• 제목/요약/키워드: Reversed phase $C_{18}$ column

검색결과 151건 처리시간 0.021초

후박나무 잎 Flavonoid 성분의 분석 (Analysis of Flavonoid Components from Machilus thunbergii Leaves)

  • 김성환
    • Journal of Plant Biology
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    • 제36권3호
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    • pp.297-300
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    • 1993
  • Six flavonoid compounds from the ethyl acetate fraction of Machilus thunbergii leaves were identified by HPLC. Separation by reversed phase chromatography on u-Bondapak C18 column was achieved by isocratic elution. The contents of the major flavonoids, guaijaverin and quercitrin were about 0.48% (w/w) and 0.98% (w/w) for the methanol extract, respectively.

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

  • 엄태윤;조기수;김연두
    • 대한화학회지
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    • 제31권4호
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    • pp.328-333
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    • 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.

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달걀 단백질 분석을 위한 HPLC 연구 (HPLC Study for Egg White Analysis)

  • 전영주;이은;김인호
    • KSBB Journal
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    • 제22권2호
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    • pp.119-122
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    • 2007
  • RP-HPLC에서 주요 변수인 이동상의 조성과 컬럼의 종류를 변화시켜 난백 단백질을 실험하였다. C4, C8 C18 컬럼을 비교 실험하여 C18 컬럼에서 가장 많은 피크를 보여 C18 컬럼을 선택하였다. 등용매 용리에서 ACN : water의 조성이 50 : 50에서 가장 많은 피크를 보여 이 결과를 토대로 기울기 용리를 하여 실험하였다. 기울기 용리에서 얻어진 4가지 피크를 확인하기 위하여 단일성분인 lysozyme와 ovalbumin의 체류시간을 측정하여 확인하였고 논문을 통해 2가지 피크를 예측할 수 있었다.

역상 액체 크로마토그래피에 의한 몇가지 금속-Dithiocarbamate 킬레이트의 용리거동 및 동시분석에 관한 연구 (Studies on the Elution Behavior and the Simultaneous Analysis of Some Metal-Dithiocarbamate Chelates by Reversed-Phase High Performance Liquid Chromatography)

  • 이대운;김연제;김현철;이원
    • 대한화학회지
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    • 제32권3호
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    • pp.211-226
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    • 1988
  • 역상 액체 크로마토그래피에 의하여 몇 가지 금속-dithiocarbamate(DTC) 킬레이트의 용리거동을 Novapak $C_{18}${\mu}$-Bondapak $C_{18}$ 분리관을 사용하여 연구하고, 아울러 동시 분리정량에 미치는 pH, 진탕시간, 흐름속도, 추출용매 종류 및 이동상의 세기등 여러가지 인자들의 영향을 조사 검토하였다. 미량 금속-DTC 킬레이트들은 Novapak $C_{18}$ 분리관에서 acetonitrile/methanol/water 또는 acetonitrile/water의 용리액을 사용하여 성공적으로 분리되었다. 모든 금속-DTC 킬레이트의 용매세기 인자는 $0{\leqq}log\;k'{\leqq}1$ 의 범위임을 확인하였고, 회수율을 97.0-106.7 %, coefficient of variation은 0.98-3.41%이었다. 최적 분석 조건에서 합성 시료중에 있는 혼합 금속 이온들은 상대 오차 ${\pm}$6.7 % 이내에서 동시 분리정량이 가능하였다.

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RP-HPLC-PAD를 이용한 갈근(葛根)과 갈근(葛根) 함유 처방의 Puerarin과 Daidzin 분석 (Determination Method of Puerarin and Daidzin from Puerariae Radix by Reversed-Phase HPLC with Pulsed Amperometric Detection)

