• Title/Summary/Keyword: on-line column switching

Search Result 10, Processing Time 0.029 seconds

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
    • /
    • v.17 no.5
    • /
    • pp.360-363
    • /
    • 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%.

  • PDF

Development and Validation of On-line Column Switching HPLC-MS/MS Method for 10 Phthalate Metabolites in Human Urine (LC-MS/MS를 이용한 인체시료 중 프탈레이트 대사체 동시분석법 확립)

  • Hong, Soon-Keun;Nam, Hye-Seon;Jung, Ki-Kyung;Kang, Il-Hyun;Kim, Tae-Sung;Cho, Sang-Eun;Jung, Su-Hee;Lee, Jang-Woo;Kim, Jun-Cheol;Kho, Young-Lim;Kang, Tae-Seok
    • Journal of Environmental Health Sciences
    • /
    • v.36 no.6
    • /
    • pp.510-517
    • /
    • 2010
  • Phthalates, such as di (2-ethylhexyl) phthalate (DEHP), dibutyl phthalate (DBP) have been proved to be teratogenics and endocrine disruptors, metabolized rapidly and excreted in the urine. In this study, a simultaneous analytical method for 10 phthalate metabolites, MnBP, MiBP, MBzP, MCHP, MEHP, MEHHP, MEOHP, MnOP, MiNP and MiDP, in human urines, based on switching system with on-line pretreatment column using HPLC-MS/MS has been developed. This method was validated according to the guideline of bioanalytical method validation of National Institute of Toxicological Research. Limits of detection range between 0.2 and 0.9 ng/ml for 10 phthalate metabolites. The calibration curves showed linearity in the range 0.997~0.999, and the results of the intra- and inter-day validations were in the range from 0.4 to 14.7% RSD and from 0.3 to 9.4% RSD, respectively. Recoveries of phthalate metabolites varied from 87.0 to 116.1%. This analytical method showed high accuracy and stable precision for all metabolites, and seems to be suitable for biomonitoring of phthalates in human urine.

A Study on the Development of Analytical Methods and Behaviors of Environmental Pollutants(III) : On-Line System for Preconcentration and Separation of Trace Phenols by HPLC (환경 오염물질의 정량법 개발과 거동에 관한 연구(III) : 미량 페놀류의 HPLC 정량을 위한 온 라인 농축)

  • Lee, Dai Woon;Kim, Jin Young;Park, Young Hun;Moon, Myeong Hee
    • Analytical Science and Technology
    • /
    • v.7 no.1
    • /
    • pp.33-39
    • /
    • 1994
  • The purpose on this study was to develop a new improved chromatographic method for determination of trace phenols from environmental waste water. The research was carried out with selected 8 phenols, and solid-phase extraction was employed as sample pretreatment method. The coupling of XAD-4 and Dowex $1{\times}8$ resin as preconcentration column increased the selectivities toward interferences coexisted in matrix. Automation was accomplished with on-line process of pretreatment and HPLC system. After elution of sample through XAD-4 column, phenols were adsorbed by dispersion force, then displaced from it by ACN basified, simultaneously and selectively readsorbed via anion exchange on Dowex $1{\times}8$. Dowex $1{\times}8$ column was washed by water. Phenols readsorbed were removed from Dowex $1{\times}8$ column by a minimum volumn of methanol containing HCl. Each pretreatment step was connected by switching valves and the eluate was directly on-line injected to obtain fast and reliable results into the HPLC. Recovery of phenols was greater than 90%. To examine utility of this method, analysis of phenols from laboratory waste water sample which was added some organic pollutants to find with phenols on environmental waste water were also accomplished without their interference effects.

  • PDF

Determination of Pesticide Residues in Water using On-line SPE-HPLC Coupling System

  • Lee, Dai Woon;Lee, Sung Kwang;Park, Young Hun;Paeng, Ki-Jung
    • Analytical Science and Technology
    • /
    • v.8 no.4
    • /
    • pp.539-543
    • /
    • 1995
  • The on-line SPE-HPLC coupling system was developed for the efficient separation and determination of trace pesticides, such as phenoxyacetic acids and esters, and triazines in aqueous solutions. By using the developed SPE-HPLC on-line system, the band broadening usually observed in single precolumn switching mode was greatly reduced, consequently, the quantitative determination of trace pesticides could be achieved, Besides, since most of the analytes preconcentrated by SPE column could be injected directly into HPLC system, the limit of detection can be improved down to ppt level.

