• Title/Summary/Keyword: HPLC-MS-MS

Search Result 911, Processing Time 0.028 seconds

Simultaneous determination of aminoglycoside antibiotics by HPLC/MS (HPLC/MS을 이용한 aminoglycoside 항생제 동시 분석에 관한 연구)

  • Roh, Young-Sun;Baek, Gui-Jung;Kim, Seung-Yong;Choi, Eun-Young;Seo, Heyng-Seok;Hur, Boo-Hong;Joung, Dong-Suk
    • Korean Journal of Veterinary Service
    • /
    • v.30 no.1
    • /
    • pp.1-12
    • /
    • 2007
  • A liquid chromatographic method has been developed for the analysis of aminoglycoside antibiotics (AMGs) using Heptafluorobutyric acid (HFBA) as a ion-pairing reagent. AMGs (amikacin, apramycin, dihydrostreptomycin, gentamicin, hygrosin B, kanamycin, neomycin, spectinomycin and tobramycin) were formed by reaction with HFBA as ion-pairing reagent. HFBA was attached to corresponding amino group of AMGs. These AMGs compounds were separated and detected by electrospray ionization mass spectrometry (ESI-MS). The experimental conditions for separation of AMGs were optimized and validated. A simple liquid chromatographic method for the determination of AMGs was demonstrated.

Isolation of 3,4-Dihydroxybenzoic Acid with Antimicrobial Activity from Bark of Aralia elata (두릅수피에서 항미생물활성을 갖는 3,4- dihydroxybenzoic acid의 분리)

  • Ma, Seung-Jin;Ko, Byoung-Seub;Park, Keun-Hyung
    • Korean Journal of Food Science and Technology
    • /
    • v.27 no.5
    • /
    • pp.807-812
    • /
    • 1995
  • The methanol extracts of Aralia elata bark showed antimicrobial activities against bacteria, yeast, fungi. The solvent fractionated acidic fraction that showed the activity was then successively purified with silica gel adsorption column chromatography, Sephadex LH-20 column chromatography, silica gel partition column chromatography, HPLC and TLC. The isolated major active substance was identified as 3,4-dihydroxybenzoic acid by MS, GC-MS, IR, $^{1}H-NMR\;and\;^{13}C-NMR$. The content of 3,4-dihydroxybenzoic acid was 0.869㎎/g in dried bark of Aralia elata.

  • PDF

Retention Factors and Resolutions of Amino Benzoic Acid Isomers with Some Ionic Liquids

  • Zheng, Jinzhu;Polyakova, Yulia;Row, Kyung-Ho
    • Biotechnology and Bioprocess Engineering:BBE
    • /
    • v.11 no.6
    • /
    • pp.477-483
    • /
    • 2006
  • Ionic liquids in the form of organic salts are being widely used as new solvent media. In this paper three positional isomers, o-amino benzoic acid, m-amino benzoic acid, and p-amino benzoic acids were separated with four different ionic liquids as mobile phase additives using high performance liquid chromatography (HPLC). The following ionic liquids were used: 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm][$BF_{4}$]), 1-ethyl-3-methylimidazolium tetrafluoroborate ([EMIm][$BF_{4}$]), 1-ethyl-3-methylimidazolium methylsulfate ([EMIm][MS]), and 1-octyl-3-methylimidazolium methylsulfate ([OMIm][MS]). The effects of the alkyl group length on the imidazolium ring and its counterion, and the concentrations of the ionic liquids on the retention factors and resolutions of amino benzoic acid isomers were tested. The results of the separations with ionic liquids as the eluents were better than those without ionic liquids. Excellent separations of the three isomers were achieved using 2.0-8.0 mM/L [OMIm][MS] and 1.0-8.0 mM/L [EMIm][MS] as the eluent modifiers.

