• 제목/요약/키워드: UPLC-MS/MS

검색결과 135건 처리시간 0.025초

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.

Rapid Screening of Phospholipid Biomarker Candidates from Prostate Cancer Urine Samples by Multiple Reaction Monitoring of UPLC-ESI-MS/MS and Statistical Approaches

  • Lim, Sangsoo;Bang, Dae Young;Rha, Koon Ho;Moon, Myeong Hee
    • Bulletin of the Korean Chemical Society
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    • 제35권4호
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    • pp.1133-1138
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    • 2014
  • Ultrahigh performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI- MS/MS) provides a high-speed method to screen a large number of samples for small molecules with specific properties. In this study, UPLC-ESI-MS/MS with multiple reaction monitoring (MRM) was employed to screen urinary phospholipid (PL) content for biomarkers of prostate cancer. From lists of urinary PLs structurally identified using nanoflow LC-ESI-MS/MS, 52 PL species were selected for quantitative analysis in urine samples between 22 cancer-free urologic patients as controls and 45 prostate cancer patients. Statistical treatment of data by receiver operating characteristic (ROC) analysis yielded 14 PL species that differed significantly in relative concentrations (area under curve (AUC) > 0.8) between the two groups. Among PLs present at higher levels in prostate cancer urine, phosphatidylcholines (PCs) and phosphatidylinositols (PIs) constituted the major head group PLs (3 PCs and 7 PIs). For technical reasons, PL species of low abundance may be underrepresented in data from UPLC-ESI-MS/MS performed in MRM mode. However, the proposed method enables the rapid screening of large numbers of plasma or urine samples in the search for biomarkers of human disease.

파브리병의 신속한 진단을 위한 소변 중 Globotriaosylsphingosine의 UPLC-ESI-MS/MS 분석법 (Quantification of Globotriaosylsphingosine in Urine using UPLC-ESI-MS/MS; Application for Screening Fabry Disease)

  • 윤혜란
    • 약학회지
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    • 제60권1호
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    • pp.15-20
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    • 2016
  • Globotriaosylsphingosine (lyso Gb3) is considered as one of the biomarkers for Fabry disease. A rapid and simple UPLC-MS/MS method was developed for the determination of reliable biomarker, lyso Gb3. Total analytical procedure takes only 15 min including sample preparation and MS/MS analysis. Limit of detection was 0.85 ng/ml (S/N=3). The calibration curve was linear over the range of 2.0~400.0 ng/ml ($R^2=0.9999$). Inter-day and intra-day assay accuracy were 93.4~100.6% (RSD, 0.6~6.0%) and 97.5~100.7% (RSD, 3.6~5.2%). Absolute recoveries of 97.6~98.6 showed excellence of a new analytical method. The method was applied to human and mice urines, proved the suitability for the quantification of lyso-Gb3 for screening, diagnosis and therapeutic monitoring of Fabry disease patients.

UPLC-MS/MS를 이용한 배추와 배추김치의 글루코시놀레이트 및 대사체 분석 (Analysis of glucosinolates and their metabolites from napa cabbage (Brassica rapa subsp. Pekinensis) and napa cabbage kimchi using UPLC-MS/MS)

  • 김재철;박효순;황금택;문보경;김선아
    • 한국식품과학회지
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    • 제52권6호
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    • pp.587-594
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    • 2020
  • 본 연구에서는 부위별 배추와 배추김치에 함유되어 있는 글루코시놀레이트류의 조성을 UPLC-MS/MS를 이용하여 탐색하고, 인돌류 대사체를 MS/MS를 이용하여 분석한 결과, 글루코시놀레이트류는 음이온 모드([M-H]-)에서 검출되었으며, glucobrassicanapin (m/z 386), glucoalyssin (m/z 450), glucobrassicin (m/z 447), 4-methoxyglucobrassicin (m/z 477), neoglucobrassicin (m/z 477)는 MS scan 모드에서, gluconapin (m/z 372→97), progoitrin (m/z 388→97), glucoiberin (m/z 422→97), 4-methoxyglucobrassicin (m/z 477→97), neoglucobrassicin (m/z 477→447)는 MS/MS MRM 모드에서 검출되었다. Glucobrassicin과 같은 인돌기 함유 글루코시놀레이트류들이 대사되어 생성되는 인돌류 대사체로는 ascorbigen (m/z 306→130)과 I3A (m/z 146→118)가 MS/MS MRM ([M+H]+) 모드에서 검출되었다. Ascorbigen은 NKC보다 IPC와 OPC에 유의적으로 많이 함유되어 있었다. I3A는 NKC에 가장 많이 함유되어 있었으나 시료 간 유의적인 차이는 없었다. 본 연구를 통하여 배추와 배추김치에 존재하는 글루코시놀레이트류와 그 대사체인 인돌류 물질을 UPLC-MS/MS를 이용하여 분석할 수 있었다.

