• Title/Summary/Keyword: G C Separation

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Identification of Curcuminoids from Turmeric (Curcuma longa) Using Ultrasonic Wave and Dipping Method (초음파 및 침적방법을 이용한 강황 (Curcuma longa)으로부터 Curcuminoids의 확인)

  • Lee, Kwang-Jin;Ma, Jin-Yeul;Kim, Young-Sik
    • KSBB Journal
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    • v.27 no.1
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    • pp.33-39
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    • 2012
  • In this study three major curcuminoids in turmeric curcumin (1), demethoxycurcumin (2) and bismethoxycurcumin (3) were efficiently extracted by optimizing extraction condition and simultaneously identified using a fast and reliable RP-HPLC-UV-MS and TLC method. The analysis by the $C_{18}$ column was performed and the UV wavelength was fixed at 425 nm. In this result, the total extraction yield of turmeric (Curcuma longa) was increased with extraction time from 1 to 7 h. So, optimum extraction time is 4 h. Also, the highest yield of extraction amount 0.433g 8.66% was obtained by ultrasonic waves with quarter frequency kHz and an extraction time of 7 h. The experiment method was consistent with theoretical Value $r^2$ = 0.987 (1), 0.997 (2) and 0.998 (3). Moreover, LC-MS analysis provided efficiently molecular weight information of three major curcuminoids in turmeric extracts and high purity (~95%) of the curcuminoids were obtained. This work offers would be useful for chemical and biological studies of natural plants and its products.

Comparative analysis of the magnetic and the transport properties of electron- and hole-doped manganite films

  • Kim, K.W.;Prokhorov, V.G.;Flis, V.S.;Park, J.S.;Eom, T.W.;Lee, Y.P.;Svetchnikov, V.L.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.226-226
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    • 2010
  • Microstructure, magnetic and transport properties of as-deposited electron-doped $La_{1-x}Ce_xMnO_3$ and hole-doped $La_{1-x}Ce_xMnO_3$ films prepared by pulse laser deposition, with x = 0.1 and 0.3, have been investigated. The microstructural analysis reveals that the $La_{1-x}Ce_xMnO_3$ films have a column-like microstructure and a strip-domain phase with a periodic spacing of about 3c, which were not found for the $La_{1-x}Ce_xMnO_3$ ones. At the same time, the experimental results manifest that there is no fundamental difference in the magnetic and the transport properties between electron- and hole-doped manganite films, except the appearance of ferromagnetic response in the low-doped $La_{0.9}Ce_{0.1}MnO_3$ film at temperatures above the Curie point. The observed magnetic behavior, typical for the Griffiths-like phase, for this film is explained by the percolation mechanism of the ferromagnetic transition and by the presence of strip-domain phase which stimulates the magnetic phase separation.

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Discrimination of Panax ginseng Roots Cultivated in Different Areas in Korea Using HPLC-ELSD and Principal Component Analysis

  • Lee, Dae-Young;Cho, Jin-Gyeong;Lee, Min-Kyung;Lee, Jae-Woong;Lee, Youn-Hyung;Yang, Deok-Chun;Baek, Nam-In
    • Journal of Ginseng Research
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    • v.35 no.1
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    • pp.31-38
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    • 2011
  • In order to distinguish the cultivation area of Panax ginseng, principal component analysis (PCA) using quantitative and qualitative data acquired from HPLC was carried out. A new HPLC method coupled with evaporative light scattering detection (HPLC-ELSD) was developed for the simultaneous quantification of ten major ginsenosides, namely $Rh_1$, $Rg_2$, $Rg_3$, $Rg_1$, Rf, Re, Rd, $Rb_2$, Rc, and $Rb_1$ in the root of P. ginseng C. A. Meyer. Simultaneous separations of these ten ginsenosides were achieved on a carbohydrate analytical column. The mobile phase consisted of acetonitrile-water-isopropanol, and acetonitrile-water-isopropanol using a gradient elution. Distinct differences in qualitative and quantitative characteristics for ginsenosides were found between the ginseng roots produced in two different Korean cultivation areas, Ganghwa and Punggi. The ginsenoside profiles obtained via HPLC analysis were subjected to PCA. PCA score plots using two principal components (PCs) showed good separation for the ginseng roots cultivated in Ganghwa and Punggi. PC1 influenced the separation, capturing 43.6% of the variance, while PC2 affected differentiation, explaining 18.0% of the variance. The highest contribution components were ginsenoside $Rg_3$ for PC1 and ginsenoside Rf for PC2. Particularly, the PCA score plot for the small ginseng roots of six-year old, each of which was light than 147 g fresh weight, showed more distinct discrimination. PC1 influenced the separation between different sample sets, capturing 51.8% of the variance, while PC2 affected differentiation, also explaining 28.0% of the variance. The highest contribution component was ginsenoside Rf for PC1 and ginsenoside $Rg_2$ for PC2. In conclusion, the HPLC-ELSD method using a carbohydrate column allowed for the simultaneous quantification of ten major ginsenosides, and PCA analysis of the ginsenoside peaks shown on the HPLC chromatogram would be a very acceptable strategy for discrimination of the cultivation area of ginseng roots.

