• Title/Summary/Keyword: Conventional HPLC

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Metabolomics Approach for Classification of Medicinal Plants

  • Lee, Dong-Ho
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2010.05a
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    • pp.5-5
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    • 2010
  • Selection of specific medicinal sources as well as bioactive compounds is important for the preparation of medicine and related products with good quality. It is necessary to pay close attention for choosing correct medicinal sources, particularly in case of medicinal plants, because of their diversity, which can affect the quality and efficacy of medicine. Discrimination of plants based on morphological or genetic characteristics has been used as a conventional classification method of pharmaceutical sources so far; however, more need demands more general methods for accurate quality assessment of medicinal plants. In this study, ultra performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF MS) technique applied to this metabolic profiling is a powerful tool due to its higher sensitivity, resolution, and speed compared to conventional HPLC technique. The metabolite profiling of several medicinal plants including Panax ginseng was carried out using UPLC/Q-TOF MS and total metabolites were then subsequently applied to various statistical tools to compare the patterns. The developed metabolomics tool with UPLC/Q-TOF MS successfully identified and classified the samples tested according to their origins.

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Development of New Surfaces and Materials for Separation Science

  • Linford, Matthew R.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.59.1-59.1
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    • 2015
  • In the Linford group at Brigham Young University we have recently developed three new sets of materials for three different areas of separations science: thin layer chromatography (TLC), high performance liquid chromatography (HPLC), and solid phase microextraction (SPME). First, via microfabrication we have grown patterned carbon nanotube (CNT) forests on planar substrates that we have infiltrated with inorganic materials such as silicon nitride. The coatings on the CNTs are conformal and typically deposited in a process like low pressure chemical vapor deposition. The resulting materials have high surface areas, are porous, and function as effective separation devices, where separations on our new TLC plates are typically significantly faster than on conventional devices. Second, we used the layer-by-layer (electrostatically driven) deposition of poly (allylamine) and nanodiamond onto carbonized poly (divinylbenzene) microspheres to create superficially porous particles for HPLC. Many interesting classes of molecules have been separated with these particles, including various cannabinoids, pesticides, tricyclic antidepressants, etc. Third, we have developed new materials for SPME by sputtering silicon onto cylindrical fiber substrates in a way that creates shadowing of the incoming flux so that materials with high porosity are obtained. These materials are currently outperforming their commercial counterparts. Throughout this work, the new materials we have made have been characterized by X-ray photoelectron spectroscopy, time-of-flight secondary ion mass spectrometry, scanning electron microscopy, transmission electron microscopy, etc.

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Quantitative Analysis of Paeoniflorin from Paeonia lactiflora Using $^1H-NMR$

  • Yoo, Jong-Su;Song, Myoung-Chong;Ahn, Eun-Mi;Lee, Youn-Hyung;Rho, Yeong-Deok;Baek, Nam-In
    • Natural Product Sciences
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    • v.12 no.4
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    • pp.237-240
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    • 2006
  • Paeoniflorin, the major component of the root of Paeonia lactiflora, was quantitatively analyzed using $^1H-NMR$ spectrometry. The quantity of paeoniflorin was calculated by the ratio of the intensity of the signals (H-9, H-10, H-2', 6') to the aldehyde peak of the known amount of internal standard, 2,4,6-trihydroxybenzaldehyde. These results were compared with the conventional HPLC method. The contents of paeoniflorin in P. lactiflora, which were respectively calculated by H-9, H-10, H-2', 6' in the $^1H-NMR$ spectra and HPLC, were determined $2.60{\pm}0.07,\;2.44{\pm}0.09,\;2.77{\pm}0.12\;and\;2.46{\pm}0.16%$. The advantages of quantitative $^1H-NMR$ analysis are that can be analyzed to identify and quantify, and no reference compounds required for calibration curves. Besides, it allows rapid and simple quantification for paeoniflorin with an analysis time for only 20 min without any preprocessing.

Separation of Non-Volatile Compounds Unsuitable for GC Using Supercritical Fluid as Mobile Phase (초임계 유체를 이동상으로 사용함으로써 기체 크로마토그래피로 분리하기 힘든 비휘발성 화합물들의 분리)

  • Pyo, Tong Jin;Kim, Hoon Ju
    • Analytical Science and Technology
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    • v.5 no.2
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    • pp.153-158
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    • 1992
  • In this work, we developed supercritical fluid chromatographic methods for the samples which are difficult to analyze with conventional GC or HPLC. Long-chain Hydrocarbons, mink oils and soybean oils unsuitable for GC because of their low volatility or limited thermal stability were separated by SFC due to the high solvating properties of supercritical carbon dioxide fluids. In our research, a new method for the analysis of polar fatty acids and pesticides was developed. This method should be used to overcome problems with polar samples in SFC.

