• 제목/요약/키워드: ultra-performance liquid chromatography (UPLC)

검색결과 93건 처리시간 0.03초

역상 초고속액체크로마토그라피에 의한 gemcitabine의 빠른 농도 분석법 (The Rapid Determination of Gemcitabine by Reversed-phase Ultra-Performance Liquid Chromatography)

  • 박대진;김우미
    • 생명과학회지
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    • 제19권12호
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    • pp.1698-1704
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    • 2009
  • Gemcitabine은 다양한 고형암 치료에 사용되는 항암제이다. 혈장내에서 cytidine deaminase에 의해 빠르게 대사되며, 친수성 성질로 인해 역상 액체크로마토그라피(reversed-phase liquid chromatography)를 이용한 농도 분석이 어렵다. 본 연구에서는 역상칼럼(reversed-phase column)을 이용한 초고속 액체크로마토그라피(ultra-performance liquid chromatography, UPLC) 방법에 의해 빠르고 정확한 속력(velocity)과 최고효능(peak efficiency)를 갖춘 분석법을 개발하고자 하였다. Gemcitabine과 2'-deoxycytidine의 머무름 시간(retension time)은 293 nm에서 각각 3.2분과 2.1분이었다. 검량선의 직선성 검정은 $0.1{\sim}20{\mu}g/ml$의 농도범위에서 높은 직선성을 나타내었다($r^2$>0.999). 일내(intra-day) 변이게수(coefficients of variation)와 일간(inter-day) 변이게수는 모두 10% 이하였다. 정확성(accuracy) 검정을 위한 일내 및 일간 평균농도 측정치가 97.3~113.5% 범위로 나타났다. 이러한 결과를 토대로, gemcitabine 농도를 측정하기 위한 새로운 분석법으로 빠르고 정확한 역상 UPLC 방법을 제안하고자 한다.

Sensitive determination of pendimethalin and dinoseb in environmental water by ultra performance liquid chromatography-tandem mass spectrometry

  • Lim, Hyun-Hee;Park, Tae-Jin;Lee, Soo-Hyung;Shin, Ho-Sang
    • 분석과학
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    • 제30권4호
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    • pp.194-204
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    • 2017
  • Direct injection (DI) and solid phase extraction (SPE) methods for the simultaneous determination of pendimethalin (PDM) and dinoseb (DNS) in environmental water have been optimized using the ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method. The limits of quantification (LOQs) of PDM and DNS were $0.01{\mu}g/L$ using the DI method and $0.0001-0.0002{\mu}g/L$ using the SPE method. The precision by SPE UPLC-MS/MS was less than 11 % for intra-day and inter-day analyses. When the proposed SPE method was used to analyze two analytes in environmental water, PDM was detected in a concentration range of $0.0002-0.011{\mu}g/L$ in 31 samples of the 114 surface water samples, and DNS was detected in a concentration range of $0.0005-0.045{\mu}g/L$ in 17 samples of the 114 surface water samples analyzed. When the DI method was used to analyze target compounds in the same samples, the detected concentrations of the two analytes were within 21% in samples with concentrations above $0.01{\mu}g/L$. The DI UPLC-MS/MS method can thus be used for the routine monitoring of PDM and DNS in environmental water, and the SPE LC-MS/MS method can be used for the determination of the ultra-trace PDM and DNS residues in environmental water.

