• Title/Summary/Keyword: Micro-HPLC

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Analysis of Carbendazim and Carbaryl by Micro-HPLC (Micro-HPLC에 의한 Carbendazim과 Carbaryl의 분석)

  • Choi, Kyoung-Sook;Lee, Hoe-Yeon;Lee, Duck-Hee;Byun, Woon-Ki
    • Analytical Science and Technology
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    • v.7 no.3
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    • pp.421-425
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    • 1994
  • A micro-high performance liquid chromatography(Micro-HPLC) techniquie with solid phase extraction was reported which detected carbendazim and carbaryl at picogram levels. They were separated on microbore packed $C_{18}$ column($1.0mm\;I.\;D{\times}150mm$, $d_f=5{\mu}m$) using a 50% methanol mobile phase and detected at UV 220nm(${\alpha}=2.94$, $R_s=4.71$), while they were not resolved on analtical HPLC system(${\alpha}=1.27$, $R_s=0.76$). The detection thresholds of carbendazim and carbaryl were 0.5ng and 0.1ng on Micro-HPLC, therefore Micro-HPLC system was 20~40 told more sensitive than anayltical HPLC system. Sep-Pak $C_{18}$ catridge was found to be efficient in enriching carbendazim and carbaryl from dilute aqueous solution with 97.0% and 97.8% recoveries of them. The Sep-Pak $C_{18}$ catridge followed by the Micro-HPLC had been applied to the quantitative analysis of carbendazim and carbaryl in spiked juices and a commercial drinking water.

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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.

Analysis of Microcystins(LR, YR and RR) in Water (Micro-HPLC/IS/MS에 의한 수 중의 Microcystins (LR, YR 및 RR)의 분석)

  • Park, Kwan Su;Bae, Jun Hyun;Kang, Jun Gil;Kim, Youn Doo
    • Journal of the Korean Chemical Society
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    • v.45 no.6
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    • pp.524-531
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    • 2001
  • Micro-HPLC/IS/MS after solid phase extraction has been employed to enhance the accu-racy in the determination of toxic microcystins, such as microcystin-LR, -YR and -RR. The absorbance at 238 nm in HPLC/UV and characteristic spectra of 135 m/z and $[M+H]^+$ m/z in MS have been widely monitored to identify those microcystin-LR, -YR and -RR. In this study, new lines at 507 m/z for LR, 520 m/z for RR and 532 m/z for YR have been additionally detected in the micro-HPLC/IS/MS spectrum, corresponding to double charge. The micro-HPLC/IS/MS methodology has been applied to investigate the presence of the toxic microcystins in Taecheong lake.

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DETERMINATION OF PURINE AND PYRIMIDINE BASES IN RUMEN MICRO-ORGANISMS BY REVERSED PHASE HPLC AFTER HYDROLYTIC DIGESTION UNDER PRESSURE

  • Han, Y.K.;Landis, J.
    • Asian-Australasian Journal of Animal Sciences
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    • v.4 no.2
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    • pp.161-164
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    • 1991
  • A rapid and accurate method is described for the determination of nucleo-bases in rumen micro-organisms. A procedure to satisfactorily hydrolyse the micro-organisms involving reaction with a mixture of readily volatile organic acids (acetic and formic acids) under high pressure, is proposed, and optimal conditions for an analytical procedure with reversed phase HPLC is described. The following nucleobases contents (mmol/kg DM) of rumen micro-organisms were found: Adenine (Ade), 82.62; Guanine (Gua), 61.34; Cytosine (Cyt), 84.61; Thymine (Thy), 35.74; Uracil (Ura), 68.62; Hypoxanthine (Hxn), 13.06; Xanthine (Xn), 8.35. Total purine-N content (g/kg N) of rumen micro-organisms were 99.60. The nucleic acid N content (g/kg N) of microbial isolates were: RNA-N, 109.9; DNA-N, 50.9.

Determination of meloxicam in human plasma by semi-micro high-performance liqiud chromatography.

  • Park, Chang-Hun;Kim, Ho-Hyun;Lee, Hee-Joo;Beom, Han-Sang
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.276.1-276.1
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    • 2003
  • This study describes a simple and sensitive semi-micro HPLC method with UV detection and direct deproteinization. The plasma protein was precipitated using perchloric acid (60%) and the supernatant was directly injected onto the semi-micro HPLC system. The separation was achieved on a C18 (25 mm ${\times}$ 2.0 mm I.D) analytical column with a mobile phase of sodium acetate buffer (pH 3.5, 50 mmol) - acetonitrile (60:40, V/V). (omitted)

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Rapid Identification of the ${\alpha}$-Glucosidase Inhibitory Compounds from Geranium thunbergii Sieb. et Zucc. by HPLC-micro-fractionation and HPLC-UV-$MS^n$

