• Title/Summary/Keyword: HPLC solvent

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The Effect of Solvent Trap Apparatus on the Analysis of Carbonyl Compounds in Cigarette Smoke (용매 포집장치가 연기 중 Carbonyl 화합물의 분석에 미치는 영향)

  • 김효근;이존태;윤오섭;이문수
    • Journal of the Korean Society of Tobacco Science
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    • v.25 no.2
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    • pp.137-143
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    • 2003
  • Among the most popular means of mainstream smoke collection for specific analysis are solvent traps. Determination of the carbonyl compounds as their 2,4-dinitrophenylhydrazones(DNPHs) by HPLC offers increased sensitivity and reproducibility in the analysis of mainstream cigarette smoke. In this work, the mainstream smoke of a reference cigarette(lR4F) was collected in four kinds of gas washing bottles and their effects on the analysis of carbonyl compounds were investigated. The results show that the porosity of fritted glass filter in gas washing bottles exerted profound effect on the composition of the carbonyl compounds in mainstream smoke.

A single-step isolation of useful antioxidant compounds from Ishige okamurae by using centrifugal partition chromatography

  • Kim, Hyung-Ho;Kim, Hyun-Soo;Ko, Ju-Young;Kim, Chul-Young;Lee, Ji-Hyeok;Jeon, You-Jin
    • Fisheries and Aquatic Sciences
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    • v.19 no.4
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    • pp.22.1-22.7
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    • 2016
  • One of the main compounds in Ishige okamurae, diphlorethohydroxycarmalol (DPHC), is known to exhibit antiviral and anti-inflammatory effects. However, it has not been investigated extensively. In this study, preparative centrifugal partition chromatography (CPC) coupled with 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) ($ABTS^+$) online HPLC was employed for effectively separating considerable amounts of antioxidant compounds from marine algae. Two main antioxidant compounds, DPHC and octaphlorethol A (OPA), respectively, were confirmed and isolated from the ethyl acetate (EtOAc) fraction of I. okamurae by $ABTS^+$ online HPLC and preparative CPC systems. The presence of DPHC and OPA was confirmed in the EtOAc fraction of I. okamurae by both liquid chromatography with diode array detection and electrospray ionization mass spectrometry (LC-DAD-ESI/MS) and $ABTS^+$ online HPLC systems: DPHC (39 mg) and OPA (23 mg) were successfully isolated from I. okamurae (500 mg) with optimum solvent composition (0.5:10:4:6; n-hexane/EtOAc/MeOH/water, v/v) with corresponding partition coefficients (K) of 1.62 and 2.71, respectively, by preparative CPC. Hence, CPC coupled with $ABTS^+$ online HPLC is convenient for the efficient and simple isolation of these antioxidant compounds from I. okamurae.

Simultaneous Analysis of Six Constituents in Oyaksungi-san using HPLC-PDA (HPLC-PDA를 이용한 오약순기산 중 6종 성분의 동시분석)

  • Seo, Chang-Seob;Kim, Jung-Hoon;Shin, Hyeun-Kyoo
    • Herbal Formula Science
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    • v.20 no.2
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    • pp.37-46
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    • 2012
  • Objectives : Oyaksungi-san(Wuyaoshunqisan) has been used for treatment of stroke and rheumatoid arthritis in Korea. In this study, a simple and accurate high-performance liquid chromatography(HPLC) method was established for simultaneous determination of six main components, liquiritin, ferulic acid, naringin, hesperidin, neohesperidin, and glycyrrhizin in Oyaksungi-san, a traditional Korean herbal prescription. Methods : The analytical column for separation of six constituents was used a Gemini $C_{18}$ column maintained at $40^{\circ}C$. The mobile phase consisted of two solvent systems, 1.0% (v/v) acetic acid in $H_2O$ (A) and 1.0% (v/v) acetic acid in acetonitrile (B) by gradient flow. The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 254 nm for glycyrrhizin, 280 nm for liquiritin, naringin, hesperidin, and neohesperidin, and 320 nm for ferulic acid. Results : Calibration curves were acquired with $r^2$ values ${\geq}0.9998$. The results of recovery test were 91.58%-105.90% with a relative standard deviations (RSDs, %) value less than 2.0%. The values of RSD for intra- and inter-day precision were 0.03%-1.72% and 0.03%-1.63%, respectively. The contents of the six compounds in Oyaksungi-san were 0.33-9.30 mg/g. Conclusions : The newly established HPLC method will be helpful to improve quality control of Oyaksungi-san.