Survey of Beet Red Contents in Foods using TLC, HPLC (TLC, HPLC를 이용한 식품 중 비트레드 함량조사)

  • Jang, Yaung-Mi;Lee, Tal-Soo;Hong, Ki-Hyoung;Park, Sung-Kwan;Park, Sung-Kug;Kwon, Yong-Kwan;Park, Jae-Seok;Chang, Sun-Young;Hwang, Hye-Shin;Kim, Eun-Jeong;Han, Yeun-Jeong;Kim, Byung-Sub;Won, Hye-Jin
    • Journal of Food Hygiene and Safety
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    • v.20 no.4
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    • pp.244-252
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    • 2005
  • This study was performed far development of new analytical method of beet red in foods. In this study, analysis of beet red in foods has been carried out by detection of betanine and isobetanine, the main color component of beet red as indicator compounds. The qualitative analysis technique consisted of clean-up of the colors with a $C_{18}$ cartridge, separation of the colors by cellulose TLC plate using acetone:3-methyl-1-butanol:distilled water (7:7:6) as a solvent system. Also, the quantitative analysis was performed using X-terra RP at wavelength 538 nm and $0.1\%$ phosphoric acid : methanol (90:10) as a solvent. The quantitative results of beet .ed were as follows:900.22$\∼$27701.60 $\mu$g/g for 60 item in nutrient supplement food, $21.95\∼713.40{\mu}g/g$ for 30 items and N.D. for 18 items in cindy, and $155.85{\∼}505.37{\mu}g/g$ for 12 items in ice creams, $43.52\∼64.75{\mu}g/g$ for 18 items and N.D. for 54 item in sauce, N.D. for 12 items in retort food.

Development of Analysis Method for Cholesterol in Infant Formula by Direct Saponification (직접 검화법을 이용한 조제분유의 콜레스테롤 분석법 개발)

  • Kim, Jin-Man;Park, Jung-Min;Yoon, Tae-Hyung;Leem, Dong-Gil;Yoon, Chang-Yong;Jeong, Ja-Young;Jeong, In-Seek;Kwak, Byung-Man;Ahn, Jang-Hyuk
    • Food Science of Animal Resources
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    • v.31 no.6
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    • pp.944-951
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    • 2011
  • An improved cholesterol analysis method was developed for powdered infant formula by gas chromatographic separation after liquid-liquid extraction and partition. In the official Korea Food Standard method for cholesterol analysis, the water phase and solvent phase were not well separated in the case of emulsified foods such as powdered infant formulas and baby foods. For the rapid and simple sample preparation method, an optimized direct saponification condition was established for heating temperature, heating time, and KOH concentration. From the results, the optimum conditions were as follows: heating temperature $90^{\circ}C$, heating time 60 min, and 16 M KOH 10 mL for a 2 g infant formula sample; improved separation condition for gas chromatography was as follows: the initial oven condition was $250^{\circ}C$ for 25 min, the oven temperature was increased to $290^{\circ}C$ by $10^{\circ}C$/min ratio, and finally the oven temperature remained at $290^{\circ}C$for 9 min. The developed method could be implemented for the study of cholesterol, providing the advantages of reduced inspection time and cost in emulsified foods such as infant formula.