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Synthesis of Periodic Mesoporous Organosilica by Microwave Heating

  • Yoon, Sang-Soon;Son, Won-Jin;Biswas, Kalidas;Ahn, Wha-Seung
    • Bulletin of the Korean Chemical Society
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    • v.29 no.3
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    • pp.609-614
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    • 2008
  • A periodic mesoporous organosilica material was synthesized by microwave heating (PMO-M) using 1,2-bis(trimethoxysilyl)ethane as a precursor in a cationic surfactant solution, and textural properties were compared with those of the product produced by conventional convection heating (PMO-C). These synthesized materials were characterized using XRD, TEM/SEM, N2 adsorption isotherm, 29Si and 13C NMR, and TGA, which confirmed their good structural orders and clear arrangements of uniform 3D-channels. Synthesis time was reduced from 21 h in PMO-C to 2-4 h in PMO-M. PMO-M was made of spherical particles of 1.5-2.2 m m size, whereas PMO-C was made of decaoctahedron-shaped particles of ca. 8.0 m m size. Effect of synthesis temperature, time, and heating mode on the PMO particle morphology was examined. The particle size of PMO-M could be controlled by changing the heating rate by adjusting microwave power level. PMO-M demonstrated improved separation of selected organic compounds compared to PMO-C in a reversed phase HPLC experiment. Ti-grafted PMO-M also resulted in higher conversion in liquid phase cyclohexene epoxidation than by Ti-PMO-C.

Simultaneous Determination of Amoxicillin and Ampicillin in Fish Meat Using High-Performance Liquid Chromatography (HPLC를 이용한 어류 중의 Amoxicillin과 Ampicillin 항생제 동시 분석법)

  • Jo, Mi-Ra;Kim, Poog-Ho;Lee, Tae-Seek;Oh, Eun-Gyoung;Yu, Hong-Sik;Lee, Hee-Jung
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.39 no.6
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    • pp.454-459
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    • 2006
  • A simultaneous high-performance liquid chromatography assay method for amoxicillin and ampicillin in fish products was developed, evaluated, and validated by monitoring these antibiotics in fish samples obtained from aquaculture and distribution. The recovery rate of this method was higher than those of conventional methods and was 95.3-106.6% for amoxicillin and 81.4-92.4% for ampicillin. Our pretreatment procedure sufficiently removed or reduced materials affecting HPLC analysis, such as low-molecular-weight substances. The performance limit of this method was evaluated as 0.01 ppm of amoxicillin and ampicillin in fish muscle. Finally, 171 fish samples, including olive flounder (Paralichthys olivaceus), common sea bass (Lateolabrax japonicus), and black rock fish (Sebastes schlegeli) collected from fish farms in the coastal area between April and September 2005 were analyzed to evaluate the overall efficiency of the method and to monitor the actual of amoxicillin and ampicillin usage in fish farms. The results indicated that the developed method was suitable for analyzing amoxicillin and ampicillin in fish muscle, and determined that those antibiotics were being used for fish farming but were not detected in fish samples during the shipping and distribution stages.

Improvement of analytical method for catechins in green tea (녹차의 카테킨류 분석법 개선)

  • Rah, Hyo-Hwan;Baik, Soon-Ok;Han, Sang-Bin;Bock, Jin-Young
    • Applied Biological Chemistry
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    • v.35 no.4
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    • pp.276-280
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    • 1992
  • Quantutative analysis of catechins by HPLC was studied. When the mobile phase was switched from the conventional(AOAC) Methanol, Acetonitril and Acetic acid solution in $H_2O$ to 0.06% Phosphate solution with Acetonitrile, N,N-Dimethyl formamide, and Ethyl acetate, retention time could be reduced from 45 min to 28 min, especially, we obtained sharper chromatogram of the compounds, either (-)EGCG or (-)ECG, which resulted in minimization of analytical erros. CVs of retention time $(0.32{\sim}3.97%)$ and peak area $(1.61{\sim}7.01%)$ indicated that the data were more reliable. Content of catechins in commerical teas analyzed by the method was $120.3{\sim}153.7\;mg/g$ in green teas which was about 4 times that in black tea.