Quantitative determination of 2'-Hydroxy-3',4'-methylenedioxy-3,4,5-trimethoxychalcone (HMTC) in rat plasma by HPLC-MS/MS and its application to a pharmacokinetic study

  • Jihyun Won;Juhyung Kang;Wonyoung Park;Jose C. J. M. D. S. Menezes;Marc Diederich;Eunyoung Kim;Wonku Kang
    • Analytical Science and Technology
    • /
    • v.36 no.1
    • /
    • pp.53-58
    • /
    • 2023
  • 2'-Hydroxy-3',4'-methylenedioxy-3,4,5-trimethoxychalcone (HMTC) is a newly synthesized chalcone that affects proliferation, cytotoxic potential and apoptosis in human leukemia cells. However, no validated determination method has been described so far for HMTC in biological samples. Thus, we developed a liquid chromatographic method using a tandem mass spectrometry to determine HMTC in rat plasma. Liquid-liquid extraction with ethyl acetate was used for the clean-up procedure. The analyte was separated on a reversedphase column with mobile phase of distilled water and acetonitrile (2:8, v/v, including 0.1 % formic acid). The ion transition of the precursor to the product ion was principally deprotonated ions [M-H]- at m/z 356.8 → 327.2 for HMTC. This analytical method was successfully applied in pharmacokinetic study of HMTC after intravenous administration in rats.

Chemotaxonomic Significance of Oregonin in Alnus japonica Native to Baekdudaegan Mountain Range in Korea

  • Hyeondu Jang;Sunmin Park;Seong Gyeom Kim;Seung Bin Bae;Hee Jeong Min;Chan Ok Lee;Hee Kyu Kim;Jin-Kyu Kim;Sun Eun Choi
    • Journal of Forest and Environmental Science
    • /
    • v.40 no.1
    • /
    • pp.53-63
    • /
    • 2024
  • Alnus japonica is indigenous to korea and usually grows in wet lowlands and damp regions in the mountains. Oregonin, is known as a representative compound of the diarylheptanoid mainly found in Alnus species and has been reported to have anti-inflammatory and antioxidant effects. In this experiment, we conducted a study on the presence of orogonin in the native Alnus japonica from the Baekdudaegan mountain range in Korea. We collected a total of 30 samples from Chuncheon, Yangyang, and Jeongseon and conducted experiments. In the HPLC analysis, we confirmed that oregonin was detected in all samples. After the quantitative analysis, samples with the highest content from each region were selected and LC-MS/MS experiments were performed. As a result, the same molecular weight as oregonin, 477.2 m/z, was confirmed in all samples.

Composition of volatile organic components on ballpoint pen inks by HS-SPME GC/MS (HS-SPME GC/MS를 이용한 볼펜잉크의 휘발성 성분 분석)

  • Choi, Mi-Jung;Kim, Chang-Seong;Sun, Yale-Shik;Park, Sung-Woo
    • Analytical Science and Technology
    • /
    • v.23 no.4
    • /
    • pp.414-422
    • /
    • 2010
  • In forensic examinations of question document, analysis about inks components and the dating of ink entries is often of considerable importance and forensic examination of inks is principally concerned with the classification and comparison of chemically complex mixtures. The authenticity about inks analysis of a questioned document may be examined through the analysis of inks used to TLC, HPLC/MS, GC/MS, LDI/MS. We collected 56 difference types of black ballpoint pen inks manufactured from 5 country groups. We identified major 6 species volatile organic components (VOCs), ethylbenzene ($0.089-0.244\;{\mu}g$/mL), o-xylene ($0.072-0.331\;{\mu}g$/mL), m,p-xylene ($0.062-0.318\;{\mu}g$/mL), benzene ($0.003-0.173\;{\mu}g$/mL), 1,1-dichloroethylene ($0.003-0.295\;{\mu}g$/mL), toluene ($0.007-0.484\;{\mu}g$/mL) using HS-SPME GC/MS. The results of this study indicated that determined VOCs of black ballpoint pen inks could make a discriminating tool of inks analysis for forensic question document and can supply methodology for classification and identification of between ballpoints pen inks.

Simultaneous and quantitative determination of anion biocides in soil by liquid chromatography-tandem mass spectrometry (토양 중 음이온 바이오사이드의 HPLC-MS/MS 동시 정량분석법)

  • Yang, Eun-Young;Shin, Ho-Sang
    • Analytical Science and Technology
    • /
    • v.28 no.5
    • /
    • pp.317-322
    • /
    • 2015
  • Simultaneous analytical method has developed for the determination of anion biocides in soil by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Chlorite and chlorate in soil were extracted with pure water, and cyanuric acid and sodium dodecylbenzenesulfonate (Na-DBS) were extracted with mobile phase (0.25 mM ammonium formate in 20 mM formic acid : acetonitrile (1:1)). The extract was injected into the LC-MS/MS system after filtration. The method detection limits in this study were 0.04 mg/kg for chlorite, 0.04 mg/kg for chlorate, 0.27 mg/kg for cyanuric acid, and 0.05 mg/kg for Na-DBS, respectively. The method was applied to the analysis of 50 soil samples collected from 40 sites sprayed with biocides and 10 background sites. As a result, anion biocides were not detected in all sites.