  • Choi, Se-Jin;Kim, Jin-Kyu;Lee, Yeon-Sil;Lim, Soon-Sung
    • 한국약용작물학회:학술대회논문집
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    • 2010.10a
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    • pp.430-430
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    • 2010
  • In this study ethanol extracts of aerial part of Geranium thunbergii Sieb. et Zucc. was investigated for their ability to inhibit a-glucosidase, and thus was fractionated using two organic solvents, including dichloromethane, ethyl acetate. The ethyl acetate-soluble fraction, which manifested potent enzyme inhibitory properties, was then followed by tracking down the active compound by combining HPLC micro-fractionation to an enzyme assay in 96-well plate. The ${\alpha}$-glucosidase inhibitory activity profile showed that two peaks exhibited potent inhibitory activity, and then the structural analyses of the two peaks were carried out by HPLC-UV-MS. The main ${\alpha}$-glucosidase inhibitory compounds in the ethyl acetate-soluble fractions of ethanol extracts of Geranium thunbergii Sieb. et Zucc. were tentatively identified as geraniin and kaempferol-7-rhamnoside.

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HPLC Analysis of Free Malonaldehyde in Nine Ginseng Polyacetylene-Treated Liver Microsome (인삼의 9종 폴리아세틸렌으로 처리한 간소포체 중의 유리 말론알데히드의 HPLC에 의한 분석)

  • Kim, Hye-Young;Kim, Shin-Il
    • Journal of Ginseng Research
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    • v.14 no.3
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    • pp.373-378
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    • 1990
  • Free malonaldehyde was determined in nine kinds of ginseng polyacetylene-treated micro- some by HPLC analysis. Antioxidant activities of some phenolic compounds and ginseng saponin were also drtermined both by a new HVLC method and by THA method. A new HPLC system separaterl malonaldehyde at a retention time 5,6 min and showed a linear relationship between the peak are a and malonaldehyde concentration. Panaxnol showed the strongest activity among nine polyacetylenes and the addition of either chlorine or aletyl group reduced polyacetylene's own activity. Since C14-polyacetylenes such as panaxyne and panaxyne-epoxide had little or no antioxidant activities, S17-structure should be preserved to exert a radical-scvenging or trapping activity. The antioxidant activities of chlorogenic acid, ferulic acid and catechol were much weaker than those of C17-polyacetylenes. Ginseng saponin showed no antioxidant activity. Since TBA reactive substances and malonaldehyde contents were almost the same in peroxiedized microsome. TBA value seems a good indicator for lipid peroxidation in this particular Fe+3 ADP/NADPH system.

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Development of Analytical Methods for Micro Levels of Naphthalene and TNT in Groundwater by HPLC-FLD and MSD (HPLC-FLD와 MSD를 이용한 지하수 중 나프탈렌 및 TNT의 미량 분석법 개발)

  • Park, Jong-Sung;Oh, Je-Ill;Jeong, Sang-Jo;Choi, Yoon-Dae;Her, Nam-Guk
    • Journal of Soil and Groundwater Environment
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    • v.14 no.6
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    • pp.35-44
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    • 2009
  • Naphthalene and TNT (2,4,6-trinitrotoluene) are defined by U.S. EPA as possible carcinogenic compounds known to have detrimental effects on the aquatic ecosystem and human body. There are, however, few researches on methods of analyzing micro-levels of naphthalene and TNT dissolved in groundwater. This study introduces and evaluates the newly developed analytical methods of measuring naphthalene and TNT in groundwater by using HPLC-FLD (Fluorescence detector) and MSD (Mass detector). The MDL, LOQ and salt effect of these methods, respectively, are compared with those of conventional methods which use HPLC-UV. For the analysis of naphthalene, HPLC-FLD was set in the maxima wavelength (Ex: 270 nM, Em: 330 nM) obtained from 3D-Fluorescence to be compared with HPLC-UV in 266 nM wavelength. The MDL ($0.3\;{\mu}g/L$) and LOQ ($2.0\;{\mu}g/L$) of naphthalene by using HPLC-FLD were approximately 80 times lower than those analyzed by HPLC-UV (MDL: $23.3\;{\mu}g/L$, LOQ: $163.1\;{\mu}g/L$). HPLC-MSD were used in comparison with HPLC-UV in 230 and 254 nM wavelength for the analysis of TNT. The MDL ($0.13\;{\mu}g/L$) and LOQ ($0.88\;{\mu}g/L$) of TNT analyzed by using HPLC-MSD were approximately 130 times lower than those obtained by using HPLC-UV in 230 nM (MDL: $16.8\;{\mu}g/L$, LOQ: $117.5\;{\mu}g/L$). The chromatogram of TNT analyzed by using HPLC-UV in 230 nM displayed elevated baseline as the concentration of ${NO_3}^-$ increases beyond 21 mg/L, while the analysis using HPLC-MSD did not demonstrate any change in baseline in presence of ${NO_3}^-$ of 63.7 mg/L which is 3.5 times higher than average concentration in groundwater. In conclusion, HPLC-FLD and HPLC-MSD may be used as suitable methods for the analysis of naphthalene and TNT in groundwater and drinking water. These methods can be applied to the monitoring of naphthalene and TNT concentration in groundwater or drinking water.

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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