• Title/Summary/Keyword: Liquid Liquid Extraction

Search Result 1,075, Processing Time 0.031 seconds

Quantitation of L-carnitine in plasma by electrospray ionization tandem mass spectrometry (ESI/MS/MS를 이용한 혈장 중 카르니틴 정량분석)

  • Kang, Seung Woo;Kim, Ho Hyun;Lee, Kyung Ryul;Yoon, Hye-Ran
    • Analytical Science and Technology
    • /
    • v.18 no.2
    • /
    • pp.163-167
    • /
    • 2005
  • In this study, a novel analytical method has been developed for the rapid determination of L-carnitine in human plasma using electrospray ionization tandem mass spectrometry. Free carnitine (FC) was analyzed after extraction with 80% methanol and total carnitine (TC) was analyzed after hydrolysis and extraction. Acyl carnitine (AC) was subtracted FC from TC. Analytical methods used multiple reaction monitoring (MRM) scan modes. A correlation coefficient of linear regression ($r^2$) was 0.9995, recovery was 97%, reproducibility was less than 10%, and limit of detection (LOD) was $0.0016{\mu}mol/L$. This method reduced sample preparation time and showed high resolution and good reproducibility compared to that with liquid chromatographic methods. Normal control showed AC was lower than FC. Clinical management of patients with inborn error of metabolism showed FC was lower than AC. Thus, carnitine fraction level was very important to monitoring patients with metabolic disorder.

Pretreatment of Fish for the determination of polycyclic aromatic hydrocarbons using alkali digestion (알칼리분해를 이용한 어류 중 다환방향족탄화수소의 전처리방법)

  • Hu, Soojung;Lee, Hyomin;Chae, Youngzoo;Yoo, Eun-Ah
    • Analytical Science and Technology
    • /
    • v.18 no.5
    • /
    • pp.403-409
    • /
    • 2005
  • Polycyclic Aromatic Hydrocarbons(PAHs) contamination arises from several sources including processing of food(smoking, direct drying, cooking) and environmental contamination of air, water, or soil, the later being considered as the most important. In this study, to establish the analytical method for some PAHs[benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene, indeno(1,2,3-c,d)pyrene] in fish, alkali digestion time, extraction solvents, elution volume of florisil cartridge for clean-up have been optimized. The methodology involved saponification and extraction with n-hexane, clean-up on Sep-Pak florisil cartridges and determination by HPLC/FLD(High Performance Liquid Chromatography/Fluorescence Detector). Overall method recoveries for 8 PAHs spiked into these products ranged from 90 to 106%.

Determination of terbutaline in human plasma by coupled column chromatography (커플드칼럼크로마토그래피에 의한 사람 혈장 중 테르부탈린의 정량)

  • Ko, Mi Young;Jeon, Sang-Seol;Kim, Kyeong Ho
    • Analytical Science and Technology
    • /
    • v.28 no.2
    • /
    • pp.125-131
    • /
    • 2015
  • A method was developed and fully validated for the determination of terbutaline, a β2-receptor agonist, in human plasma. Plasma samples were prepared by solid-phase extraction with Sep-Pak silica, followed by high-performance liquid chromatography (HPLC). The terbutaline was pre-separated from the interfering components in plasma on a Luna C18 (2) column, and terbutaline and salbutamol as an internal standard were resolved and determined on a Luna Silica column. The two columns were connected by a switching valve equipped with silica pre-column. The pre-column was used to concentrate the terbutaline in the eluent from the C18 column before back-flushing onto the silica column with fluorescence detection at an excitation/emission wavelength of 276/306 nm. The method was shown to be specific by testing six different human plasma sources. Linearity was established for a concentration range of 0.4-20.0 ng/mL with a correlation coefficient of 0.9999. The lower limit of quantitation was 0.4 ng/mL with a precision of 10.1% as C.V.%.

토양의 특성에 따른 토양증기추출법 (Soil Vapor Extraction)의 Trichloroethylene (TCE)과 Toluene 정화 효율 실험

