• Title/Summary/Keyword: 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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A Study on the Separation of n-Hexane by Molecular Sieve 5A and the Purification for HPLC use (분자체 5A를 이용한 n-헥산의 분리와 HPLC급으로의 정제에 관한 연구)

  • Choi, Beom Suk;Kim, Young Man;Kim, Sun Tae
    • Analytical Science and Technology
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    • v.6 no.1
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    • pp.21-27
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    • 1993
  • Technical grade n-hexane whose purity is 54% has been purified for HPLC use. Methylcyclopentane, 2-methylpentane, and 3-methylpentane which are hardly isolated by fractional distillation were separated by the liquid-solid chromatography using molecular sieve 5A. UV and fluorescence impurities whose contents are critically regulated for HPLC solvent were removed by the adsorptive separation with alumina and silica gel. The present method also reduced the impurities of color(APHA), acidity, water, residue after evaporation, sulfur, and thiophene content, and the impurity contents were well within the specifications of HPLC solvent.

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Determination of Pantothenic acid in Fortified Foods by HPLC (시판 영양강화식품중 판토텐산의 분석)

  • 최윤주;장재희;박혜경;박건상;구용의;황인경;김대병
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.33 no.2
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    • pp.381-385
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    • 2004
  • This study was conducted to develop an HPLC method for determining pantothenic acid in fortified foods which has typically been determined by microbiological assay (MBA) according to AOAC and Korean Food Code approved methods. Pantothenic acid was determined by reversed-phase ion-pair HPLC using UV absorption (200 nm) after extraction with 20 mM potassium phosphate solution by sonication. The recovery of spiked samples and detection limit (LOD) by HPLC were 83.5∼109.6% and 0.5 ppm (mg/kg), respectively. The LOD of the microbiological assay (MBA) was much lower than that of HPLC. The concentrations of pantothenic acid analyzed in all tested samples (n=13) confirmed compliance with declared label claims. The range of recovery ratio by the HPLC method when compared to the microbiological assay was 91.9∼117.6%. There was not significant difference (p<0.01) between the HPLC and MBA methods and the equation of the regression curve was y=1.1428x-0.2269 (r=0.9842). This proposed HPLC method for determining pantothenic acid appears to be suitable for determining pantothenic acid concentrations above 0.25 mg/100 g in fortified foods.

A Study on Discriminative Criteria of 6 Kinds of Achyranthis Radix Using HPLC/DAD;Isolation and Identification of 20-hydroxyecdysone from Aclryranthes japonica $N-{AKAI}$ and Comparison of Patterns of Achyranthis Radix from Different Locations by HPLC (HPLC/DAD를 이용한 6종(種) 우슬(牛膝)의 분류기준 연구;우슬(牛膝)(쇠무릎, Achyranthes japonica $N_{AKAI}$)로부터 20-hydroxyecdysone 분리.동정 및 산지별 우슬의 HPLC 패턴 비교)

  • Kim, Jeong-Hi;Kim, Jong-Mun;Kang, Dae-Hoon
    • The Korea Journal of Herbology
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    • v.23 no.1
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    • pp.109-116
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    • 2008
  • Objectives : This study was performed to investigate the discriminative criteria of 6 kinds of Achyranthis Radix by HPLC/DAD. Methods : 20-hydroxyecdysone is isolated by silica gel column chromatography ($CHCl_3$:MeOH, 7:1-1:1 v/v) and identified by nuclear magnetic resonance, A high-performance liquid chromatographic method with diode array detection was used to identify 20-hydroxyecdysone in A. japonica. The analysis was performed using $C_{18}$ column with isocratic elution consisted of 18% acetonitrile and 82% water and the detection was carried out by DAD at 254 nm. 6 kinds of Achyranthis Radix from different locations were extracted in MeOH. Each extracts was analyzed by HPLC in same condition as used in analysis of 20-hydroxyecdysone. The identities of each extracts were determined by comparing the retention time and UV spectrum with that of reference compound. Results : 1. A. japonica and A. bidentata showed the similar patterns of HPLC chromatogram and 20-hydroxycedysone was present in both of them because the peaks having the same retention time and UV spectrum as 20-hydroxyecdysone were shown in the HPLC chromatograms of A. japonica and A. bidentata 2. Cyathula officinalis and C. capitata showed the similar patterns of HPLC chromatogram. The peak having the same retention time and UV spectrum as 20-hydroxyecdysone was shown in the HPLC chromatogram of C. capitata but not shown in the HPLC chromatogram of C. officinalis. 3. Two species of medicinal drugs from Sacheon province showed similar patterns of HPLC chromatogram. Achyranthis Radix from Sacheon(wild) did not have 20-hydroxycedysone but Achyranthis Radix from Sacheon(cultivated) showed the peak having the same retention time as 20-hydroxyecdysone but UV spectrum of the peak was different from that of 20-hydroxyecdysone. Conclusions : These results suggested that 20-hydroxyecdysone could be the discriminative criteria for Achyranthis Radix contain 20-hydroxyecdysone though they belong to different genus and species. And the patterns of HPLC chromatogram also could be the discriminative criteria as the different species of Achyranthis Radix belonging to the same genus showed similar patterns of HPLC chromatogram.