Determination of Alisol B 23-acetate and Alisol C 23-acetate in Alismatis Rhizoma by HPLC-ESI-MS

  • Ahn, Mi-Jeong;Lee, Cheol-Ho;Shin, Yong-Wook;Chun, Man-Seog;Kim, Chul-Young;Kim, Jin-Woong
    • Natural Product Sciences
    • /
    • v.14 no.3
    • /
    • pp.152-155
    • /
    • 2008
  • An HPLC-ESI-MS method has been developed to identify and quantify two main tetracyclic triterpenes, alisol B 23-acetate and alisol C 23-acetate in the Alismatis Rhizoma (Taeg-Sa). The relative distribution of the two triterpenes in the methanolic extract of commercially available Alismatis Rhizoma was established by selective ion monitoring (SIM) mode via electrospray ionization (ESI) source. Regression equations revealed good linear relationship, and the correlation coefficients were 0.999 and 0.998 for alisol B 23-acetate and alisol C 23-acetate, respectively, between the peak areas of the components and their concentration in a range of $0.06-2.0{\mu}g/mL$. It was found that there were significant differences in the amount of alisol B 23-acetate and alisol C 23-acetate between Korean and Chinese origins. The results showed that this method could be used to identify the two components in Alismatis Rhizoma with high sensitivity and selectivity.

Quantitative and Qualitative Analysis of Alkaloids in Coptis chinensis (Coptidis Rhizoma) by LC-DAD and LC-ESI/MS

  • Yu, Young-Beob;Bae, Chang-Hyu
    • Korean Journal of Plant Resources
    • /
    • v.30 no.6
    • /
    • pp.693-698
    • /
    • 2017
  • The quality control of natural products is principal key to guarantee the Good Manufacturing Practices (GMP) and Good Clinical Practices (GCP) for the functional food, pharmaceuticals and cosmeceuticals in the industry. In this study, we examined the quantitative analysis of berberine as marker substance of Coptidis Rhizoma by high performance liquid chromatography-photodiode array detector (HPLC-DAD). The HPLC method was validated and met all the requirements for the quality control analysis recommended by FDA and ICH. The berberine was separated on a Xterra $C_{18}$ column ($5{\mu}m$, $4.6{\times}250mm$) using mobile phase consisting of distilled water and acetonitrile with $KH_2PO_4$ (3.4 g) and $Na_2SO_4$ (1.7 g). Calibration curve of berberine has been estimated (y = 42293.47x-41589 with the correlation coefficient 0.9999). The amount of berberine was calculated as 4.25%. And berberastine, palmatine, columbamine, jatrorrhizine, epiberberine, berberine and coptisine in the Coptidis Rhizoma were identified by high performance liquid chromatography - electrospray ionization-mass spectrometer (HPLC-ESI-MS) method.

Identification of Carotenoids from Green Alga Haematococcus pluvialis by HPLC and LC-MS (APCI) and Their Antioxidant Properties

  • Ranga, Rao;Sarada, A.R.;Baskaran, V.;Ravishankar, G.A.
    • Journal of Microbiology and Biotechnology
    • /
    • v.19 no.11
    • /
    • pp.1333-1341
    • /
    • 2009
  • Haematococcus pluvial is, a green alga, accumulates astaxanthin (3,3'-dihydroxy-$\beta$,$\beta$'-carotene-4,4'-dione) upto 2-3% on a dry weight basis. In the present study, identification of carotenoids from Haematococcus cyst cell extract by HPLC and LC-MS (APCI) and their antioxidant properties were evaluated in in vitro model systems. The extract exhibited 89% and 78% antioxidant activities in the $\beta$-carotene linoleate model and the hydroxyl radical scavenging model, at 9 ppm of total carotenoid, respectively. The extract also showed 80%, 85%, and 79% antioxidant activities against lipid peroxidation in the kidney, brain, and liver of rats. Low-density lipoprotein oxidation induced by $Cu^{2+}$ ions was also protected (45%, 64%, and 75%) by the extract in a dose-dependent manner with different carotenoid levels. Thiobarbituric acid reactive substances concentration in the blood, liver, and kidney of rats were also significantly (p<0.005) decreased in H. pluvialis-treated rats. The potent antioxidant activity is attributable to various carotenoids present in the extract.