• 제목/요약/키워드: reversed phase

검색결과 605건 처리시간 0.022초

LC-ESI-MS/MS를 이용한 생체시료 중 브롬화피나베리움의 고감도 분석 및 이를 이용한 생체이용률 평가 (Sensitive Determination of Pinaverium Bromide in Human Plasma by LC-ESI-MS/MS : Applicability to Oral Bioavailability Determination)

  • 박석;이예리;김호현;이희주;김윤균;염정록;한상범
    • Journal of Pharmaceutical Investigation
    • /
    • 제34권6호
    • /
    • pp.513-519
    • /
    • 2004
  • A sensitive method for quantification of pinaverium bromide in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS/MS). Glimepiride was used as internal standard. Pinaverium bromide and internal standard in plasma sample were extracted using tert-butylmethylether(TBME). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of acetonitrile-5 mM ammonium formate (80/20, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS with multiple reaction monitoring (MRM) mode, pinaverium and glimepirde were detected without severe interference from human plasma matrix. Pinaverium produced a protonated precursor ion $([M+H]^+)$ at m/z 510.3 and a corresponding product ion at m/z 228.9. Internal standard produced a protonated precursor ion $([M+H]^+)$ at m/z 491.5 and a corresponding product ion at m/z 352.0. Detection of pinaverium bromide in human plasma was accurate and precise, with limit of quantitation at 0.5 ng/ml. The method has been successfully applied to bioavailability study of pinaverium bromide tablet in Korean healthy male volunteers. Pharmacokinetic parameters such as $AUC_t,\;C_{max},\;T_{max},\;K_{el}\;and\;t_{1/2}$ were calculated.

당귀(Angelica gigas) 중 Decursin 및 Decursinol Angelate 추출 방법과 HPLC 분석 (HPLC Analysis and Extraction Methods of Decursin and Decursinol Angelate in Angelica gigas Roots)

  • 이장훈;채희정;김동현;이상현;박상용;강영구
    • 생약학회지
    • /
    • 제34권3호통권134호
    • /
    • pp.201-205
    • /
    • 2003
  • This paper is intended as an investigation of the analysis of high-performance liquid chromatography and the method of extraction of decursin and decursinol angelate in Angelica gigas roots. There are three kinds of extraction methods: distilled water, 50% EtOH and 100% EtOH. The condition of HPLC was obtained on a reversed-phase column $(Polarity\;dC_{18},\;4.6{\times}250 mm,\;5\;{\mu}m)$ using a phosphate buffer-acetonitrile-sodium lauryl sulfate as the mobile phase. Under these chromatographic conditions, UV detector was 230 nm, column temperature $30^{\circ}C$ and the speed of a current 1.0 ml/min, respectively. The results of extraction with distilled water, 50% EtOH and 100% EtOH in Angelica gigas roots were as follows. The concentrations of decursin and decursinol angelate were 182 and 153 ppm (distilled water), 3,142 and 2,547 ppm (50% EtOH) and 3,341 and 2,778 ppm (100% EtOH). There were high positive correlations between the concentrations of decursin and EtOH (r=0.8928, p<0.01) and decursinol angelate and EtOH (r=0.9009, p<0.01).

부안산 참굴(Crassostrea gigas) 추출물로부터 피부 상재균에 대한 새로운 항균 펩타이드, cgCAFLP의 탐색 및 정제 (Screening and Purification of a Novel Antibacterial Peptide, cgCAFLP, Against Skin Pathogens from the Extract of the Pacific Oyster Crassostrea gigas from Buan in Korea)

  • 이지은;서정길
    • 한국수산과학회지
    • /
    • 제54권6호
    • /
    • pp.927-937
    • /
    • 2021
  • This study was performed to screen the antimicrobial activities of the extract from the Pacific oyster Crassostrea gigas against skin pathogens and to purify the relevant antibacterial peptide. The acidified extract showed potent antibacterial activities against gram-positive and gram-negative bacteria but showed no activity against Candida albicans and no significant cell toxicity. Among acne-causing pathogens, the acidified extract showed potent antibacterial activity only against Staphylococcus aureus, and its antibacterial activity was completely abolished by treatment with trypsin or chymotrypsin, and was inhibited by salt treatment. The acidified extract showed strong DNA-binding ability but did not show bacterial membrane permeabilizing ability. Based on antimicrobial activity screening and cytotoxic effects, a novel antibacterial peptide was purified from the acidified gill extract using solid-phase extraction, cation-exchange, and reversed-phase HPLC. The resulting peptide had a molecular weight of 4800.8 Da and showed partial sequence homology with the carbonic anhydrase 4 (CA4) protein in the hard-shelled mussel. Overall, we purified a novel antibacterial peptide, named cgCAFLP, which is related to carbonic anhydrase 4 (CA4) protein, against skin pathogens. Our results suggest that the Pacific oyster extract could be used as an additive to control some acne-related skin pathogens (S. aureus).