Comparison of Methods for Detection of Escherichia coli O157:H7 in Ground Beef and Radish Sprouts

  • Lee, Jae-Hoon;Hyeon, Ji-Yeon;Heo, Seok;Hwang, In-Gyun;Kwak, Hyo-Sun;Choi, In-Soo;Park, Chan-Kyu;Seo, Kun-Ho
    • Food Science of Animal Resources
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    • v.30 no.2
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    • pp.179-184
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    • 2010
  • Escherichia coli O157:H7 is a food-borne pathogen that causes bloody diarrhea, hemorrhagic colitis, and hemolytic uremic syndrome (HUS). We compared three selective media and evaluated the performance of immunomagnetic separation (IMS) for the detection of low levels of E. coli O157:H7 in ground beef and radish sprouts with different levels of background flora. Bulk food samples (500 g for each trial) were artificially inoculated with nalidixic acid-resistant E. coli O157:H7 at the lowest dose that would generate 20 partial-positive samples of 25 g each. All samples were homogenized in mTSB (225 mL) and incubated overnight at $37^{\circ}C$. IMS was performed using the enriched mTSB samples (1 mL) along with conventional spreads plated onto three different selective media: Sorbitol MacConkey agar (SMAC), Sorbitol MacConkey agar with cefixime and tellulite (CT-SMAC), and Sorbitol MacConkey agar with nalidixic acid (NAL-SMAC) as the gold standard. Two suspicious colonies from each medium were selected and confirmed usinga serological test after transfer to tryptic soy broth with yeast extract (TSAYE). CT-SMAC was better than SMAC for detecting E. coli O157:H7 in all food types. Although there was no statistical difference in the number of positive samples when using IMS vs. non-IMS techniques, more positive samples were detected when IMS was used in both ground beef and radish sprouts. It appears that the improvement was more significant in radish sprouts, which had a higher level of background flora than ground beef. The results also suggest that the combination of CT-SMAC and IMS is sufficient to recover low levels of E. coli O157:H7 in high background flora food samples.

Rapid and Simple Method for the Determination of Pregabalin in Human Plasma using Liquid Chromatography-tandem Mass Spectrometry (LC-MS/MS): Application to a Bioequivalence Study of Daewoong Pregabalin Capsule To Lyrica® Capsule (Pregabalin 150 mg)

  • Jang, Ki-Ho;Seo, Ji-Hyung;Yim, Sung-Vin;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.41 no.4
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    • pp.255-262
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    • 2011
  • Method using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed and validated for the determination of pregabalin in plasma samples. Acquisition was performed by monitoring the transitions: m/z 160.1${\rightarrow}$142.2 for pregabalin and m/z 423.2${\rightarrow}$207.1 for losartan (as an internal standard). After cold acetonitrileinduced protein precipitation of the plasma samples, separation was performed with C18 column by isocratic mobile phase consisted of 10 mM ammonium acetate and acetonitrile (15:85, v/v). Results were linear over the concentration ranged from 0.1 to $10{\mu}g$/mL and the correlation coefficients (r) were $\geq0.99$. Intra- and inter-day precisions were $\leq6.02$ and $\leq11.04%$, respectively, and intra- and inter-day accuracies were 96.60-101.09 and 98.10-102.60%, respectively. This validated method was successfully applied to a bioequivalence study of two formulations of pregabalin, Daewoong pregabalin capsule (Daewoong Pharm. Co., Ltd.) and Lyrica$^{(R)}$ capsule (Pfizer Korea Ltd.) in twenty eight healthy Korean volunteers. The subjects received a single oral dose of each formulation (150 mg as pregabalin) in a randomized $2{\times}2$ crossover study and plasma samples were obtained from each subject at predetermined time intervals. Then, the pharmacokinetic parameters ($AUC_{0-t}$, $C_{max}$ and $T_{max}$) were calculated and statistically analyzed to assess the differences between two formulations. The 90% confidence intervals for the log-transformed data were acceptable range of log 0.8-log 1.25 (e.g., log 1.0048-log 1.0692 for AUC0-t, log 0.9142-log 1.0421 for $C_{max}$). Thus, $AUC_{0-t}$ and $C_{max}$ met the criteria of the Korea Food and Drug Administration (KFDA) for bioequivalence test indicating that Daewoong pregabalin capsule was bioequivalent to Lyrica$^{(R)}$ capsule.