  • 강현민;이민희;정상용
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
    • /
    • 2002.04a
    • /
    • pp.191-194
    • /
    • 2002
  • 토양증기추출(Soil Vapor Extraction)법을 이용하여 대표적 휘발성 NAPL (Non-aqueous phase liquid)인 TCE (trichloroethylene)와 toluene을 토양으로부터 제거하는 칼럼 실험을 실시하였다. 토양특성 및 증기추출 조건들이 정화효율에 미치는 영향을 규명하는데, 균질한 Ottawa sand와 실제 오염지역의 토양들을 직경 2.5cm, 길이 30cm인 유리 칼럼이 충진시켰으며, 빨갛게 염색된 TCE 또는 toluene 4 g이 주입되었다 공기 유량계를 설치하여 0.03L/min의 일정한 속도로 공기가 주입되도록 하고, 퍼지장치를 설치하여 주입 공기의 습윤도를 99% 이상으로 유지하였다. 가스크로마토그래피로 유출 가스 농도를 분석하였다. Ottawa sand로 충진된 칼럼실험에서는 매질의 입자크기, 함수율, 토양 내 오염물 체류시간 등을 변화시켜 실험을 반복하였다. TCE로 오염된 세립질 Ottawa sand 칼럼실험에서 유출 공기의 최대 농도는 조립질 Ottawa sand 칼럼의 유출 농도보다 약 20% 정도 감소하였고, 오염지역의 실제토양 칼럼실험에서는 최대유출농도가 조립질 Ottawa sand 칼럼의 농도보다 약 50% 감소하였으나, 20 liter공기 주입 후부터는 모두 비슷한 농도감소 현상을 나타내었으며, 초기 주입량의 90 % 이상이 제거되었다. 함수율증가에 따른 유출공기의 농도 감소는 거의 나타나지 않았으며, TCE 주입 후 7일 동안 방치하였다가 SVE를 실시한 칼럼 실험에서도 잔류하는 TCE의 양이 약간 증가하였지만 20 liter 공기 추출 후에는 초기 주입량의 90% 가, 40 liter공기 추출 후에는 98% 이상이 제거되었다. Toluene으로 오염된 칼럼 실험에서도 TCE와 비슷한 제거 경향을 나타냈으며 200 liter 공기 추출 후에는 오염물 초기 주입량의 98% 이상이 제거되었다. 본 실험 결과로부터 증기추출법을 이용한 TCE, toluene 정화 효율성이 규명되었으며, 휘발성 NAPL로 오염된 실제 토양을 복원하기 위한 SVE법의 적용가능성을 확인할 수 있었다.

  • PDF

Quantitative Analysis of Platycodin D from Platycodon grandiflorum by HPLC-ELSD (HPLC-ELSD법에 의한 길경의 platycodin D 정량분석)

  • Kim, Geum-Soog;Kim, Hyun-Tae;Seong, Jae-Duck;Park, Hee-Saeng;Kim, Soo-Dong
    • Korean Journal of Medicinal Crop Science
    • /
    • v.10 no.3
    • /
    • pp.200-205
    • /
    • 2002
  • Platycodin D was isolated from n-butanol extract of Platycodi radix(Platycodon grandiflorum and identified by the spectroscopic analysis using $^1H$ and $^{13}C$ NMR techniques. A new method of analysis of platycodin D by high performance liquid chromatography(HPLC) was established using a reversed phase system with YMC-Pack ODS-AM( 250 X 4.6 mm) column and 30% acetonitrile as a mobile phase. Evaporative light scattering detector was used as detector. The kinds of extraction solvents and methods were examined to determine the efficient extraction condition and HPLC analysis was carried out to establish the optimum drying condition for the root of Platycodon grandiflorum. The contents of Platycodin D was highest as 0.083% when platycodon roots were dried at $60^{\circ}C$ using dry oven.

The Antimicrobial, Antioxidant, and Tyrosinase Inhibitory Activities of Solvent Extracts of Asterina pectinifera and Asterias amurensis (별 불가사리(Asterina pectinifera) 및 아므르 불가사리 (Asterias amurensis)추출물의 항균, 항산화 활성 및 미백 효과)

  • Cho, Woo-Jin;Lee, Hyun-Hwa;Jung, Yeon-Jung;Kim, Hun;Jeong, Eun-Jeong;Park, Sihyang;Lim, Chi-Won;Cha, Yong-Jun
    • Korean Journal of Fisheries and Aquatic Sciences
    • /
    • v.48 no.4
    • /
    • pp.432-438
    • /
    • 2015
  • This study examined the antimicrobial, antioxidant, and tyrosinase inhibitory activities of bioactive compounds extracted from two starfish, Asterina pectinifera and Asterias amurensis, using solvent extraction after $Protamex^{TM}$ hydrolysis. Methanol and acetone fractions collected by stepwise extraction from specimens were subjected to silica gel column chromatography (SGCC) (200 mesh and 400 mesh), followed by high-performance liquid chromatography (HPLC). Two fractions (7:3 and 5:5 chloroform : methanol ratio, v/v) eluted using silica gel column chromatography from the two starfishes showed higher antimicrobial activity against Propionibacterium acnes and dermatophyte fungi (Epidermophyton floccosum, Microsporum audouinii, Trichophyton ferrugineum, Trichophyton mentagrophytes, and Trichophyton rubrum), antioxidant activity ($EDA_{50}$, mg/mL), and tyrosinase inhibitory activity compared to the other fractions. The final fractions obtained from Asterina pectinifera (RT 7.53, 8.93, and 10.48 min) and Asterias amurensis (RT 5.02 min) by SGCC (400 mesh) and HPLC from two SGCC fractions (200 mesh) showed 8.94 and 15.59 mg/mL antioxidant activity ($EDA_{50}$) and 46.89 and 40.19 % tyrosinase inhibitory activity, respectively. Extracts from starfishes are potential cosmetic basic material.

