• Title/Summary/Keyword: HPLC quantification

Search Result 403, Processing Time 0.019 seconds

LC-MS/MS Assay Validation for a New Immune Modulator, JHL45, and its Major Metabolite in Plasma: Application to Pharmacokinetic Studies in Rats

  • Baek, In-Hwan;Chae, Jung-Woo;Song, Gyu-Yong;Kwon, Kwang-Il
    • Bulletin of the Korean Chemical Society
    • /
    • v.30 no.11
    • /
    • pp.2631-2636
    • /
    • 2009
  • JHL45, a novel immune modulator for anti-atopic dermatitis and allergic airway disease, was synthesized from decursin isolated from Angelica gigas. In order to conduct a pharmacokinetic study of JHL45, an analytical method, ideally one that uses a minimal amount of biological sample must first be validated. In this study, a HPLC-MS/MS method was developed and validated for the quantification of JHL45 and its major metabolite, (+)-decursinol, from 10 ${\mu}L$ of rat plasma. JHL45 was stable under the analysis conditions, and intra- and inter-day accuracies exceeded 90.06%, with a precision variability ${\leq}$ 13.16% for each analyte. The mean values for Cmax, AUC8h, half-life of JHL45 in rats after intravenous administration of 5 mg/kg JHL45 were 24.59 μg/mL, 10.02 ${\mu}g{\cdot}h/mL$, and 1.88 h, respectively. The validated method herein will be useful for further pharmacokinetic studies of JHL45, as well as in preclinical and clinical phases.

Analysis of studies on Bojungikgi-tang(Buzhongyiqi-tang) to establish the fundament for Evidence Based Medicine (EBM) (EBM 기반구축을 위한 보중익기탕 실험 연구 분석)

  • Kim, Jung-Hoon;Lee, Jun-Kyoung;Shin, Hyeun-Kyoo
    • Korean Journal of Oriental Medicine
    • /
    • v.17 no.2
    • /
    • pp.135-167
    • /
    • 2011
  • Objective : To establish the fundament for EBM of Traditional Korean Medicine, the papers on Bojungikgitang(Buzhongyiqi-tang) frequently used in medical institutions of Traditional Korean Medicine were analyzed through researching domestic and international papers. Methods : The papers were classified by the registration of domestic or international journals, the year of publishment, experimental fields and the kinds of studies on biological activities. Results : Among 2005 volumes of papers on Bojungikgi-tang(Buzhongyiqi-tang), 219 volumes were selected according to selective criteria. 71 volumes were published in domestic journals, 52 volumes were in Chinese journal, 96 volumes were in Japanese journal. The papers on instrumental analyses reported the quantification of standard compounds of herbal medicines in Bojungikgi-tang(Buzhongyiqi-tang) using HPLC method. The papers on biological activities of Bojungikgi-tang(Buzhongyiqi-tang) showed mainly immune regulation, anti-infection, anti-cancer, gastrointestinal activity, neuropsychiatric regulation, anti-inflammation, hepatoprotection, musculoskeletal regulation. Among biological activities, papers on immume regulation were reported mostly. Conclusions : The efficacy of Bojungikgi-tang(Buzhongyiqi-tang) could be related to immune regulation, gastrointestinal activity, anti-fatigue and further study need to be preceeded to establish the fundament for EBM of Bojungikgitang(Buzhongyiqi-tang).

Quantification of Cyanidin-3-glucoside(C3G) in Mulberry Fruits and Grapes (오디와 포도의 안토시아닌 색소 물질 조성 비교 및 C3G 정량)

  • 김현복
    • Journal of Sericultural and Entomological Science
    • /
    • v.45 no.1
    • /
    • pp.1-5
    • /
    • 2003
  • This study was carried out to investigate the anthocyanin pigments in the fruits of mulberry and grape. The anthocyanin pigments in the fruits of mulberry and grape were extracted with l% methanolic hydrochloric acid. The cyanidin-3-glu-coside (C3G) was separated and quantified by HPLC system using a Nova-Pack C$\sub$18/ column. The cyanidin-3-glucoside (C3G) contents of mulberry fruits were higher than that of grapes. Especially, anthocyanin pigments of mulberry fruits showed only C3G peak, but anthocyanin pigments of grapes showed some species peaks.