Partial Purification and Some Properties of Amylases from Germinating Corn(Zea mays L.) (발아 옥수수 amylases의 정제 및 특성)

  • Lee, Tae-Ho;Jung, Tae-Yung;Park, Mi-yeon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.19 no.6
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    • pp.625-635
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    • 1990
  • The purpose of this study was focused on investigation of biochemical properties of amylases in germinating corn(Zea mays L.) the amylase(I), (II) and (III) from germinating corn seeds were partially purified by ammonium sulfate precipitation, DEAE-Sephadex A-50 ion exchange column chromatography and Sephadex G-100 gel filtration. The last step was effective for separation of the corn amylases to a homogeneous slate. the purified amylase(I) was identified as a kind of $\alpha$-amylase from the fact that 5% starch solution was hydrolysed into mainly maltose and maltotetrose by it, and amylase(II) and amylase(III) were enzymes producing maltotetrose as main product. The molecular weight and specific activity of the amylase(I), (II) and (III) were determined to be 54,000 and 70.47 unit/mg, 39,000 and 62.98 unit/mg, and 51,000 and 80.39 unit/mg, respectively. It showed a tendency to increase the amylases activities in presence of Ba, Ca, Co and Fe groups, but inhibits in that of Ag, Sn, Hg and Zn groups, and amylase(I), (II) and (III) remained stable at pH 5-6 and 2$0^{\circ}C$ for 40 days in containing of 1 mM CaCl$_2$. The optimum pH and optimum temperatures were pH 6, pH 5 and pH 6 and 35$^{\circ}C$, 55$^{\circ}C$ and 55$^{\circ}C$, respectively. These results suggest that the amylase(I), (II) and (III) were different amylases.

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Study on Characteristics and Preparation of Binderless ZSM-5 Granules for Adsorption of Xylene Isomers (Binderless ZSM-5 성형체의 합성 및 자일렌 이성체의 흡착 특성에 관한 연구)

  • Yun, Hyo-Sang;Hong, Ji-Sook;Suh, Jeong-Kwon;Shin, Chae-Ho
    • Applied Chemistry for Engineering
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    • v.21 no.4
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    • pp.417-423
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    • 2010
  • In this study, an effective method to prepare granular binderless ZSM-5 which is as efficient p-xylene separatory adsorbent was explored. Colloidal silica sol 30 wt% solution as an inorganic binder and microcrystalline cellulose as an organic additive were added to ZSM-5 powder ($SiO_2/Al_2O_3$ = 50). Adsorbent with enough strength (0.721 kgf), high crystallinity (94.6%) and high BET specific surface area ($379.2m^2$/g) was obtained by calcination, binderless treatment, ${NH_4}^+$ ion exchange, and activation after spherical granulation process. A batch type adsorption experiment was proceeded with solutions comprising 3 xylene isomers by 1 : 1 : 1 weight ratio to evaluate adsorption characteristics of prepared absorbent. As a result, the obtained binderless ZSM-5 granule showed a higher selective adsorption performance for para-xylene than that of commercial adsorbent.

Radical Scavenging Effects of 10 Plant Essential Oils and Active Compound Screening Analysis (식물정유 10 종의 라디칼 소거 활성과 주요 활성 성분의 탐색)

  • Kim, A Young;Pyo, Byoung Sik;Kim, Sun Min;Park, Mi Jin;Lee, Sung Suk;Lee, Kyoung In
    • Korean Journal of Medicinal Crop Science
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    • v.27 no.6
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    • pp.427-435
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    • 2019
  • Background: A growing interest in health has increased the need for the development of potent antioxidant materials known to play a role in various physiological activities. Currently research and development of non-toxic natural antioxidants with high activity is ongoing. Methods and Results: In this study, we measured 2,2'-azinobis- (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) and 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging ability of 10 plant essential oils, selecting samples of Dendranthema indicum, Dendranthema zawadskii, and Citrus sunki essential oils. The samples were analyzed using liquid chromatography (LC) and the radical scavenging activity on LC-based systems with the same conditions. In the LC-mass spectroscopy (MS)/MS analysis of the active compound peak, 2-methoxy-4-vinylphenol with a molecular weight of 150.1 g/mol was identified in C. sunki essential oils. Eugenol or isoeugenol with a molecular weight of 164.1 g/mol as identified in D. indicum and D. zawadskii essential oils as radical scavenging active compounds. Conclusions: In the LC-based measurement system, the active ingredient can be identified by simultaneously conducting profile analysis and the radical scavenging activity of essential oil samples. In addition, LC-MS/MS analysis of the active compound peaks can be performed under the same separation conditions to obtain data that can identify the active compounds in the sample.