  • 초진영;권하정;정지선;이제현;홍선표
    • 대한본초학회지
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    • 제23권4호
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    • pp.171-177
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    • 2008
  • Objectives: This study presents a reversed-phase high-performance liquid chromatography- pulsed amperometric detection(RP-HPLC-PAD) method for the determination of puerarin and daidzin in Puerariae Radix extract and Chinese medicinal preparations. Methods: Chromatographic separation was performed using a 10% acetonitrile with a reversed-phase column(Unison UK-C18, $100mm{\times}2.0mm$ I.D.; $3{\mu}m$). The analyses were detected by pulsed amperometric detector(PAD) in alkaline conditions by combining with post-column NaOH solution. Geniposide was used as an internal standard. Results: The limit of detection(S/N=3) and the limit of quantification(S/N=10) were 0.025 ng, 0.075 ng for puerarin, and 0.05 ng, 0.15 ng for daidzin, respectively. The intra- and inter-day precisions(RSDs) were less than 6.5% and average recoveries of puerarin were 99.7-101.3% and those of daidzin were 101.0-102.8%. Conclusions: According to above results, we developed a determination method for puerarin and daidzin in Puerariae Radix with high sensitivity and selectivitely.

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Solid-Phase Extraction of Caffeine and Catechin Compounds from Green Tea by Caffeine Molecular Imprinted Polymer

  • Jin, Yinzhe;Row, Kyung-Ho
    • Bulletin of the Korean Chemical Society
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    • 제28권2호
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    • pp.276-280
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    • 2007
  • In this work, caffeine and some catechin compounds + C, EC, EGC, and EGCG were extracted from green tea by using molecular imprinted polymers (MIP) as sorbent materials in a solid-phase extraction (SPE) process known as MISPE (molecular imprinted solid-phase extraction). For synthesis of MIP, caffeine was employed as the template, MAA as the monomer, EGDMA as the crosslinker, and AIBN as the initiator. A solution of caffeine (0.2 mg/mL in methanol) was utilized in the solid extraction cartridges following loading, washing, and elution procedures with acetonitrile, methanol, and methanol-acetic acid (90/10, %v/v) as the solvents, respectively. This solid-phase extraction protocol was applied for the extraction of caffeine and some catechin compounds from green tea. A comparison was made between the results obtained with the MIP cartridges and a traditional C18 reversed-phase cartridge. It was thereupon found that the recovery of caffeine by the MIPbased sorbent used in this work was almost two and four times greater than that by a commercially available C18 material. A quantitative analysis was conducted by high performance liquid chromatography (HPLC) using a C18 column (5 μm, 250 × 4.6 mm) with methanol/water (40/60, %v/v) as the mobile phase at a flow rate of 0.5 mL/min.

역상 고속 액체크로마토그래피를 이용한 인삼 사포닌의 분석 (Determination of Ginseng Saponins by Reversed-Phase High Performance Liquid Chromatography)

  • 정승일;김천석;이노운;최강주;이용구;김일광
    • 분석과학
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    • 제11권6호
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    • pp.436-439
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    • 1998
  • 인삼 사포닌을 역상 고속 액체크로마토그래피 방법을 이용하여 여러 종류의 컬럼으로 분석하였다. 최적 조건은 Novapak $C_{18}$ ODS 역상 칼럼($3.9mm{\times}150mm$, $5{\mu}m$), $CH_3CN/H_2O$ 이성분 이동상 용액과 기울기 제어장치, 그리고 1.5 mL/min의 용매 흐름속도였으며, UV 검출기(203 nm)를 사용하였다. 인삼의 주성분인 ginsenoside $Rb_1$, $Rb_2$, Rc, Rd, Re, Rf 그리고 $Rg_1$ 7종을 50분 안에 양호하게 분리하였다. 각 성분에 대한 검량선은 직선성이 좋았으며, 회귀계수는 0.98~0.99이었다.

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Effects of Column Length and Particle Diameter on Phospholipid Analysis by Nanoflow Liquid Chromatography-Electrospray Ionization-Mass Spectrometry

  • Lee, Ju-Yong;Lim, Sang-Soo;Moon, Myeong-Hee
    • Mass Spectrometry Letters
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    • 제2권3호
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    • pp.65-68
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    • 2011
  • The effects of column length and particle size on the efficiency of separation and characterization of phospholipids (PLs) are investigated using nanoflow liquid chromatography-electrospray ionization-tandem mass spectrometry (nLC-ESI-MS-MS). Since PLs are associated with cell proliferation, apoptosis, and signal transduction, it is of increasing interests in lipidomics to establish reliable analytical methods for the qualitative and quantitative profiling of PLs related to biomarker development in adult diseases. Due to the complexity of PLs, the preliminary separation of PLs is necessary prior to MS analysis. In this study, length of capillary column and the particle size of reversed phase ($C_{18}$) packing materials are varied to find a reliable condition for the high speed and high resolution separation using 8 PL standard mixtures. From experiments, it was found that a capillary column of nLC-ESI-MS-MS analysis for PL mixtures can be minimized to a 5 cm long pulled tip column packed with 3 ${\mu}m$ $C_{18}$ particles without losing resolution.

