• 제목/요약/키워드: acetonitrile extraction

검색결과 219건 처리시간 0.025초

Synthesis and characterization of α-mangostin imprinted polymers and its application for solid phase extraction

  • Zakia, Neena;Zulfikar, Muhammad A.;Amran, Muhammad B.
    • Advances in materials Research
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    • 제9권4호
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    • pp.251-263
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    • 2020
  • α-mangostin imprinted polymers have been synthesized by a non-covalent imprinting approach with α-mangostin as a template molecule. The α-mangostin molecularly imprinted polymers (MIPs) prepared by radical polymerization using methacrylic acid, ethlylene glycol dimethacrylate, benzoyl peroxide, and acetonitrile, as a monomer, crosslinker, initiator, and porogen, respectively. The template was removed by using methanol:acetic acid 90:10 (v/v). The physical characteristics of the polymers were investigated by Fourier Transform Infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). The rebinding studies were carried out by batch methods. The results exhibited that the MIPs was able to adsorb the α-mangostin at pH 2 and the contact time of 180 min. The kinetic adsorption data of α-mangostin performed the pseudo-second order model and followed the Langmuir isotherm model with the adsorption capacity of 16.19 mg·g-1. MIPs applied as a sorbent material in solid-phase extraction, namely molecularly imprinted solid-phase extraction (MISPE) and it shows the ability for enrichment and clean-up of α-mangostin from the complex matrix in medicinal herbal product and crude extract of mangosteen (Garcinia mangostana L.) pericarp. Both samples, respectively, which were spiked with α-mangostin gives recovery more than 90% after through by MISPE in all concentration ranges.

Determination of Levofloaxcin in Human Serum by High-Performance Liquid Chromatography/Diode Array Detector and its Application to Pharmacokinetics of Levofloxacin in Volunteers

  • Kim, Seung-Yong;Chung, Youn-Bok;Kwon, Oh-Seung
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.305.1-305.1
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    • 2003
  • A simple, specific and sensitive method for the determination of levofloaxcin (LFX) in human serum was developed by a high performance liquid chromatography/diode array detector and applied to pharmacokinetic study of LFX in human volunteers. This method involves several steps such as precipitation with acetonitrile, extraction with methylene chloride, evaporation, and concentration, using 0.5ml of the serum. (omitted)

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최적 분석조건에 의한 강황으로부터 Curcuminoids의 고체상추출(SPE) (Solid Phase Extraction(SPE) of Curcuminoids from Turmeric by Optimization Analytical Condition)

  • 이광진;마진열;김영준;김영식
    • 한국산학기술학회논문지
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    • 제13권10호
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    • pp.4927-4935
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    • 2012
  • 강황은 다양한 약리활성을 가진 약초이다. 강황에 포함된 curcumin, demethoxycurcumin(DMC)과 bisdemethoxycurcumin(BDMC)을 침적과 초음파방법을 이용하여 추출하였다. 그리고 고체상추출(SPE)을 사용하여 추출효율을 확인 하였다. 추출액은 3가지 상업용 $C_{18}$ 역상 고성능 액체 크로마토그래피에 의해 이동상으로 물과 아세토나이트릴을 사용하여 일정용매법으로 동시분리 분석을 하였다. 유속은 1.0mL/min, 주입부피는 $10{\mu}L$, 컬럼오븐 온도 $40^{\circ}C$, 파장 425nm에서 수행되었다. 실험결과, RS tech column을 사용하고 물과 아세토나이트릴의 조성비가 (50 : 50vol%)일 때 최적 조건을 얻을 수 있었다. 용매조성(물과 메탄올)에 따른 추출 수율에의 영향을 살펴본 결과 100% 메탄올에서 curcuminoids(추출시간 4h)가 가장 많이 추출되었고, 수용성 메탄올 조성보다 함량이 높았다. 100% 물에 의해, 고체상추출은 curcuminoids의 추출함량(mAU${\times}$mim)이 침적과 초음파방법보다 24.5와 14.3배 높았다. 이상의 결과는 제약 및 기능성 소재로서의 응용 가능성을 나타내었다.