역상 고성능 액체 크로마토그래피를 이용한 마늘에서 diallyl disulfide의 분석 (Determination of diallyl disulfide in garlic by reversed-phase high performance liquid chromatography)

  • 만효룡;;노경호
    • 분석과학
    • /
    • 제20권5호
    • /
    • pp.442-447
    • /
    • 2007
  • 마늘(Allium sativum L.)의 특성은 organosulfur 화합물이다. 마늘에 포함된 diallyl disulfide(DADS)를 분석하기 위한, 간단하고 신속한 시료준비와 분석방법을 제시하였다. 모든 마늘시료들은 메탄올, 벤젠, 또는 테트라하이드로퓨란과 같은 용매로 추출하여 분석하였다. 실험결과에 의하면, 메탄올로 추출한 시료가 가장 우수하였다. 분석조건으로는 이동상은 메탄올과 물로 구성되고 기울기법을 적용하였다. 분말가루로 된 마늘 1 g에 0.61 mg DADS를 추출하였다. 기존 분석방법에 비해 우수하여 마늘관련 연구에 도움이 될 것이다.

1,1-Diphenyl-2-picrylhydrazyl Radical Scavenging Compounds of Fraxini Cortex

  • Kim, Hyun-Chul;An, Ren-Bo;Jeong, Gil-Saeng;Oh, Seung-Hwan;Kim, Youn-Chul
    • Natural Product Sciences
    • /
    • 제11권3호
    • /
    • pp.150-154
    • /
    • 2005
  • The radical scavenging effect of the MeOH extract of Fraxini Cortex on 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical was examined. The $CH_2Cl_2$-and n-BuOH-soluble fractions of MeOH extract showed the promising DPPH radical scavenging effects, and further purified by silica gel, Sephadex LH-20 column chromatography, and reversed-phase C-18 MPLC to yield five coumarins, esculetin (1), fraxidin (2), fraxetin (3), fraxidin $8-O-{\beta}-D-glucopyranoside$ (fraxin methyl ether) (5), esculin (6), and a secoiridoid oleuropein (4), and a coumarin-secoiridoid escuside (7). Compounds 1, 3, and 4 showed potent DPPH radical scavenging effects, exhibiting $IC_{50}$ values of 14.68, 9.64, and $22.03\;{\mu}M$, respectively. Compounds 6 and 7 also showed moderate effects with $IC_{50}$ values of 147.79 and $72.73\;{\mu}M$, respectively. L-Ascorbic acid was used as a positive control and exhibited the $IC_{50}$ value of $50.31\;{\mu}M$.

Hydrophobic Reagent를 흡착시킨 분리관에서의 양이온 분리 (Separation of Cations on the Hydrophobic Reagent Coated Column)

  • 엄태윤;조기수;김연두
    • 대한화학회지
    • /
    • 제31권4호
    • /
    • pp.328-333
    • /
    • 1987
  • $C_18$ 역상 충전제에 1-eicosylsulfate($C_{20}H_{41}SO_4^-$)를 흡착하는 조건을 조사하였으며 $1.46{\times}10^{-4}M$의 흡착용액(25% 아세토니트릴 수용액) 1.2l를 통과시켰을 때 흡착평형이 일어났다. 이 분리관은 0.05 M ${\alpha}$-HiBA 용리액 10l까지 안정하였으며 Eu, Nd, Ce , La에 대한 분리관효율은 0.15M ${\alpha}$-HiBA 용리액 1.0ml/min에서 약 0.04 mm의 HETP를 나타내었다. 이 흡착분리관으로 희토류 원소 및 전이원소들을 개별 분리하였다.

  • PDF

A New Flavonol Glycoside from Tristemma hirtum (Melastomataceae)

  • Kenfack, Joseph Nandjou;Ponou, Beaudelaire Kemvoufo;Kuhlborn, Jonas;Teponno, Remy Bertrand;Nono, Raymond Ngansop;Fouedjou, Romuald Tematio;Opatz, Till;Park, Hee Juhn;Tapondjou, Leon Azefack
    • Natural Product Sciences
    • /
    • 제24권3호
    • /
    • pp.213-218
    • /
    • 2018
  • Chemical investigation of the plant Tristemma hirtum P. Beauv (Melastomataceae) resulted to the isolation of a new flavonol glycoside named quercetin-7-O-${\alpha}$-D-arabinofuranoside (1), together with nine known compounds including 3'-hexadecanoyl-2'-(9aZ)-tetradecanoyl-glycerol 1'-O-[${\beta}$-D-galactopyranosyl-(1'' ${\rightarrow}$ 6'')-${\alpha}$-D-galactopyranoside] (2), arjunolic acid (3), ${\beta}$-sitosterol-3-O-${\beta}$-D-glucopyranoside (4), terminolic acid (5), quercetin (6), asiatic acid (7), maslinic acid (8), $1{\beta}$-O-galloylpedunculagin (9) and 6-hydroxyapigenin 7-O-${\beta}$-D-glucopyranoside (10) from the methanol extract using normal and reversed phase column chromatography. The structures of these compounds were determined by comprehensive interpretation of their spectral data mainly including 1D- 2D-NMR ($^1H-^1H$ COSY, HSQC, and HMBC) spectroscopic and ESI-TOF-MS mass spectrometric analysis.