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Studies on Pretreatment for Analysis of Pesticides by Using HPLC and GC (HPLC 및 GC에 의한 농약분석에서 전처리에 대한 연구)

  • Oh, Bo Young;Bae, Jun Hyun;Kang, Jun Gil;Kim, Youn Doo
    • Journal of the Korean Chemical Society
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    • v.43 no.6
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    • pp.663-669
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    • 1999
  • For determination of separated pesticides by using GC and HPLC, liquid-liquid extraction(LLE) and solid phase extraction(SPE) have been carried out to separate and concentrate the organophophorous pesticides such as Diazinon, Fenitrothion, Phosmet, Phosalon and EPN in environmental water samples. ln determination of pesticides by HPLC/UV, SPE has resulted in higher recovery and more precision than LLE, while in determination of pesticides by GC/FPD, vice versa. HPLC/UV after the pretreatment process of sample by solid phase extraction (SPE-HPLC/UV) has suggested the possibility of determination of pesticides ppb level. ln comparison of detection limit, both SPE-HPLC/UV and LLE-GC/FPD are reasonably suitable for analysis of residue pesticides. ln the respect of the rapidity and the solvent required, SPE-HPLC/UV method has proven to be superior to LLE-GC/FPD.

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Analysis of Fatty Acyl Groups of Diacyl Galactolipid Molecular Species by HPLC/ESI-MS with In-source Fragmentation

  • Gil, Ji-Hye;Hong, Jong-Ki;Choe, Joong-Chul;Kim, Young-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.24 no.8
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    • pp.1163-1168
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    • 2003
  • The structures of molecular species of galactolipids, such as monogalactosyl diacylglycerol (MGDG) and digalactosyl diacylglycerol (DGDG), isolated from wheat flour have been investigated using negative-ion electrospray ionization (ESI) mass spectrometry interfaced with high performance liquid chromatography (HPLC). According to the result of HPLC analysis, MGDG and DGDG were found to consist of mixtures of five and four molecular species, respectively. The galactolipids have been also analyzed to determine their fatty acid compositions, using HPLC/ESI-MS combined with in-source (or cone voltage) fragmentation. HPLC/ ESI-MS is very useful for one-step analysis of mixtures of galactolipids with a small sample quantity. Especially, the carboxylate anions produced in in-source fragmentations of the negative-ion of each component separated by HPLC provide valuable information on the composition of its fatty acyl chains.

Bioactivity Analysis of Curcuminoids from Turmeric using On-line Screening HPLC-ABTS (On-line Screening HPLC-ABTS를 이용한 강황으로부터 Curcuminoids의 생물활성 분석)

  • Choi, Sun Do
    • Journal of Applied Biological Chemistry
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    • v.56 no.3
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    • pp.137-139
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    • 2013
  • Free radical scavengers in the bisdemethoxycurcumin (BDMC), demethoxycurcumin (DMC) and curcumin of turmeric (Curcuma longa) were screened, identified, quantified and isolation using coupled off-line-2,2'-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) (ABTS) and on-line screening high-performance liquid chromatography (HPLC)-ABTS assay. There was a very small margin of error between the off-line-ABTS method and the on-line screening HPLC-ABTS method.

HPLC Analysis and Screening of Standard Compound on Saposhnikoviae Radix for Standardization of GCSB-5 Preparation (생약복합제 GCSB-5의 품질 표준화를 위한 방풍의 지표성분 탐색 및 HPLC 분석)

  • Cha, Bae-Cheon;Lee, Eun-Hee
    • Korean Journal of Pharmacognosy
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    • v.40 no.2
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    • pp.103-108
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    • 2009
  • GCSB-5 preparation is a purified extract from a mixture of 6 medicinal plants(Acanthopanacis Cortex, Achyranthis Radix, Saposhnikoviae Radix, Cibotii Rhizoma, Glycine Semen Nigra, Eucommiae Cortex) that have been widely used for the treatment of various bone disorders. The aim of this study was to investigate HPLC analysis method and screening of standard compound on Saposhnikoviae Radix for quality standardization of a medicinal crude drug GCSB-5. Standard compound of Saposhnikoviae Radix was decided with cimifugin by isolation and instrumental analysis such as NMR. HPLC analysis method for the simultaneous determination of cimifugin was established for the quality control of the medicinal plants of Saposhnikoviae Radix species, GCSB-5 raw material and preparation. And validation of HPLC analysis methods were conformed for verification of HPLC methods by check to specificity, linearity, intra-day precision, inter-day precision and accuracy following ICH guideline.

The Application of Chiral HPLC Columns for Enantiomer Separation of Chiral Drugs (Chiral Drugs의 광학분할을 위한 HPLC Column의 응용)

  • Lee, Won-Jae
    • YAKHAK HOEJI
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    • v.53 no.2
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    • pp.60-68
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    • 2009
  • In terms of chiral issue, two enantiomers of chiral drugs often differ significantly in their pharmacological, toxicological and pharmacokinetic profile. Chiral switches of racemic drugs have been redeveloped as single enantiomers. Several chiral resolution techniques in chirotechnology are introduced and the most used chiral HPLC chromatographic method among several chiral analysis techniques is described with its several advantages. Several types of chiral HPLC columns derived from their chiral selectors are discussed with their property and applications for enantiomer separation.