Ultrasonic-assisted Micellar Extraction and Cloud-point Pre-concentration of Major Saikosaponins in Radix Bupleuri using High Performance Liquid Chromatography with Evaporative Light Scattering Detection

  • Suh, Joon-Hyuk;Yang, Dong-Hyug;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • 제32권8호
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    • pp.2637-2642
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    • 2011
  • A new ultrasonic-assisted micellar extraction and cloud-point pre-concentration method was developed for the determination of major saikosaponins, namely saikosaponins -A, -C and -D, in Radix Bupleuri by high performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD). The non-ionic surfactant Genapol X-080 (oligoethylene glycol monoalkyl ether) was chosen as the extraction additive and parameters affecting the extraction efficiency were optimized. The highest yield was obtained with 10% (w/v) Genapol X-080, a liquid/solid ratio of 200:1 (mL/g) and ultrasonic-assisted extraction for 40 min. In addition, the optimum cloud-point pre-concentration was reached with 10% sodium sulfate and equilibration at $60^{\circ}C$ for 30 min. Separation was achieved on an Ascentis Express C18 column (100 ${\times}$ 4.6 mm i.d., 2.7 ${\mu}M$) using a binary mobile phase composed of 0.1% acetic acid and acetonitrile. Saikosaponins were detected by ELSD, which was operated at a $50^{\circ}C$ drift tube temperature and 3.0 bar nebulizer gas ($N_2$) pressure. The water-based solvent modified with Genapol X-080 showed better extraction efficiency compared to that of the conventional solvent methanol. Recovery of saikosaponins ranged from 93.1 to 101.9%. An environmentally-friendly extraction method was successfully applied to extract and enrich major saikosaponins in Radix Bupleuri.

초음파를 이용한 고삼에 포함된 Genistein 및 Formononetin의 추출 (Extraction of Genistein and Formononetin from Sophoraflavescens Aiton using Ultrasonic wave)

  • 김영식;이광진
    • Korean Chemical Engineering Research
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    • 제47권2호
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    • pp.258-261
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    • 2009
  • 본 연구에서는 추출용매 물 100%을 이용하여 다양한 초음파 에너지(35, 72, 170 KHz)와 추출 시간(30, 60 min)에 의한 고삼으로부터 식물성에스트로겐 제니스테인 및 포르모노네틴의 추출량과 일반성분의 영향을 비교하였다. 전처리 단계는 초음파추출, 여과, 농축, 막분리로 구성되었다. 추출된 용액은 역상 고성능 액체크로마토그래피 (HPLC)를 사용하여 분석하였다. 이동상 조성은 A는 물/아세트산(99.9/0.1 vol%), B는 아세토니트릴/아세트산(99.9/0.1 vol%)이며, A/B를 80/20~65/35 vol%로 60분 동안 선형적으로 변화시켰다. 실험결과에 의하면 일반성분은 탄수화물(0.255~0.413%)을 제외한 나머지 성분들의 함량은 거의 비슷하게 확인되었다. 또한 주파수 170 KHz, 60 min에서 추출량이 3.17 g으로 추출 수율이 가장 우수하였고 천연물관련 화학 및 생물학 연구에 기초자료로 도움이 될 것이다.

Maximization of Extracted Condition of Pro-angiogenic Components in Citrus unshiu Peels using Dimethyl Sulfoxide

  • Lee, Jungwhoi;Kim, Myungseung;Kim, Jae Hoon
    • Natural Product Sciences
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    • 제22권4호
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    • pp.287-292
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    • 2016
  • Aqueous extraction of Citrus unshiu peels (AECUP) is mainly comprised with pro-angiogenichesperidin and narirutin. In this study, we report approaches to increasing the yields of extracted hesperidin and narirutinfrom Citrus unshiu peels using proper solvents. Significantly improved yields of both compounds were obtained using methanol and dimethyl sulfoxide (DMSO) compared to acetonitrile, ethyl acetate, ethanol, and isopropyl alcohol. Especially, effect of DMSO was by far the better of the two solvents in extraction of hesperidin. In addition, the DMSO extracted hesperidin significantly induced the pro-angiogenic effects of human umbilical vein endothelial cells (HUVECs) and markedly up-regulated phosphorylation of the ERK1/2 signaling pathway. These results demonstrate that pro-angiogenic inducer; hesperidin and narirutin can be simply, easily, and effectively extracted from Citrus unshiu peels.