Isolation of Flavonoid Glycosides with Cholinesterase Inhibition Activity and Quantification from Stachys japonica

  • Nugroho, Agung;Choi, Jae Sue;Seong, Su Hui;Song, Byong-Min;Park, Kyoung-Sik;Park, Hee-Juhn
    • Natural Product Sciences
    • /
    • v.24 no.4
    • /
    • pp.259-265
    • /
    • 2018
  • The three flavone glycosides, 4'-O-methylisoscutellarein 7-O-(6'''-O-acetyl)-${\beta}$-D-allopyranosyl(1${\rightarrow}$2)-${\beta}$-D-glucopyranoside (1), isoscutellarein 7-O-(6'''-O-acetyl)-${\beta}$-D-allopyranosyl(1${\rightarrow}$2)-${\beta}$-D-glucopyranoside (3), and isoscutellarein 7-O-${\beta}$-D-allopyranosyl(1${\rightarrow}$2)-${\beta}$-D-glucopyranoside (4) in addition to a flavonol glycoside, kaempferol 3-O-${\beta}$-D-glucopyranoside (astragalin, 2), were isolated from Stachys japonica (Lamiaceae). In cholinesterase inhibition assay, compound 1 significantly inhibited aceylcholinesterase (AChE) and butyrylcholinesterase (BChE) activities ($IC_{50}s$, $39.94{\mu}g/ml$ for AChE and $86.98{\mu}g/ml$ for BChE). The content of isolated compounds were evaluated in this plant extract by HPLC analysis. Our experimental results suggest that the flavonoid glycosides of S. japonica could prevent the memory impairment of Alzheimer's disease.

Inhibitory Effects on Melanogensis of Scrophularia koraiensis Nakai in Melanocytes

  • So-Yeon Han;Hye-Jeong Park;Da-Yoon Lee;Seo-Yoon Park;Jun-Hwan Jeong;Yoon-Jae Kwon;Tae-Won Jang;Jae-Ho Park
    • Proceedings of the Plant Resources Society of Korea Conference
    • /
    • 2022.09a
    • /
    • pp.110-110
    • /
    • 2022
  • Scrophularia koraiensis Nakai (S. koraiensis) has used its roots as traditional herbal medicine. Some research is reported to be effective in allergic inflammation and osteoporosis. In a present study, we conducted to investigate the bioactivity of the ethanol extract of S. koraiensis (ESK) on the inhibition of melanogenesis and the apoptosis of melanocytes. We analyzed Harpagoside of ESK by using LCMS and HPLC-PDA and investigated the regulation of ESK on reactive oxygen species. Also, the expressions of melanin synthesis-related factors and apoptosis-related factors were confirmed. As a result, the quantification results of quercetin and rutin in ESK were 77.2 and 7.4 mg/g. IC50 on DPPH and ABTS radical scavenging activity is 33.1 and 9.5 ug/mL. ESK attenuated not only the expression of tyrosinase, TYRP-1, TYRP-2, and MITF in melanogenesis. It is thought that ESK may be effective in the inhibition of melanogenesis through MAPK cell signaling pathway in melanocytes. These study results suggest that ESK has the ability to inhibit melanin production and induce apoptosis.

  • PDF

Determination of Four Macrolide Antibiotics Residues in Chicken Muscle Using High-Performance Liquid Chromatography (액체크로마토그래피를 이용한 닭고기 시료에서의 마크로라이드계 동시분석법 개발)

  • Lee, Sang-Hee;Yoo, Miyoung;Shin, Dong-Bin
    • Journal of Food Hygiene and Safety
    • /
    • v.28 no.1
    • /
    • pp.19-23
    • /
    • 2013
  • A simple and rapid method has been developed and validated for simultaneous determination of each macrolides residues (spiramycin, josamycin, tilmicosin, tylosin) in chicken muscle by high-performance liquid chromatography- photo diode array (HPLC-PDA). Chicken muscle sample have been extracted with liquid-liquid extraction process; analytes was extracted by acetonitrile, and then defatted with hexane saturated by acetonitrile. The HPLC separation was performed on a Unison UK-$C_{18}$ ($150mm{\times}3.0mm$, $3{\mu}m$) with a gradient system of 0.1% trifloroacetic acid (TFA) and 0.1% trifloroacetic acid (TFA) in acetonitrile as the mobile phase. The drugs were detected at 232 nm for spiramycin and josamycin, and 287 nm for tilmicosin and tylosin. The limits of quantification (LOQs) were between 27 and $59{\mu}g/kg$; and the intra- and inter-day precision (relative standard deviation; RSD) was between 0.9-13.2 and 2.4-13.1%, respectively in chicken muscle sample. The method may has been successfully applied for multiresidue determination of four macrolides below the maximum residue limits (MRLs) established by the European Union (EU).

Comparison of Extraction Methods for Determination of Vitamin K1 in Vegetables (채소류의 비타민 K1 분석을 위한 추출방법의 비교)

  • Kim, Hyeongi;Choi, Youngmin;Cho, Young-Sook;Sung, Jeehye;Ham, Hyeonmi;Lee, Junsoo
    • Journal of the Korean Society of Food Science and Nutrition
    • /
    • v.43 no.11
    • /
    • pp.1791-1795
    • /
    • 2014
  • The objective of this study was to compare two extraction methods for determination of vitamin K1 (phylloquinone) in vegetables. In addition, analytical method validation parameters such as accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and linearity were calculated to ensure the method's validity. Vitamin K1 was quantified by reversed-phase HPLC using post-column derivatization and fluorescence detection ($Ex{\lambda}=243nm$, $Ex{\lambda}=430nm$). Higher analytical values were observed using solvent extraction compared to those from the enzyme extraction method. The results from the method validation showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9994. The LOD and LOQ were 0.1335 and 0.2784 ng/injection volume ($50{\mu}L$), respectively. The inter-day precision and inter-day precision were 2.0% and 2.1%, respectively. Overall recovery was close to 100% (n=5). The phylloquinone contents ranged from 9.42 to $1,212.57{\mu}g/100g$. Our study provides reliable data on the phylloquinone contents in commonly consumed vegetables in Korea.