Quantitative Analysis of Twelve Marker Compounds in Palmijihwang-hwan using Ultra-Performance Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Natural Product Sciences
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    • 제20권3호
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    • pp.182-190
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    • 2014
  • An ultra-performance liquid chromatography (UPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry (MS) method was established for quantitative analysis of twelve components, allantoin (1), morroniside (2), 5-hydroxymethyl-2-furfural (5-HMF) (3), loganin (4), coumarin (5), cinnamic acid (6), mesaconitine (7), cinnamaldehyde (8), hypaconitine (9), aconitine (10), alisol B (11), and alisol B acetate (12) in a Palmijihwang-hwan decoction. The twelve constituents were separated on a UPLC BEH C18 column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $40^{\circ}C$ by gradient elution with 0.1% (v/v) formic acid in water and acetonitrile as the mobile phase. The flow rate was 0.3 mL/min and the injection volume was $2.0{\mu}L$. Calibration curves of all compounds were acquired with values of the correlation coefficient ${\geq}0.99$ within the test ranges. The limits of detection and quantification for all analytes were 0.01 - 4.53 ng/mL and 0.03 - 13.60 ng/mL, respectively. The concentrations of the compounds 1 - 9 and 12 were 72.83, 4389.00, 4859.00, 3155.17, 223.67, 33.50, 1.97, 518.00, 2.25, and $25.00{\mu}g/g$, respectively. However, compounds 10 and 11 were not detected.

꾸지뽕나무 열매 isoflavonoid 화합물에 대한 정량분석법 개발 (Development of Quantitative Analytical Method for Isoflavonoid Compounds from Fruits of Cudrania Tricuspidata)

  • 윤순영;김석주;심수진;이학주
    • Journal of the Korean Wood Science and Technology
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    • 제44권3호
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    • pp.337-349
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    • 2016
  • 본 연구는 꾸지뽕나무 열매에서 분리 및 정제한 isoflavonoid 성분에 대하여 Ultra Performance Liquid Chromatography(UPLC)을 이용하여 분석법을 개발하고 검증하고자 하였다. 꾸지뽕나무 열매를 methanol로 추출하여 n-hexane, ethyl acetate, 물 순으로 분액 후, ethyl acetate 추출물을 silica gel 컬럼과 sephadex LH-20 컬럼을 사용하여 4종의 isoflavonoid들을 분리하였다. 분리한 4종의 isoflavonoid들은 기기분석(UV-Vis spectroscopy, ESI-MS, $^1H\;NMR$, $^{13}C\;NMR$)을 통하여 alpinumisoflavone, 6,8-diprenyl orobol, 6,8-diprenyl genistein, 4'-O-methylalpinumisoflavone으로 확인 및 동정하였다. 이 성분들을 2% acetic acid 용액(용매 A)과 2% acetic acid가 함유된 MeOH 용액(용매 B)을 기울기 이동상으로 하여 $C_{18}$ 컬럼이 장착된 UPLC로 분석하였다. 분석 조건은 ICH (International Conference on Harmonisation) 가이드라인에 기술된 선택성, 직선성, 정량한계, 검출한계, 정확성 및 정밀성을 측정하여 분석법의 타당성을 검증하였다. 또한 검증한 분석방법을 이용하여 꾸지뽕나무 열매의 채취시기별 함량을 조사하였다. 그 결과, 미숙과는 7월과 8월에 각 성분의 함량이 증가하였다가 9월에는 감소하였고, 성숙과의 경우 9월 미숙과 보다 각 성분들이 전반적으로 많이 함유되어 있었다.

UPLC-ESI-MS/MS를 이용한 온경탕 중 25종 성분의 함량분석 (Quantification of the 25 Components in Onkyung-Tang by Ultra Performance Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry)

  • 서창섭;신현규
    • 생약학회지
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    • 제47권1호
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    • pp.92-101
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    • 2016
  • In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous determination of the 25 marker components, including chlorogenic acid, gallic acid, oxypaeoniflorin, homogentisic acid, methyl gallate, caffeic acid, 3,4-dihydroxybenzaldehyde, paeoniflorin, albiflorin, liquiritin, nodakenin, ferulic acid, ginsenoside Rg1, liquiritigenin, coumarin, cinnamic acid, benzoylpaeoniflorin, ginsenoside Rb1, cinnamaldehyde, paeonol, glycyrrhizin, 6-gingerol, evodiamine, rutecarpine, and spicatoside A in traditional Korean formula, Onkyung-tang. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was carried out using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization (ESI) source in the positive and negative modes. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$, respectively. The correlation coefficient of all analytes in the test ranges was greater than 0.98. The limits of detection and quantification values of the 25 marker compounds were in the ranges 0.03-19.43 and 0.09-58.29 ng/mL, respectively. As a result, methyl gallate, 3,4-dihydroxybenzaldehyde, evodiamine, and rutecarpine were not detected in this sample and the concentrations of the 21 compounds except for the above 4 compounds were $33.09-3,496.32{\mu}g/g$ in Onkyung-tang decoction. Among these compounds, paeonol was detected at the highest amount as a $3,496.32{\mu}g/g$.