역상 액체 크로마토그래피에 의한 금속-2-hydroxy-arylazopyrazolone 유도체 킬레이트의 용리거동에 관한 연구 (II) (The Elution Behaviors of Some Metal-2-Hydroxy-arylazopyrazolone Chelates by Reversed Phase Liquid Chromatography (II))

  • 이원;김인환;강창희;김은경
    • 분석과학
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    • 제7권3호
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    • pp.379-386
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    • 1994
  • Ni(II), Cu(II), Co(III) 및 Cr(III) 이온과 2-hydroxy-arylazopyrazolone 유도체들 사이에 형성하는 킬레이트들에 대한 역상 액체 크로마토그래피에서의 용리 메카니즘을 열역학적인 접근방법으로 고찰하였다. van't Hoff plot에 의해 온도와 용량인자(k')와의 상관관계를 조사한 결과 온도와 용량인자와의 관계는 양호한 직선성을 나타냈으며, 온도 변화와 무관한 동일한 메카니즘에 의해 분리됨을 알 수 있었다. van't Hoff plot으로부터 엔탈피$({\Delta}H)^{\circ}$, 엔트로피$({\Delta}S)^{\circ}$를 구하고, 엔탈피와 용량인자와의 상관관계를 조사한 결과 [pm(2-OH)(5-Cl)PaPz](r=0.787)을 제외한 대부분이 킬레이트들은 비교적 좋은 직선성(r=0.980~0.999)을 보였고, 보정온도(${\beta}$) 역시 일정한 값을 나타내었다. 이것은 금속-2-hydroxy-arylazopyrazolone 킬레이트와 정지상($C_{18}$)과의 상호작용이 등평형 거동을 하고 있음을 의미한다. 또한 엔탈피와 용량인자와의 상관관계로부터 구한 보정온도는 374.63~806.9k 범위의 값을 나타냈고, 이들 결과로부터 역상 액체 크로마토그래피에서 금속 킬레이트들의 머무름 메카니즘은 소수성 효과에 기인하고 있음을 확인할 수 있었다.

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Simultaneous Determination of Cysteamine and Cystamine in Cosmetics by Ion-Pairing Reversed-Phase High-Performance Liquid Chromatography

  • Kim, Yejin;Na, Dong Hee
    • Toxicological Research
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    • 제35권2호
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    • pp.161-165
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    • 2019
  • Cysteamine has been used in cosmetics as an antioxidant, a hair straightening agent, and a hair waving agent. However, recent studies indicate that cysteamine can act as an allergen to hairdressers. The objective of this study was to develop and validate a simple and effective reversed-phase high-performance liquid chromatography (RP-HPLC) method for the measurement of cysteamine and its dimer, cystamine. Sodium 1-heptanesulfonate (NaHpSO) was used as an ion-pairing agent to improve chromatographic performance. Separation was performed on a Gemini C18 column ($250mm{\times}4.6mm$, $5{\mu}m$ particle size) using a mobile phase composed of 85:15 (v/v) 4 mM NaHpSO in 0.1% phosphoric acid:acetonitrile. UV absorbance was monitored at 215 nm. The RP-HPLC method developed in this study was validated for specificity, linearity, limit of detection, limit of quantitation, precision, accuracy, and recovery. Cysteamine and cystamine were chromatographically resolved from other reducing agents such as thioglycolic acid and cysteine. Extraction using water and chloroform resulted in the recovery for cysteamine and cystamine ranging from 100.2-102.7% and 90.6-98.7%, respectively. This validated RP-HPLC method would be useful for quality control and monitoring of cysteamine and cystamine in cosmetics.