Recovery of Catechin Compound from Korean Green Tea by Solvent Extraction and Partition (용매 추출과 분배에 의한 한국산 녹차로부터 카테킨 화합물이 회수)

  • 김정일;노경호
    • KSBB Journal
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    • v.16 no.5
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    • pp.442-445
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    • 2001
  • Catechin compounds as anticancer and antioxidant were target materials from Korean Green Tea in this work. The methodologies of solvent extraction and partition were utilized to recover catechin compounds from green tea and the optimal experimental conditions were found by comparing the degree of recovery as slovent. extraction times and operating temperatures. The extract was partitioned with chloroform, which was best fit to remove caffeine after the extraction of green tea with 80$^{\circ}C$ water for 40 min. Further, the resulting extract was partitioned in ethyl acetate layer to purify the catechin compounds of EGC, EC EGCG and ECG. This experimental result could be extended to preparative HPLC to obtain EGCG on a commercial scale.

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A Study on the Component Analysis of Sappan Wood Extracts (소목 추출물의 구조분석)

  • 이상락;김인회;남성우
    • Textile Coloration and Finishing
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    • v.14 no.4
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    • pp.229-239
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    • 2002
  • Colorants were extracted from the heartwood of sappan lin. with MeOH under reflux, and the concentrate or the powder of dye was prepared by low pressure concentration method using suitable organic solvent. Various components were isolated from sappan wood, and the chemical structure and mechanism of compound having the excellent antibacterial and deodorization properties were analyzed. The results obtained are as follows ; The seventeen components of sappan wood were seperated by HPLC chromatography, and the five components among them were existed more than 6% and the other components were existed lower than 0.6%. The resolving powers of the non-polar solvent and polar solvent systems were evaluated by their ability to resolve the samples. It showed that chloroform-methanol-water(800:150:10) system has the best resolving power. Although the seperation rate is very slow, polyamide C-100 column chromatography gives a clear seperation of sappan wood. On the basis of the spectrometric data such as IR, UV, $GC-Mass,\;^1H-NMR,\;^{13}C-NMR\;and\;^1H-^{ 13}C-NMR$, the chemical structure of compound haying the excellent antibacterial and deodorization properties was established as brazilin containing the functional groups such as two quaternary carbon, one benzyl carbon, methylene contiguous to oxygen and methylene caused by oxygen atom.

Extraction of Genistein from Sophora flavescens with Supercritical Carbon Dioxide (초임계유체를 이용한 고삼으로부터 Genistein의 추출)

  • Han, Chang-Nam;Kang, Choon-Hyoung
    • Korean Chemical Engineering Research
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    • v.53 no.4
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    • pp.445-449
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    • 2015
  • This study was directed to finding an optimum extraction condition of genistein from the S. flavescens with supercritical carbon dioxide as a solvent. In this effort, effects of the extraction conditions including pressure, temperature and a co-solvent on the extraction efficiency were investigated. The aqueous ethanol and methanol solutions were used as co-solvents while the tested operating pressure and temperature ranges were from 200 bar to 300 bar and from 308.15 K to 323.15 K, respectively. The concentration of genistein was determined by means of HPLC equipped with a UV detector. From the results, it was observed that an increase in pressure led to the higher extraction efficiency. Further, methanol showed better performance as a co-slovent than ethanol. The DPPH radical scavenging activities were measured to compare antioxidant activities of S. flavescens extracts.

Determination of Hyperin in the Fruits of Acanthopanax Species by High Performance Liquid Chromatography

  • Lee, Jeong-Min;Kim, Hye-Min;Lee, Su-Llim;Han, Saem;Cho, Seon-Haeng;Lee, Sang-Hyun
    • Natural Product Sciences
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    • v.16 no.1
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    • pp.39-42
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    • 2010
  • The content of hyperin in Acanthopanax species was determined by high performance liquid chromatography (HPLC). Hyperin was quantified by a reverse-phase column with elution program [initially gradient solvent (acetonitrile : water = 85 : 15 to 80 : 20 for 20 min), then isocratic solvent (acetonitrile : water = 80 : 20 for 20 min), and finally gradient solvent (acetonitrile : water = 80 : 20 to 65 : 35 for 20 min)]. UV detection was conducted at 210 nm. The content of hyperin in the fruits of Acanthopanax was measured in the species A. chiisanensis (2.04 mg/g), A. sessiliflorus (1.13 mg/g), A. divaricatus (0.98 mg/g), A. koreanum (0.75 mg/g) and A. senticosus (0.05 mg/g). The content of hyperin in A. chiisanensis was higher than that of other Acanthopanax species.

