• 제목/요약/키워드: Reversed-Phase HPLC

검색결과 357건 처리시간 0.034초

2-Bromoacetyltriphenylene 유도체화제를 이용한 카르복실기 함유성분의 분석법 (III) - 감초중 glycyrrhetinic acid의 HPLC에 의한 분리정량 (HPLC Determination of Carboxyl Grop usinf 2-Bromoacetyltriphenylene as Pre-labeling Reagent (III) - Separative determination of glycyrrhetinic acid contained in licorice power)

  • 정해수;예덕천;김박광;박만기;이왕규
    • 약학회지
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    • 제31권5호
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    • pp.315-321
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    • 1987
  • A high performance liquid chromatographic method was developed for the determination of glycyrrhetinic acid contained in licorice powder. Glycyrrhetinic acid which is hydrolysate of glycyrrhizin extracted from licorice powder, was determined with good result by HPLC using 2-bromoacetyltriphenylene labeling reagent. The glycyrrhetinic acids were labeled with 2-bromoacetyltriphenylene in acetonitrile using 18-crown-6-ether and KOH as a catalyst. Derivatized glycyrrhetinic acids were separated from the extracted licorice powder on a reversed-phase column (chemopak $C_{18}$) using 100% acetonitrile as a mobile phase and monitored by an UV-detector at 268nm. Linearity of calibration curve was obtained between 5 ng and 20 ng, and the lower limit of detection was 2 ng. The recovery of glycyrrhetinic acid to licorice powder was about 99.3%. This method was sensitive, reliable and useful for, determination of glycyrrhetinic acid.

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역상 HPLC에 의한 polysorbates의 산화에틸렌(EO) 분리 및 정량분석 (Determination and Ethylene Oxide(EO) Separation of Polysorbates by RP-HPLC)

  • 이용화
    • 한국응용과학기술학회지
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    • 제29권4호
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    • pp.585-593
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    • 2012
  • 역상 HPLC에 의한 polysorbate 20, polysorbate 40, polysorbate 60, polysorbate 80의 ethylene oxide(EO)분리 및 간편하고 빠른 정량분석 방법을 개발하였다. 분석조건으로 분리관은 YMC Pack Ph ($250mm{\times}4.6mm$ i.d., $5{\mu}m$) 과 Phenomenex C4 ($250mm{\times}4.6mm$ i.d., $5{\mu}m$)을 사용하였고, 검출기는 ELSD를 사용하였으며, 이동상은 water/acetonitrile의 기울기 용리에 의해 분석되었다. 이때 검량선의 상관계수($r^2$)는 $180.2{\sim}980.5{\mu}g/mL$ 농도 범위에서 0.997이상 이었고, 검출한계, 정밀성이 우수하였다. 이 방법은 olysorbates의 산화에틸렌 분리분석 및 간편하고 빠르게 정량분석 가능함을 보여 주었다.

On-line Trace Enrichment for the Determination of Insulin in Biological Samples Using Reversed-Phase High Performance Liquid Chromatography with Column Switching

  • Lee, Jung-Sook;Lee, Heeyong;Lee, Hye-Suk;Lee, Kang-Choon
    • Archives of Pharmacal Research
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    • 제17권5호
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    • pp.360-363
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    • 1994
  • Column--swtiching technique with a reversed-phase high performance liquid chromatographic method has been developed for the routine analysis of radioiodinated insulin and its degadation products in biological fluids. The diluted biological samples were loaded onto a precolumn packed with LiChrosorb RP-8 $(25-40{\;}{\mu}m)$ using 0.1% trifuoroacetic acid (TFA) in water as a washing solvent. After valve switching, the concentrated insulins were eluted in the back-flush mode and separated by a W-Porex $C_{18}$ column with a gradient of 0.1% TFA in water and 0.1% TFA in acetonitrile as the mobile phase. The method showed good precision, accuracy and speed with the detection limit of 20 pg/ml. Total analysis time per sample was about 40 min and the coefficients of variation were less than 8, 2%.

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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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Simultaneous Determination of Tin, Nickel, Lead, Cadmium and Mercury in Cigarette Material by Solid Phase Extraction and HPLC

  • Hu, Qun;Yang, Guangyu;Ma, Jing;Liu, Jikai
    • Bulletin of the Korean Chemical Society
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    • 제24권10호
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    • pp.1433-1436
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    • 2003
  • A new method for the simultaneous determination of heavy metal ions in cigarette material by microwave digestion and reversed-phase high-performance liquid chromatography (RP-HPLC) has been developed. The cigarette material was digested by microwave digestion. Lead, cadmium, mercury, nickel and tin ions in the digested samples were pre-column derivatized with tetra-(2-chlorophenyl)-porphyrin ($T_2$-CPP) to form color chelates, which were then enriched by solid phase extraction with a $C_{18}$ cartridge. The chelates were separated on a Waters Xterra$^{TM}RP_{18}$ column by gradient elution with methanol (containing 0.05 mol/L pyrrolidine-aceticacid buffer salt, pH = 10.0) and acetone (containin0.05 mol/L pyrrolidine-acetic acid buffer salt, pH = 10.0)as mobile phase at a flow rate of 0.5mL/min and analyzed with a photodiode array detector from 350-600 nm. The detection limits of lead, cadmium, mercury, nickel and tin were 4,3,3,8 and 5 ng/L, respectively, in the original samples. This method was afforded good results.