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Analysis of Oxolinic Acid in Fish Products Using HPLC (HPLC를 이용한 어류 중의 Oxolinic Acid 분석)

  • LEE Hee Jung;LEE Tae Seek;SON Kwang Tae;KIM Poong Ho;JO Mi Ra;PARK Mi Jung;Yi Young Ho
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.38 no.6
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    • pp.379-384
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    • 2005
  • A high-performance liquid chromatography assay method for oxolinic acid in fish products was developed, evaluated and validated through the monitoring of oxolinic acid based on farming and distribution. The recovery rate of the developed method was $102.3-106.7\%$ as compared to conventional methods. The stock solution was stable for 3 weeks under refrigerated condition at $4^{\circ}C$ The performance limit was evaluated as 0.01ppm of oxolinic acid in fish muscle. 478 fish samples such as olive flounder, genuine porgy, common sea bass and black rock fish collected from fish farms in the coastal area from September 2001 to October 2004 were analyzed to evaluate overall efficiency of the modified method and to monitor the actual condition of oxolinic acid usage in fish farm. According to the monitoring results, the modified method was suitable for analysis of oxolinic acid in fish muscle and oxolinic acid might be used in a small portion of fish farms. The suggested analysis method of oxolinic acid was registered in the Korean Official Methods of Food Analysis and is being utilized for fishery products by the Korea Food and Drug Adminstration and the National Fisheries Products Quality Inspection Service.

Solid-Phase Refolding of Inclusion Body Protein in Packed Bed Adsorption and Expanded Bed Adsorption Chromatography (Packed Bed Adsorption과 Expanded Bed Adsorption 크로마토그래피를 이용한 내포체 단백질의 고체상 재접힘)

  • 최원찬;김민영;서창우;이은규
    • KSBB Journal
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    • v.18 no.6
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    • pp.500-505
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    • 2003
  • ‘LK (lipoprotein kringle) 68’is a polypeptide of a modified ansiostatin consisting of three kringle structures that might be clinically useful as a potential cancer therapeutics. It can be produced by overexpressing it as inclusion body in recombinant E. coli. In this study, solid-phase refolding processes using packed bed adsorption (PBA) and expanded bed adsorption (EBA) column were carried out to compare their refolding yields with that of the conventional, solution-phase refolding process, For the solution-phase and the PBA-mediated processes employing Q-Sepharose, washed inclusion body was used as the starting material, whereas both washed inclusion body and E. coli homogenate were used for the EBA-mediated process employing streamline DEAE. On the final recovery LK68 per unit mass of wet cell basis, the EBA- and PBA-mediated processes showed about 2.7- and 1.5-fold higher yields, respectively, than the solution-phase refolding method. The solid-phase refolded LK68 demonstrated the same Iysine binding bioactivity and the retention time in the RP-and SEC-HPLC as those of the native protein.

An Improved Method for Determination of Catechin and Its Derivatives in Extract and Oil of Grape Seeds (포도씨유 및 추출물의 카테킨류 측정방법 개선)

  • Moon, Sung-Ok;Lee, Jun-Young;Kim, Eun-Jung;Choi, Sang-Won
    • Korean Journal of Food Science and Technology
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    • v.35 no.4
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    • pp.576-585
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    • 2003
  • An improved method in place of a conventional vanillin spectroscopic method (CVSM) was developed for determination of catechin and its derivatives in extract and oil of grape seeds. For the CVSM, grape seed extracts had relatively high catechin content in the range of $17{\sim}43%$ (g/100g of extract), while grape seed oils had relatively smaller catechin content in the range of $30{\sim}40mg%$ (mg/100g of oil). For the improved vanillin spectroscopic method (IVSM) using a polyamide cartridge, catechin content of grape seed extracts was in the range of $4.0{\sim}7.5%$, while that of grape seed oils was below 5 ppm. Meanwhile, the quantities of catechin and its derivatives were determined by HPLC in the grape seed extracts and oils. Four major catechins [(+)-catechin, procyanidin B2, (-)-epicatechin, and epicatechin gallate] were detected from grape seed extracts, and the ranges of concentrations were as follows: (+)-catechin, $1.35{\sim}2.60%$; procyanidin $B_2$, $0.77{\sim}1.36%$; (-)-epicatechin, $2.35{\sim}4.59%$; (-)-epicatechin gallate, $0.06{\sim}0.30%$. In contrast, four catechins were barely detectable in the grape seed oils. The reproducibility of four major catechins in grape seed extracts, given as coefficient of variation, was below 5%, and the recovery close to above 95%. The achieved detection level of four catechins was $1{\sim}5\;ppm$. Additionally, the contents of catechin compositions in grape seed extract were also determined by HPLC in relation to different cultivars and producing areas. Thus, HPLC method and IVSM using polyamide cartridge can be used as alternative to CVSM for determination of catechin and its derivatives in extract and oil of grape seeds.