A Chemical Component of the Marine Alga Ishige Okamurae

  • Kim, Eun-Sook;Choi, Byoung-Wook;Lee, Bong-Ho
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.255.3-256
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    • 2003
  • Marine Algae of order Chordariales are rich resources of bioactive metabolites. Methanolic extracts of the brown alga /shige Okamurae exhibited potent antioxidative and butyrylcholinesterase(BChE) inhibitory effects. Bio-guided purification [solvent partition, ODS flash, silica flash, gel-filtration on Sephadex LH 20, ODS HPLC] of them gave a compound 1. Its structure was elucidated by detailed analysis of spectroscopic data of 1 and comparison of literature data. A variety of bioassay for 1 is in progress.

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Speciation Analysis of Arsenic Species in Surface Water (수중의 비소 종 분리 분석)

  • Jeong, Gwan-Jo;Kim, Dok-Chan
    • Journal of Korean Society of Environmental Engineers
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    • v.30 no.6
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    • pp.621-627
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    • 2008
  • In this study, a technique of speciation and determination of the trace inorganic arsenic(As(III) and As(V)) in water sample using HPLC-DRC-ICP-MS has been developed. Isocratic mobile phase of 10 mM ammonium nitrate and 10 mM ammonium phosphate monobasic was used and methanol(5 v/v%) was used as flushing solvent. Selection of the best flow rate of reaction gas, O$_2$, and optimization of the parameters such as pH and flow rate of mobile phase, and injection volume of sample for the separation and detection of arsenic species were carried out. The oxygen flow rate of 0.5 mL/min, pH of 9.4 and flow rate of 1.5 mL/min of mobile phase, and injection volume of sample of 100 $\mu$L were found to be the best parameters for the speciation and determination of arsenic species. The analytical features of the method were detection limit 0.10 and 0.08 $\mu$g/L, precision(RSD) 4.3% and 3.6%, and recovery 95.2% and 96.4% for As(III) and As(V), respectively. Analysis time was 4 minutes per sample. Linear calibration graphs with r$^2$ = 0.998 were obtained for both As(III) and As(V). Speciation analysis of arsenic species in the raw water samples collected from the tributary streams to Han River and main stream of Paldnag were performed by the proposed method. The concentrations of As(III) ranged from 0.10 to 0.22 $\mu$g/L and As(V) concentrations ranged from 0.44 to 1.19 $\mu$g/L, and 93.5% of total arsenic was found to be As(V).

Validation of an HPLC Method for the Pharmacokinetic Study of Glipizide in Human (글리피짓 체내동태 연구를 위한 혈청 중 글리피짓의 HPLC 정량법 검증)

  • Cho, Hea-Young;Lee, Hwa-Jeong;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.35 no.3
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    • pp.137-142
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    • 2005
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of glipizide in human serum was validated and applied to the pharmacokinetic study of glipizide. Glipizide and internal standard, tolbutamide, were extracted from human serum by liquid-liquid extraction with benzene and analyzed on a Nova Pak $C_{18}\;60{\AA}$ column with the mobile phase of acetonitrile-potassium dihydrogen phosphate (10 mM, pH 3.5) (4:6, v/v). Detection wavelength of 275 nm and flow rate of 0.7 ml/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed glipizide concentration (500 ng/ ml) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-1000 ng/ml with correlation coefficient greater than 0.999. The lower limit of quantitation using 0.5 ml of serum was 10.0 ng/ml, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 82.6 to 105.0% for glipizide with overall precision (% C.V.) being 1.13-13.20%. The percent recovery for human serum was in the range of 85.2 93.5%. Stability studies showed that glipizide was stable during storage, or during the assay procedure in human serum. The peak area and retention time of glipizide were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of glipizide in human serum samples for the pharmacokinetic studies at three different laboratories, demonstrating the suitability of the method.