UPLC를 활용한 데리스 추출물 함유 유기농자재 중 Rotenone과 Deguelin 정량분석 (Quantitative Analysis of Rotenone and Deguelin in Biopesticides Containing Derris Extract by Ultra performance Liquid Chromatography)

  • 임성진;김진효;최근형;박병준
    • 한국환경농학회지
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    • 제34권1호
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    • pp.52-56
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    • 2015
  • BACKGROUND: Three commercial biopesticides containing derris extract, which is permitted as a commercial biopesticide substances by the Environmentally-friendly Agriculture Promotion Act, have been marketed in Korea. But, the quantitative analytical method of active substances for crop protection in biopesticides containing derris extract has not known. METHODS AND RESULTS: Solid phase extraction (SPE) cartridge clean-up method for the quantitative analysis of rotenone and deguelin in biopesticides containing derris extract was developed and validated by ultra-performance liquid chromatography (UPLC). The clean-up method was established using hydrophilic lipophilic balance (HLB) SPE cartridges for the bioactive substances in biopesticides containing derris extract, and the eluate was analyzed to quantify the rotenone and deguelin by the UPLC. LOQ and recovery rates of rotenone and deguelin were 0.085 and 0.044 mg/L, 95.7 and 93.3%, respectively. The content of rotenone and deguelin in three biopesticides containing derris extract were analyzed by the developed method, the results showed 0.001-0.236 and

Method validation for quantitative analyzing aflatoxin productivity in Aspergillus sp. isolated from soybean paste

  • SeongEui Yoo;WooSoo Jeong;Soo-Hwan Yeo;So-Young Kim
    • 한국식품저장유통학회지
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    • 제30권1호
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    • pp.28-41
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    • 2023
  • Non-aflatoxigenic Aspergillus oryzae and aflatoxigenic A. flavus cannot be clearly identified by partial sequencing of the internal transcribed spacer (ITS) and 18S ribosomal ribonucleic acid (18S rRNA) regions. This study aimed to compare the accuracy among three aflatoxin detection methods using ultra-performance liquid chromatography (UPLC), high-performance liquid chromatography (HPLC), and an enzyme-linked immunosorbent assay (ELISA) kit and to select the non-aflatoxigenic Aspergillus sp. isolated from soybean paste. All analytical methods were suitable according to the international standards of Codex Alimentarius FAO-WHO (CODEX) or the Ministry of Food and Drug Safety (MFDS). UPLC exhibited the best of limit of detection (LOD) and limit of quantification (LOQ). Based on UPLC, HPLC, and the ELISA kit assay, the P5 and P7 strains isolated from soybean paste had 1,663.49, 1,468.12, and >20 ㎍/kg and 1,470.08, 1,056.73, and >20 ㎍/kg, respectively, detected and re-identified as A. flavus. In contrast, the P3 and P4 strains (A. oryzae), which were detected below the MFDS standards in all assays, were confirmed as non-aflatoxigenic fungi. Among the methods evaluated for quantitative analysis of aflatoxin, UPLC and HPLC are superior in terms of accuracy, and the ELISA kit rapidly detects low concentrations of aflatoxin. Furthermore, this study demonstrates that any Aspergillus sp. isolated for use as a fermentation starter should be analyzed for potential aflatoxin production using UPLC and HPLC for accurate quantitative analysis or ELISA for the rapid detection of low-level concentrations of aflatoxin.