  • PDF

On-line Trace Enrichment in High Performance Liquid Chromatography Using XAD-2 Precolumn for the Determination of Lonazolac in Human Plasma

  • Lee, Hye-Suk;Kim, Eun-Joo;Zee, Ok-Pyo;Lee, Yoon-Joong
    • Archives of Pharmacal Research
    • /
    • v.12 no.2
    • /
    • pp.108-113
    • /
    • 1989
  • A new column-switching high performance liquid chromatographic method was developed for the determination of lonazolac in plasma. This method was based on the on-line trace enrichment of lonazolac using a precolumn packed with Amberlite XAD-2. The analysis was complete in 20 min. between injections and the limit of detection was $0.1{\mu}g/ml$ using $100{\mu}l$ of plasma. The method was linear in range of $0.1-10{\mu}g/ml$ with a correlation coefficient of 0.9991. Absolute recovery of lonazolac from the spiked plasma samples ranged from 95.6% to 97.1%. The method was shown to be reproducible over the concentration range studied.

  • PDF

Simultaneous Determination of Polycyclic Aromatic Hydrocarbons and Their Nitro-derivatives in Airborne Particulates by Using Two-dimensional High-performance Liquid Chromatography with On-line Reduction and Fluorescence Detection

  • Boongla, Yaowatat;Orakij, Walaiporn;Nagaoka, Yuuki;Tang, Ning;Hayakawa, Kazuichi;Toriba, Akira
    • Asian Journal of Atmospheric Environment
    • /
    • v.11 no.4
    • /
    • pp.283-299
    • /
    • 2017
  • An analytical method using high-performance liquid chromatography (HPLC) with fluorescence (FL) detection was developed for simultaneously analyzing 10 polycyclic aromatic hydrocarbons (PAHs) and 18 nitro-derivatives of PAHs (NPAHs). The two-dimensional HPLC system consists of an on-line clean-up and reduction for NPAHs in the 1st dimension, and separation of the PAHs and the reduced NPAHs and their FL detection in the 2nd dimension after column-switching. To identify an ideal clean-up column for removing sample matrix that may interfere with detection of the analytes, the characteristics of 8 reversed-phase columns were evaluated. The nitrophenylethyl (NPE)-bonded silica column was selected because of its shorter elution band and larger retention factors of the analytes due to strong dipole-dipole interactions. The amino-substituted PAHs (reduced NPAHs), PAHs and deuterated internal standards were separated on polymeric octadecyl-bonded silica (ODS) columns and by dual-channel detection within 120 min including clean-up and reduction steps. The limits of detection were 0.1-9.2 pg per injection for PAHs and 0.1-140 pg per injection for NPAHs. For validation, the method was applied to analyze crude extracts of fine particulate matter ($PM_{2.5}$) samples and achieved good analytical precision and accuracy. Moreover, the standard reference material (SRM1649b, urban dust) was analyzed by this method and the observed concentrations of PAHs and NPAHs were similar to those in previous reports. Thus, the method developed here-in has the potential to become a standard HPLC-based method, especially for NPAHs.

Determination of Phthalate Metabolites in Korean Children's Urine by High Performance Liquid Chromatography with Triple Quadrupole Tandem Mass Spectrometry (LC/MS/MS를 이용한 어린이 소변 중 프탈레이트 대사산물 분석)