A Study on Korean Green Tea(II) -Analysis of free Amino Acid and Mineral- (한국산(韓國産) 녹다(緣茶)에 대(對)한 연구(硏究) (제 II 보) -Free amino Acid와 무기성분(無機成分)에 대(對)하여-)

  • Jung, Jai-Kie;Yu, Choon-Hie;Chung, Tai-Young;La, Sang-Moo
    • Journal of Nutrition and Health
    • /
    • v.6 no.3
    • /
    • pp.17-20
    • /
    • 1973
  • Quantitative analysis was achieved by gas-liquid chromatographic method (GLC) with a single column system of OV-17 for 16 of free amino acids in Korean green tea and the contents of mineral in it was determined by atomic absorption flame emission. The results are summarized as follows: 1) Korean green tea contained Mn 1% or over out of the total ash content and $0.05{\sim}0.20%$ in the water extraction, as the major mineral. 2) Ba, Cr, Ni, Pb and V were analyzed also by small quantities relatively and Co, Tin and Ywere not detected in the water extraction. 3) GLC indicated the presence of 16 components in free ammo acids. 4) The quantities of free amino acids in Korean green tea were determined $2.96{\sim}6.61%$ Alanine, $1.01{\sim}l.89mg%$ Glycine, $2.07{\sim}7.81mg%$ Valine, $1.27{\sim}8.76mg%$ Leucine and Isoleucine, $94.31{\sim}316.27mg%$ Threonine, $9.10{\sim}39.91mg%$ Serine, $2.18{\sim}36.76mg%$ Hydroxyproline, $2.72{\sim}5.90mg%$ Proline, $39.64{\sim}70.02mg%$ Aspartic Acid, $25.93{\sim}101.28mg%$ Glutamic Acid and Lysine, $8.32{\sim}18.30mg%$ Phenylalanine and Tyrosine in trace amount. 5) The total free amino acid contents in Korean green tea ranged from 207.24mg% to 516.06mg% and Moo-Deoung tea contained outstandingly high, 516 mg% or over.

  • PDF

Separation of 6-Gingerol from Ginger [Zingiber officinale Roscoe] and Antioxidative Activity (생강으로부터 6-Gingerol의 분리 및 항산화 활성)

  • Lee, Bong-Soo;Ko, Meyong-Seok;Kim, Hyun-Jong;Kwak, In-Seob;Kim, Dong-Ho;Chung, Bong-Woo
    • KSBB Journal
    • /
    • v.21 no.6 s.101
    • /
    • pp.484-488
    • /
    • 2006
  • Ginger (Zingiber officinale) is widely used as a dietary condiment throughout the world. Its major constituent, 6-gingerol, exhibits diverse pharmacological activities including anti-oxidant and anti-tumor. Ginger were extracted by 0% to 95% ethanol. Maximum yield of 6-gingerol was obtained with 80% ethanol as extracting solvent at $30^{\circ}C$. We obtained increased yield (7%) of extraction by pretreatment with ultrasonication. Gingerols in the crude ginger extract was isolated by Sepacore preparative liquid chromatography on silica gel. We got the 6-gingerol which weight is 0.53 mg/mL, from fraction F9. Antioxidant effect of 6-gingerol were detected by DPPH moth(10. Its radical scavenging activity was $95{\sim}99%$ which compared with ascorbic acid.

Purification of Crude Protein Mixture from Panax ginseng and Hairy Root for Proteome Analysis (인삼 및 모상근의 프로테옴 분석을 위한 단백질 추출 방법)

  • 김승일;김수정;남명희;서종복;김수현;권경훈;김영환;최종순;유종신
    • Korean Journal of Plant Tissue Culture
    • /
    • v.28 no.6
    • /
    • pp.347-351
    • /
    • 2001
  • Panax ginseng C.A. Meyer is a well-known Korean traditional medicine. Until now, even though major research of ginseng has been focused on the pharmacological effect, clinical application and chemical analysis of extracted secondary metabolite for several years, the physiology and gene functions of ginseng were not well known. In this research, we have developed the protein extraction methods of ginseng root and hairy root for proteome analysis in order to elucidate the gene(s) function of ginseng. Using the liquid nitrogen (equation omitted) TCA method as protein extraction method, about 660 protein spots were detected on the 2-DE gel of hairy root. Additionally, comparative analysis result of 2-DEs of ginseng root (equation omitted) hairy root suggested that proteomes of same organism could be changeable according to the culture condition, growth stages and other stimulus.

  • PDF

Liquid Chromatographic Determination of Astaxanthin in Phaffia rhodozyma (HPLC에 의한 Phaffia rhodozyma 중의 Astaxanthin의 측정법)

  • Xu, Bao-Jun;Fang, Zhe-Ming;Kang, Hyo-Jin;Wang, Qi-Jun;Mo, Eun-Kyoung;Sung, Chang-Keun
    • The Korean Journal of Food And Nutrition
    • /
    • v.16 no.3
    • /
    • pp.165-170
    • /
    • 2003
  • A sensitive and accurate method for the detection of astaxanthin was developed. The optimum HPLC system for the extraction and quantification of astaxanthin was based on a reversed phase column, and a quaternate mobile phase contained dichloromethane. The amount of astaxanthin can be accurately quantified in Phaffia rhodozyma cultures. The results of this study suggest that the mixture solution of dimethylsulphoxide and acetone is the optimal extraction solvent for astaxanthin and samples treatment for astaxanthin analysis must control low temperature and absent light operation strictly.