HPLC Method Validation of Naringin Determination in Goheung Yuzu Extract as a Functional Ingredient (건강기능식품 기능성 원료로서 고흥 유자 추출물의 지표성분 Naringin 분석법)

  • Moon, So-Hyun;Ko, Eun-Young;Assefa, Awraris Derbie;Park, Se-Won
    • Journal of the Korean Society of Food Science and Nutrition
    • /
    • v.43 no.11
    • /
    • pp.1737-1741
    • /
    • 2014
  • An HPLC method for determination of naringin was developed to standardize it as a marker compound in Goheung yuzu extract as a functional health food. Optimum results were obtained by C-18 column chromatography using solvent mixtures (A: 0.5% acetic acid, B: acetonitrile) as the stationary phase and mobile phase. The method was fully validated and sensitive with a limit of detection (LOD) of 0.0218 mg/L and limit of quantification (LOQ) of 0.0661 mg/L. The method showed high linearity (coefficient of correlation=0.9986) and high accuracy, as recovery rates of naringin at concentrations of 1, 0.5, 0.1, 0.05 mg/mL were in the ranges of 95.74~98.25%, 97.67~101.01%, 97.33~104.64%, and 95.53~106.82%, respectively. Intra-day and inter-day variation, which are measures of method precision, were 1.39~1.95% and 0.17~1.49%, respectively. Therefore, the method could be used without modification for determination of naringin as a marker compound in Goheung yuzu extracts.

Determination of Fructooligosaccharides and Raffinose in Infant Formula by High Performance Liquid Chromatography with Evaporative Light Scattering Detector (HPLC-ELSC를 이용한 조제분유 중 fructooligosaccharides 및 raffinose 분석)

  • Shin, Man-Sub;Park, Jae-Woo;Cho, Mi-Ran;Song, Sung-Ok;Kim, Chun-Sun;Choi, Chun-Bae;Lee, Seoung-Won;Lee, Ki-Woong;Chang, Chi-Hoon;Kwak, Byung-Man
    • Korean Journal of Food Science and Technology
    • /
    • v.38 no.6
    • /
    • pp.725-729
    • /
    • 2006
  • A method was developed for the determination of fructooligosaccharides and raffinose contents in infant formula. The samples were extracted and analyzed by liquid chromatography equipped with carbohydrate column and evaporative light scattering detector. The mobile phase used for the gradient mode was water-acetonitrile, at a flow rate of 1.0mL/min. The method showed a mean recovery of 95-99%, the relative standard deviation obtained in the precision study was 0.774-8.982%, the quantification and detection limits were 25-50mg/L.

Analysis of Zearalenone Contamination in Cereal-Based Products Using High Performance Liquid Chromatography-Fluorescence Detector and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry (곡류가공품 중 제랄레논 오염도 조사)

  • Jang, Mi-Ran;Lee, Chang-Hee;Choi, In-Sun;Shin, Choon-Shik;Kim, Jin-Hee;Jang, Young-Mi;Kim, Dong-Sul;Ahn, Dong-Hyun
    • Korean Journal of Food Science and Technology
    • /
    • v.43 no.2
    • /
    • pp.224-229
    • /
    • 2011
  • Zearalenone (ZEA) is an estrogenic mycotoxin mainly produced by Fusarium graminerum, a species which colonizes a wide variety of cereals, including wheat, barley and processed products. A survey of ZEA contamination was conducted on 141 dried confectioneries, 59 breads and rice cakes, 135 noodles and 101 other products, for a total of 432 commercial samples. Samples were analyzed by high performance liquid chromatography with fluorescence detection (HPLC-FLD) after immunoaffinity clean-up and was confirmed by liquid chromatography tandem mass spectrometry (LCMS/MS). The limits of detection and quantification were 2.0 and $6.0{\mu}g/kg$, respectively. The recovery ranged from 80.2% to 98.4% in the cereal based product. ZEA was detected in 38 samples (8.8% incidence), including 3 snack, 2 biscuit and 33 other cereal products. The ZEA contamination levels were in the range of $5.38-53.76{\mu}g/kg$. Finally, LC-MS/MS analysis of the contaminated samples was conducted to confirm the detected ZEA, and all 38 samples showing ZEA by HPLC-FLD were confirmed by LC-MS/MS.