Sasa borealis의 Diastereomeric 성분들의 역상 고속액체크로마토그래프 분석방법 (Reverse-Phase HPLC Method for Identification of Diastereomeric Constituents from Sasa borealis)

  • 정연희;이준;권영주;서은경
    • 약학회지
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    • 제50권1호
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    • pp.21-25
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    • 2006
  • Reiterated normal-phase column chromatography lead to the isolation and purification of six known compounds but for the first time from the whole plant of Sasa borealis (Hack.) Makino (Gramineae): tricin 4'-O-(erythro-${\beta}$-guaia-cylglyceryl) ether (1), tricin 4'-O-(threo-${\beta}$-guaiacylglyceryl) ether (2), tricin 4'-O-[erythro-${\beta}$-guaiacyl-(9'-O-acetyl)-glyceryl] ether (3), tricin 4'-O-[threo-${\beta}$-guaiacyl-(9'-O-acetyl)-glyceryl] ether (4), (-)-pinoresinol (5), and vanillin (6). The structures of the compounds (1-6) were established based on interpretation of high resolution NMR (COSY, HSQC, HMBC, and NOESY) spectral data. In particular, compounds 1 and 3 were diastereomers of compounds 2 and 4, respectively. These two sets of diastereomers were able to be simultaneously identified and quantified by a gradient reversed-phase HPLC method with UV photodiode array, This sensitive HPLC method is noteworthy as a simultaneous separation and identification method to test the extract of the family Gramineae which contains these compounds.

Van der Waals Volume을 이용한 역상 컬럼에서의 유기화합물들의 용출거동 (Retention Behavior of Organic Compounds on Reversed-Phase Column expected by Van der Waals Volume)

  • 박운규;이용문;문동철;강종성
    • 분석과학
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    • 제6권4호
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    • pp.383-390
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    • 1993
  • 지방족 카르복실산류, 방향족화합물류 및 알킬벤젠류에 대하여 역상 HPLC에서의 용출예측 방법을 검토하였다. 용출 파라미터로서 분자 크기를 나타내는 Van der Waasls 부피와 log k'와의 상관성을 검토한 결과, 양호한 직선성을 얻을 수 있었다. 용리액의 조성을 변화시키면서 또는 분리컬럼 온도를 변화시키면서 지방족 카르복실산류, 방향족화합물류 및 알킬벤젠류에 대하여 검토한 결과, acetonitrile이 log k'와 Van der Waals 부피와의 상관성이 가장 좋았다. 본 방법을 이용하여 역상 HPLC system에서 Van der Waasls 부피가 40~250 사이의 유기화합물들의 용출을 예측할 수 있었다. 각 용매의 용출력 세기는 methanol

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RP-HPLC를 이용한 백소엽(白蘇葉)과 자소엽(紫蘇葉)의 카페익산과 로즈마린산 분석 (Determination of Rosmarinic Acid and Caffeic Acid from Perilla frutescens var. japonica and var. acuta by Reversed-Phase HPLC)

  • 김병연;정지선;권하정;이제현;홍선표
    • 대한본초학회지
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    • 제23권3호
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    • pp.67-72
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    • 2008
  • Objectives : This study presents a high performance liquid chromatography methods for the quantitative and qualitative analysis of rosmarinic acid (RA) and caffeic acid (CA) in Perilla frutescens var. japonica and var. acuta. Methods : Chromatographic separation was performed using a mixture of methanol, water and formic acid (35 : 64.2 : 0.8) with a reversed-phase column (Gemini C18, 4.6 ${\times}$ 150 mm, 3 ${\mu}m$). The analyses were detected at UV (280 nm). Results : The samples were extracted with 50% EtOH under reflux for 1 h, and simultaneous determination for RA and CA in hyang-so-san and haeng-so-san was possible without interference peaks Conclusions : According the results, we developed a determination method for RA and CA in Perillae Folium. Owing to Perilla frutescens var. japonica and var. acuta did not show significant difference in contents of RA and CA, both Perilla frutescens could be available as herbal medicine.

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해산물 시료에서 solid-phase extraction 및 HPLC-ICP/MS를 이용한 셀레늄 화학종의 정량분석 (Quantitative analysis of selenium species in sea food using solid phase extraction and HPLC-ICP/MS)

  • 김은주;주민규;권효식;박용남
    • 분석과학
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    • 제26권5호
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    • pp.307-314
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    • 2013
  • 셀레늄은 다양한 화학종으로 존재하며 그 농도와 형태에 따라 활성도나 생물학적 이용도가 달라지므로 식품에 대한 셀레늄 화학종의 정확한 분리 및 정량이 필요하다. 본 연구에서는 역상 (RP; reversed phase) 고성능 액체 크로마토그래피 (HPLC; high performance liquid chromatography)와 유도결합 플라즈마 (ICP; inductively coupled plasma) 질량분석법 (MS; mass spectrometry)을 사용하여 해산물 시료 중 셀레늄 화학종을 분리 검출 한 뒤에 후 컬럼 동위원소희석법 (post column isotope dilution)으로 정확히 정량 하였다. 시료 중 $^{80}Se$의 간섭요인인 $^{79}Br$을 제거하기 위해 고체상 추출법을 사용하여 대부분의 $^{79}Br$을 제거하였고 남아있는 $^{79}Br$은 수학적 보정식을 이용하여 보정해주었다. CRM (certified reference material) DOLT-4를 사용하여 셀레늄의 총량을 분석한 결과는 인증치와 잘 일치하였지만 각 화학종에 대한 정보는 비교할 수 없었다. 한국인 식탁에 오르는 대표적인 해산물 시료인 갈치, 삼치, 오징어, 등을 분석한 결과, 주된 셀레늄 화학종은 SeCys (selenocysteine)와 SeMet (selenomethionine)이었으며 각각은 0-661.6 mg/kg and 137.3-462.7 mg/kg의 농도로 존재함 을 알 수 있었다.