인삼속(人蔘屬)과 오가피속(五加皮屬)의 Nucleobases 및 Nucleosides의 분석(分析) (Determination of Nucleobases and Nucleosides in Panax and Acanthopanax genus)

  • 조영현;홍순근;박내정
    • 한국식품영양과학회지
    • /
    • 제12권1호
    • /
    • pp.1-6
    • /
    • 1983
  • 인삼(人蔘)과 오가피중(五加皮中)의 핵산계(核酸系) 성분(成分)을 HPLC로 분리(分離) 정량(定量)하여 다음과 같은 결과를 얻었다. 1. 동일한 원료수삼에서 제조한 백삼(白蔘)과 홍삼(紅蔘)의 핵산유리염기(核酸遊離鹽基)와 nucleoside의 조성이 거의 같았다. 2. 인삼(人蔘)과 오가피(五加皮)중의 nucleosides 함량에서 adenosine, guanosine, cytidine 등이 특징적(特徵的)인 차이(差異)를 나타냈으며 인삼속(人蔘屬)이 약(約) 3배(倍)이상 많게 나타났다. 그러나 tymidine과 inosine은 오가피속(五加皮屬)이 다소 많았다. 3. nucleobase 함량면에서는 인삼(人蔘)이나 오가피간(五加皮間)에 비슷한 함량으로 1~2mg/100g를 함유했다.

  • PDF

Molecular Identification of Four Different α-amylase Inhibitors from Baru (Dipteryx alata) Seeds with Activity Toward Insect Enzymes

  • Bonavides, Krishna B.;Pelegrini, Patricia B.;Laumann, Raul A.;Grossi-De-Sa, Maria F.;Bloch, Carlos Jr.;Melo, Jorge A.T.;Quirino, Betania F.;Noronha, Eliane F.;Franco, Octavio L.
    • BMB Reports
    • /
    • 제40권4호
    • /
    • pp.494-500
    • /
    • 2007
  • The endophytic bruchid pest Callosobruchus maculatus causes severe damage to storage cowpea seeds, leading to economical losses. For this reason the use of $\alpha$-amylase inhibitors to interfere with the pest digestion process has been an interesting alternative to control bruchids. With this aim, $\alpha$-amylase inhibitors from baru seeds (Dipteryx alata) were isolated by affinity chromatographic procedures, causing enhanced inhibition of C. maculatus and Anthonomus grandis $\alpha$-amylases. To attempt further purification, this fraction was applied onto a reversed-phase HPLC column, generating four peaks with remarkable inhibition toward C. maculatus $\alpha$-amylases. SDS-PAGE and MALDI-ToF analysis identified major proteins of approximately 5.0, 11.0, 20.0 and 55 kDa that showed $\alpha$-amylase inhibition. Results of in vivo bioassays using artificial seeds containing 1.0% (w/w) of baru crude extract revealed 40% cowpea weevil larvae mortality. These results provide evidence that several $\alpha$-amylase inhibitors classes, with biotechnological potential, can be isolated from a single plant species.

황련 중 berberine의 추출효율에 관한 연구 (A Study on the Extraction Efficiency of Berberine in Coptidis Rhizoma)

  • 이재성;박호군;우은란;이은주;안덕균;윤원식;신광호
    • 분석과학
    • /
    • 제10권2호
    • /
    • pp.83-90
    • /
    • 1997
  • 본 연구에서는 황련의 지표물질인 berberine의 추출효율을 측정하기 위하여 추출온도, 추출용매, 추출시간 등의 조건 변화에 따른 최적의 추출조건을 찾았다. $60^{\circ}C$에서 2~3시간 환류하였을 때 추출효율이 가장 좋았으며, 추출용매로는 메탄올이나 아세트산을 사용하였을 때 각각 추출효율이 우수하였다. 이온쌍 추출법에서는 사용되는 sodium lauryl sulfate의 첨가 효과는 추출 효율을 오히려 감소시키는 결과를 나타내었다.

  • PDF