Development of a UPLC-MS/MS method for the therapeutic monitoring of L-asparaginase

  • Jeong, Hyeon-Cheol;Kim, Therasa;Yang, Deok-Hwan;Shin, Kwang-Hee
    • Translational and Clinical Pharmacology
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    • 제26권3호
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    • pp.134-140
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    • 2018
  • This study aimed to develop a UPLC-MS/MS method for determining plasma levels of L-aspartic acid and L-asparagine and the activity of L-asparaginase. L-aspartic acid, L-asparagine, and L-aspartic acid-2,3,3-$d_3$ were extracted from human plasma by protein precipitation with sulfosalicylic acid (30%, v/v). The plasma samples were analyzed using an Imtakt Intrada amino acid analysis column with 25 mM ammonium formate and 0.5% formic acid in acetonitrile as the mobile phase with step gradient method at a flow rate of 0.5 mL/min. The injection volume was $5{\mu}L$, and the total run time was 15 min. Inter- and intra-batch accuracies (%) ranged from 96.62-106.0% for L-aspartic acid and 89.85-104.8%, for L-asparagine, and the coefficient of variation (CV%) did not exceed 7%. The validation results for L-aspartic acid and L-asparagine satisfied the specified criterion, however, the results for L-asparaginase activity assay showed a borderline validity. This study could be a foundation for further development of therapeutic drug monitoring systems using UPLC-MS/MS.

UPLC-Q-TOF-MS/MS Analysis for Steaming Times-dependent Profiling of Steamed Panax quinquefolius and Its Ginsenosides Transformations Induced by Repetitious Steaming

  • Sun, Bai-Shen;Xu, Ming-Yang;Li, Zheng;Wang, Yi-Bo;Sung, Chang-Keun
    • Journal of Ginseng Research
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    • 제36권3호
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    • pp.277-290
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    • 2012
  • The metabolic profiles of Panax quinquefolius and its associated therapeutic values are critically affected by the repetitious steaming times. The times-dependent steaming effect of P. quinquefolius is not well-characterized and there is also no official guideline on its times of steaming. In this paper, a UPLC-Q-TOF-MS/MS method was developed for the qualitative profiling of multi-parametric metabolic changes of raw P. quinquefolius during the repetitious steaming process. Our method was successful in discriminating the differentially multi-steamed herbs. Meantime, the repetitious steaming-inducing chemical transformations in the preparation of black American ginseng (American ginseng that was subjected to 9 cycles of steaming treatment) were evaluated by this UPLC-Q-TOF-MS/MS based chemical profiling method. Under the optimized UPLC-Q-TOF-MS/MS conditions, 29 major ginsenosides were unambiguously identified and/or tentatively assigned in both raw and multi-steamed P. quinquefolius within 19 min, among them 18 ginsenosides were detected to be newly generated during the preparatory process of black American ginseng. The mechanisms involved were further deduced to be hydrolysis, dehydration, decarboxylation and addition reactions of the original ginsenosides in raw P. quinquefolius through analyzing mimic 9 cycles of steaming extracts of 14 pure reference ginsenosides. Our novel steaming times-dependent metabolic profiling approach represents the paradigm shift in the global quality control of multi-steamed P. quinquefolius products.