  • Kho, Young-Lim;Jeong, Jee-Yeon;Choi, Kyung-Ho;Kim, Pan-Gyi
    • Journal of Environmental Health Sciences
    • /
    • v.34 no.4
    • /
    • pp.271-278
    • /
    • 2008
  • Dialkylated phthalates have been commonly used as plasticizers and a variety of applications. Phthalate diesters have been shown to be developmental and reproductive toxicants. It is very difficult to exactly estimate the dose of dialkylated phthalates taken up by the general population because of environmental contamination. Urinary metabolites of phthalates enabled to estimate internal exposure. The objective of this study was quantitative determination of phthalate metabolites by LC/MS/MS with on-line cleanup method to analyze phthalate metabolites in Korean children's urine. We employed LC/MS/MS with on-line enrichment and column-switching techniques for this biological monitoring. Metabolites determined were 4 primary metabolites; MEHP, MnBP, MiBP, MEP and 2 secondary metabolites of DEHP; 5-OH-MEHP), 5-oxo-MEHP. We analyzed children's urine from 30 boys and 30 girls. The method detection limit of phthalate metabolites were 0.03 ng/mL for MEP, 1.05 ng/mL for MBP, 0.22 ng/mL for MEHP, 0.15 ng/mL for 5-OHMEHP and 0.16 ng/mL for 5-oxo-MEHP, respectively. Switching Column LC/MS/MS was proven to be a useful tool to determine metabolites of phthalate diesters in human urine. The correlation among phthalate metabolites was very high and statistically significant, except MEP. The children's age (months) was negatively correlated to the concentration of phthalate metabolites. The geometric mean concentration of phthalate metabolites (mg/g creatinine) in children's urine were 25.5 for MEP, 130.3 for MnBP, 56.8 for MiBP, 19.5 for MEHP, 85.6 for 5-OH-MEHP and 83.1 for 5-oxo-MEHP, respectively. Levels of estimated daily intake of parent phthalate compounds (${\mu}g$/kg bw/day) were 0.8 for DEP, 5.0 for DnBP, 1.9 for DiBP and $8.9{\sim}14.2$ for DEHP, respectively. Estimated daily intake for DEP and DiBP were lower than those of other studies but the value for DEHP was higher than that of other study.

An Optical True Time-Delay for Two-Dimensional X-Band Phased Array Antennas (2차원 X-밴드 위상 배열 안테나용 광 실시간 지연선로)

  • Jung, Byung-Min;Kim, Sung-Chul;Shin, Jong-Dug;Kim, Boo-Gyoun
    • Korean Journal of Optics and Photonics
    • /
    • v.16 no.3
    • /
    • pp.287-294
    • /
    • 2005
  • In this paper, an optical true time-delay (TTD) for two-dimensional (2-D) phased array antennas (PAAs), composed of a multi-wavelength optical source and a fiber optic delay line matrix consisting of $2\times2$ optical switches with optical fiber connected between cross ports, has been proposed. A 2-bit $\times4-bit$ optical TTD for 10-GHz 2-D PAAs has been implemented by cascading a wavelength dependent TTD (WD-TTD) and a wavelength independent TTD (WI-TTD). The unit time delay for WD-TTD and WI-TTD have been chosen as ${\Delta}T=12ps$ and $\Delta\tau=6ps$, respectively. Time delay have been measured at all radiation angles. The maximum delay error for WD-TTD was measured to be 3 ps due to jitter incurred from gain switching. For the case of WI-TTD, error was within ${\pm}\;1\;ps$. The proposed optical TTD for a 2-D PAA has the following advantages: 1) higher gain compared to one-dimensional linear PAAs, 2) stabilization of optical power and wavelength by using a multi-wavelength optical source, and 3) fast beam scan and simple operation due to electronic control of the $2\times2$ optical switches matrix on a column-by-column basis.

Core Circuit Technologies for PN-Diode-Cell PRAM

  • Kang, Hee-Bok;Hong, Suk-Kyoung;Hong, Sung-Joo;Sung, Man-Young;Choi, Bok-Gil;Chung, Jin-Yong
    • JSTS:Journal of Semiconductor Technology and Science
    • /
    • v.8 no.2
    • /
    • pp.128-133
    • /
    • 2008
  • Phase-change random access memory (PRAM) chip cell phase of amorphous state is rapidly changed to crystal state above 160 Celsius degree within several seconds during Infrared (IR) reflow. Thus, on-board programming method is considered for PRAM chip programming. We demonstrated the functional 512Mb PRAM with 90nm technology using several novel core circuits, such as metal-2 line based global row decoding scheme, PN-diode cells based BL discharge (BLDIS) scheme, and PMOS switch based column decoding scheme. The reverse-state standby current of each PRAM cell is near 10 pA range. The total leak current of 512Mb PRAM chip in standby mode on discharging state can be more than 5 mA. Thus in the proposed BLDIS control, all bitlines (BLs) are in floating state in standby mode, then in active mode, the activated BLs are discharged to low level in the early timing of the active period by the short pulse BLDIS control timing operation. In the conventional sense amplifier, the simultaneous switching activation timing operation invokes the large coupling noise between the VSAREF node and the inner amplification nodes of the sense amplifiers. The coupling noise at VSAREF degrades the sensing voltage margin of the conventional sense amplifier. The merit of the proposed sense amplifier is almost removing the coupling noise at VSAREF from sharing with other sense amplifiers.