Qualitative and Quantitative Analysis of Thirteen Marker Components in Traditional Korean Formula, Samryeongbaekchul-san using an Ultra-Performance Liquid Chromatography Equipped with Electrospray Ionization Tandem Mass Spectrometry

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Natural Product Sciences
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    • 제22권2호
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    • pp.93-101
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    • 2016
  • For efficient quality control of the Samryeongbaekchul-san decoction, a powerful and accurate an ultra-performance liquid chromatography (UPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry (MS) method was developed for quantitative analysis of the thirteen constituents: allantoin (1), spinosin (2), liquiritin (3), ginsenoside Rg1 (4), liquiritigenin (5), platycodin D2 (6), platycodin D (7), ginsenoside Rb1 (8), glycyrrhizin (9), 6-gingerol (10), atractylenolide III (11), atractylenolide II (12), and atractylenolide I (13). Separation of the compounds 1 - 13 was performed on a UPLC BEH $C_{18}$ column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $40^{\circ}C$ with a gradient solvent system of 0.1% (v/v) formic acid aqueous-acetonitrile. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$. Calibration curves of all compounds were showed good linearity with values of the correlation coefficient ${\geq}0.9920$ within the test ranges. The values of limits of detection and quantification for all analytes were 0.04 - 4.53 ng/mL and 0.13 - 13.60 ng/mL. The result of an experiment, compounds 2, 6, 12, and 13 were not detected while compounds 1, 3 - 5, and 7 - 11 were detected with 1,570.42, 5,239.85, 299.35, 318.88, 562.27, 340.87, 12,253.69, 73.80, and $115.01{\mu}g/g$, respectively.

UPLC-MS/MS를 이용한 산천목 중 10종 성분의 함량 분석 (Quantitative Analysis of the Ten Phytochmicals in Acer tegmentosum Maxim by UPLC-MS/MS)

  • 황윤환;이위;양혜진;마진열
    • 생약학회지
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    • 제49권1호
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    • pp.70-75
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    • 2018
  • Acer tegmentosum Maxim (ATM) has been used to treat hepatic disorders in traditional oriental medicine. However, there is little information about phytochemical constituents for quality control of ATM. In this study, we developed and established a simultaneous analytical method of the 10 marker compounds (three coumarins, 3 flavonoids, 1 lignan, 3 phenolics) in ATM using ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS). Chromatographic separation of ten target analytes was achieved with a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$), using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. Identifications and quantitation of all analytes were performed using a Q-Exactive UPLC-MS/MS system. Correlation coefficients of the calibration curve for all analytes were ${\geq}0.9986$. The values of limits of detection and quantification of all analytes were 0.5-10.0 and 5.0-50.0 ng/mL, respectively. The established UPLC-MS/MS method successfully identified all target analytes in ATM, and the phytochemicals were 0.01-67.98 mg/g in its lyophilized water extract.

Metabolomics Approach for Classification of Medicinal Plants

  • Lee, Dong-Ho
    • 한국자원식물학회:학술대회논문집
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    • 한국자원식물학회 2010년도 정기총회 및 춘계학술발표회
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    • pp.5-5
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    • 2010
  • Selection of specific medicinal sources as well as bioactive compounds is important for the preparation of medicine and related products with good quality. It is necessary to pay close attention for choosing correct medicinal sources, particularly in case of medicinal plants, because of their diversity, which can affect the quality and efficacy of medicine. Discrimination of plants based on morphological or genetic characteristics has been used as a conventional classification method of pharmaceutical sources so far; however, more need demands more general methods for accurate quality assessment of medicinal plants. In this study, ultra performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF MS) technique applied to this metabolic profiling is a powerful tool due to its higher sensitivity, resolution, and speed compared to conventional HPLC technique. The metabolite profiling of several medicinal plants including Panax ginseng was carried out using UPLC/Q-TOF MS and total metabolites were then subsequently applied to various statistical tools to compare the patterns. The developed metabolomics tool with UPLC/Q-TOF MS successfully identified and classified the samples tested according to their origins.

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