• Title/Summary/Keyword: Column-switching technique

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

  • 박성진;김혜경;함태식;김병용
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.28 no.6
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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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    • v.17 no.5
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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
    • Proceedings of the PSK Conference
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    • 2003.04a
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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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    • v.8 no.4
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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.

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

  • Yun I-Ran;Choi You-Jeong;Lee Min-Kwon;Jeong Myeong-Ho;Kim Byeong-Hun
    • Korean Journal of Veterinary Service
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    • v.29 no.3
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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.

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

  • Song, Kyung-Sun;Eum, Chul-Hun;Kim, Sang-Yeon
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.383-388
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    • 2006
  • Simple post-wash method by ion chromatography (IC) was established for the rapid and precise determination of fluoride ion in wastewater from mine in fluorite mineralized area. High sulfate in sample was retained in a pre-column and less strongly held fluoride ion was transferred to the principal separation system using modified conventional IC with switching technique. An analytical column with high capacity (AS 9 HC) was used as a pre-column to retain the amount of high sulfate. A guard column (AG 14) as a separation column was used to increase the response of fluoride and reduce the system pressure. According to the recovery of fluoride ion with one detector and the observation of sulfate peak with another conductivity detector, the optimum switching time of 10-port chromatographic injector was 4.3 min. The limit of detection (S/N = 3) of fluoride in synthetic solution containing $500mg\;L^{-1}$ sulfate was $2.4{\mu}g/L$, with $25{\mu}L$ sample volume.

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

  • Jang, Je-Heon;Kim, Yun-Seok;Choi, Jae-Won
    • Journal of Korean Society on Water Environment
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    • v.28 no.6
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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.

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

  • Kwon, Kwang-Il;Lee, Hye-Suk;Zee, Ok-Pyo
    • YAKHAK HOEJI
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    • v.34 no.5
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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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Breakup Lengths of Circular and Elliptical Liquid Jets in a Crossflow (횡단류 유동 내 원형 및 타원형 액체제트의 분열길이)

  • Song, Yoonho;Ahn, Kyubok
    • Journal of ILASS-Korea
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    • v.23 no.1
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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.

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

  • Youn, Ju Min;Park, Cheon Kyu;Yim, Eui Soon;Jung, Choong Sub
    • Korean Chemical Engineering Research
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    • v.50 no.2
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    • pp.353-357
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    • 2012
  • The new qualitative and quantitative analytical method for hydrocarbon compounds in DME-LPG blending fuel, mixing dimethyl ether (DME) with liquefied petroleum gas (LPG), by using gas chromatography (GC) was investigated. It is difficult to analyze all components of DME-LPG blending fuel by using single column in GC due to consisting of the non-polar LPG and the polar DME which is oxygen-containing compound. Therefore, it has been introduced the Deans switching system, which are useful for analyzing mixtures of a very different nature and/or target analytes in very complex matrix. This technique is to control the pressure between two columns and to selectively change the path of effluent flows to either one of two columns. As a result, we found that DME and LPG can be completely separated at the different columns and the determination of all hydrocarbon compounds in DME-LPG blending fuel can be achieved to this method qualitatively and quantitatively during the operation of one injection. In addition, this method can be applied to the determination of trace components of by-product, such as methanol, methyl formate and ethyl methyl ether, which will be derived from DME synthesis process.