주사제의 지원자에 대한 생물학적 동등성 시험 (Bioequivalence of Cefamandole Nafate I.V. (Mandol and Mancef) of Human Volunteers)

  • 권광일;이혜숙;지옥표
    • 약학회지
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    • 제34권5호
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    • pp.334-340
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    • 1990
  • The bioequivalence of Mandol and Mancef (cefamondole nafate injection preparation) was investigated for 8 healthy human volunteers. Cefamandole nafate hydrolysis to cefamandole base in the blood and shows antibacterial activity. As the rate of the hydrolysis can be varied according to the buffer used in the preparation, the bioequivalence of cefamandole nafate I.V. was studied. A new HPLC method, the column switching technique, was developed and used for the simultaneous determination of cefamandole and cefamandole nafate in the plasma and in the urine. There were no statistically significant difference in between Mandol and Mancef for the parameters of AUC and Cp 0.25 hr even through the power of the test was not enough.

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횡단류 유동 내 원형 및 타원형 액체제트의 분열길이 (Breakup Lengths of Circular and Elliptical Liquid Jets in a Crossflow)

  • 송윤호;안규복
    • 한국분무공학회지
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    • 제23권1호
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    • pp.9-15
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    • 2018
  • Breakup lengths of circular and elliptical liquid jets in a subsonic crossflow were experimentally studied. Two circular-shaped and four elliptical-shaped plain-orifice injectors, which had different aspect ratios and orifice length to diameter ratios, were used to provide various liquid jet conditions such as steady, cavitation, and hydraulic flip. By varying the injection pressure drop from 1 bar to 6 bar, spray images were taken using a shadowgraph technique. Breakup lengths were measured and analyzed. As the aspect ratio in orifices increased, liquid column breakup lengths normalized by the equivalent diameter were reduced irrespectively of the switching of the major or minor axis to the crossflow. It was also found that when hydraulic flip developed inside the orifice, x-directional breakup lengths more decreased for both circular and elliptical liquid jets.

Deans Switching을 이용한 가스크로마토그래피에서 DME-LPG 혼합연료의 탄화수소 화합물 분석방법 (Determination Method of Hydrocarbon Compounds in DME-LPG Blending Fuels by Gas Chromatography with Deans Switching)

  • 연주민;박천규;임의순;정충섭
    • Korean Chemical Engineering Research
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    • 제50권2호
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    • pp.353-357
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    • 2012
  • 액화석유가스(liquefied petroleum gas, LPG)에 디메틸에테르(dimethyl ether, DME)가 첨가된 DME-LPG 혼합연료의 탄화수소 화합물을 가스크로마토그래피(GC)를 이용하여 정성 정량분석하는 새로운 분석방법을 연구하였다. DME-LPG 혼합연료는 함산소화합물(oxygen-containing compound)인 극성의 DME와 비극성물질인 LPG로 구성되어 있기때문에 하나의 GC 컬럼에서 모든 성분을 완전히 분리하기가 어렵다. 따라서 서로 다른 성질의 화합물이나 아주 복잡한 화합물 중 목표물질의 분석에 응용되고 있는 Deans switching 시스템을 도입하였다. 상기 시스템은 두 개의 GC 컬럼 사이에 유체의 압력 제어를 통하여 용출되는 물질의 흐름 방향을 변경시켜주는 기술로서, 이 방법을 이용하여 DME와 LPG를 서로 다른 컬럼에서 분리하여 한번의 시료 주입으로 DME-LPG 혼합연료의 모든 탄화수소 화합물을 정성 정량분석할 수 있었다. 또한 DME 합성과정에서 부산물로 생성될 수 있는 메탄올, 포름산메틸, 에틸메틸에테르 같은 미량성분까지 분석이 가능하였다.