UPLC-MS/MS를 이용한 소변 시료 중 내분비계 교란물질 27종 동시분석법 확립 (Simultaneous Analysis Method for 27 Endocrine Disrupting Chemicals in Human Urine using UPLC-MS/MS)

  • 박수빈;박나연;고영림
    • 대한화학회지
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    • 제68권4호
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    • pp.191-198
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    • 2024
  • 내분비 교란 화학물질(EDCs)은 생체 외부로부터 유입되어 인체의 내분비 기관 내에서 호르몬 작용을 교란시키는 화합물이다. 파라벤, 벤조페논, 비스페놀, 프탈레이트 등이 대표적이며, 현재 광범위한 분야에서 사용되고 있다. 하지만 이들에게 지속적으로 노출되면 혈당조절, 생식, 대사, 신경계 발달, 임신, 출산, 성장 등에 부정적인 영향을 끼칠 수 있다. 본 연구에서는 EDCs의 노출정도를 파악하기 위하여 인체시료(소변)를 liquid-liquid-extraction을 사용하여 전처리한 뒤 UPLC-MS/MS로 효과적이고 빠르게 분석하였다. 이와 같이 분석조건을 확립하고, 분석법의 유효성 검증을 통해 동시분석법의 신뢰도를 평가하였다. 결과는 정확도가 75.28~122.36%, 정밀도가 2.16~22.74%의 수치를 보였다. 본 연구에서 확립된 분석법은 추후 인체시료 중 EDCs의 노출을 평가하고 모니터링할 수 있는 연구의 방법론으로 이용될 수 있을 것이다.

Determination of Free Amino Acids in Isatidis Radix By HILIC-UPLC-MS/MS

  • Pan, Yilin;Li, Jin;Li, Xiang;Chen, Jianwei;Bai, Ganggang
    • Bulletin of the Korean Chemical Society
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    • 제35권1호
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    • pp.197-203
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    • 2014
  • A rapid, accurate and precise method for the determination of 22 amino acids in Isatidis Radix by Hydrophilic Interaction Ultra-High-Performance Liquid Chromatography Coupled with Triple-Quadrupole Mass Spectrometry (HILIC-UPLC-MS/MS) was established. Chromatographic separation was carried out on a Acquity UPLC BEH Amide column ($2.1mm{\times}100mm$, $1.7{\mu}m$) with gradient elution of acetonitrile (containing 0.05% formic acid and 2 mM ammonium formate) and water (containing 0.15% formic acid and 10 mM ammonium formate) at a flow rate of 0.4 mL/min; Waters Xevo$^{TM}$ TQ worked in multiple reaction monitoring mode. All components were separated in 17 min. All calibration curves were linear ($R^2$ > 0.991) over the tested ranges. The limits of detection (LOD) and limits of quantitation (LOQ) for these compounds were 0.21-79.55 and 0.72-294.23 ng/mL, respectively. The average recoveries were in the range of 93.75-104.16% with RSD value less than 6.56%. Therefore, this method could be an alternative assay for the determination of 22 amino acids in Isatidis Radix due to its rapidness, sensitivity, less sample and solvent consumption.

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 $3,496.32{\mu}g/g$.

건강기능식품 프랑스해안송껍질추출물 중 UPLC-MS/MS를 이용한 Ferulic acid, Caffeic acid, Catechin, Taxifolin 동시분석법 개발 연구 (Development of Simultaneous Analysis of Ferulic Acid, Caffeic Acid, Catechin and Taxifolin from Health Functional Food Pinus Pinaster Bark Extract by UPLC-MS/MS)

  • 오재명;김지안;허수정;최윤희;오금순
    • 한국식품위생안전성학회지
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    • 제34권5호
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    • pp.431-437
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    • 2019
  • 본 연구는 건강기능식품 프랑스해안송껍질추출물 중 catechin, caffeic acid, ferulic acid, taxifolin에 대한 동시분석법을 개발하는 연구이다. 최적분석조건을 확립하기 위해 시료 채취량, 용매 조건을 비교 검토하였으며, UPLC-MS/MS를 이용하여 각 4개 성분에 대한 정확한 분석 및 분석시간의 효율성도 향상하였다. 분석 시 사용한 컬럼은 Acquity UPLC BEH $C_{18}$이며, 정량이온으로 catechin, caffeic acid, ferulic acid, taxifolin 각각 133, 135, 245 및 248을 선정하였다. 확립된 시험법에 대해 특이성, 직선성, 검출한계, 정량한계, 정확성, 정밀성 등의 밸리데이션을 수행하였다. 4개 성분 모두 50-25000 mg/L 농도에서 결정계수(R2) 0.999이상으로 높은 직선성을 확인하였다. 또한 회수율은 84.9-104%이었고, 정밀성은 1.2-4.3%의 RSD를 확인하였다. 개발된 시험법은 프랑스해안송껍질추출물 중 catechin, caffeic acid, ferulic acid, taxifolin 분석을 위한 시험법으로 활용되기에 적합한 것으로 판단된다.