GC/MS-SIM for the Determination of Alkylphenols, Chlorophenols and Bisphenol A in Paper Materials

  • Kim, Hyub
    • 한국환경독성학회:학술대회논문집
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    • 한국환경독성학회 2003년도 춘계학술대회
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    • pp.145-145
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    • 2003
  • A method for the determination of alkylphenols, chlorophenols and bisphenol A in paper materials using GC/MS-SIM has been developed. Eleven endocrine disrupting chemicals (EDCs) of phenols in paper samples were extracted with acetonitrile. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 82.4∼108.8 % by area ratio of pheranthrene-d$\sub$10/ vs bisphenol A d$\sub$l6/. (isoBOC derivatization and TBDMS derivatization) The SIM responses were linear with the correlation coefficient varying 0.9717∼0.9995 (isoBOC derivatization), and 0.9842∼0.9980 (TBDMS derivatization). The range of concentrations was respectively, 0.95∼l.44 ng/g in 2,4-dichlorophenol, 1.01∼1.17 ng/g in t-butylphenol, 2.17∼5.84 ng/g in pentachlorophenol, 12.68∼14.88 ng/g in nonylphenol and 30.84∼153.72 ng/g in bisphenol A.

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지리산 오갈피나무로부터 Acanthoside-D의 추출 및 정제 (Extraction and Purification of Acanthoside-D from Acanthopanax chilsanensis)

  • 이광진;강지훈;노경호
    • KSBB Journal
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    • 제16권1호
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    • pp.71-75
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    • 2001
  • 지리산 오갈피에 주로 포함된 Acanthoside-D은 인삼과 유사한 물질로 알려져 있다. Acanthoside-D에 대한 분석용뿐만 아니라 제조용에서의 실험조건을 구하는 것이 연구의 목적이 된다. 지리한 오갈피의 줄기의 파우더를 ethanol 용액으로 추출한 후 hexane으로 분배하였다. 정제된 추출액을 $\mu$-Bondapak $C_{18}$ (3.9 $\times$ 300 mm, $10\mu\textrm{m}$) 칼럼을 이용하여 지라산 오갈피 줄기에 포함된 Acanthoside-D를 분리하기 위한 분석조건을 확립하였다. 본 연구의 결과에 의하면 목적물질인 Acanthoside-D를 분리하기 위해 이동상의 조성은 water/acetonitrile/methanol=80/14/6 %(v/v)이었고, 유속은 1.0 mL/min, UV 검지기는 210 mm로 고정하였다. 위의 분석조건을 이용하여 반제조용 컬럼(3.9 $\times$ 300 mm, $15\mu\textrm{m}$,Lichrospher 100RP-18)에서 분리 가능한 최대 주입량은 $250\mu\textrm{L}$ 이었다.

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GC/MS/MS를 이용한 105종의 잔류농약 분석에 관한 연구 (Determination of 105 pesticide residues by GC/MS/MS)

  • 김우성;도정아;이희정;이주영;양승주;이선희
    • 분석과학
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    • 제23권4호
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    • pp.395-404
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    • 2010
  • 레몬과 콩 그리고 채소류에서 105개의 잔류농약을 다종 다성분 분석법으로 GC/MS/MS 분석하였다. 각 시료로부터 acetonitrile로 1차 추출하고 NaCl 15 g을 첨가한 다음 액-액 분배하였으며, Florisil 고체상(SPE) Cartridge로 정제하여 분석하였다. 레몬과 콩에서의 105개 농약의 회수율은 azinphos-methyl, famoxadone, fenamidone, flufenoxuron, triadimefon을 제외한 모든 농약에서 우수한 것으로 나타났는데 레몬에서 71.1~126.0%, 콩에서는 72.5~124.5% 였다. 또한 레몬에서의 검출한계와 정량한계는 각각 0.001~150 ng/mL와 0.004~500 ng/mL으로 확인되었다.

HPLC-PDA를 이용한 Amitraz의 분석법 확립 및 검증 (Determination of amitraz by high-performance Liquid chromatography with photodiode array detection and method validation)

  • 윤형준;윤소미;이명헌;손성완
    • 대한수의학회지
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    • 제48권1호
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    • pp.33-38
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    • 2008
  • In veterinary medicine amitraz has been used as an insecticide to eliminates mites, lice, and ticks in dogs, cats, goats, swine and cattle. The objective of present study was to developed an analytical method using one-step extraction and determination of the amitraz in veterinary drugs by liquid chromatography (LC). The amitraz was analyzed by LC equipped with Waters XTerra RP18 ($4.8{\times}250mm;\;5{\mu}m;\;Waters,\;USA$) analytical column, using 75% acetonitrile (acetonitrile/D.W; 75/25) at 1.0 ml/ min. The UV-VIS detection of amitraz was made at 290 nm. Calibration graphs were linear with very good correlation coefficients ($r^2>0.9999$) from $80{\sim}120{\mu}g/ml$. The limit of detection was $0.09{\mu}g/ml $ and limit of quantification was $0.27{\mu}g/ml $. The method showed good intra-day precision (CV 0.05~0.09%) and inter-day precision (CV 0.06~0.18%).