• Title/Summary/Keyword: Chromatographic analyses

Search Result 61, Processing Time 0.03 seconds

Simultaneous Liquid Chromatography Tandem Mass Spectrometric Determination of 35 Prohibited Substances in Equine Plasma for Doping Control

  • Kwak, Young Beom;Yu, Jundong;Yoo, Hye Hyun
    • Mass Spectrometry Letters
    • /
    • v.13 no.4
    • /
    • pp.158-165
    • /
    • 2022
  • Many therapeutic class drugs such as beta-blocker, corticosteroids, NSAIDs, etc are prohibited substances in the horse racing industry. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology makes it possible to isolate drugs from interference, enables various drug analyses in complex biological samples due to its sensitive sensitivity, and has been successfully applied to doping control. In this paper, we describe a rapid and sensitive method based on solid-phase extraction (SPE) using solid phase cartridge and LC-MS/MS to screen for different class's 35 drug targets in equine plasma. Plasma samples were pretreated by SPE with the NEXUS cartridge consisted non-polar carbon resin and minimum buffer solvent. Chromatographic separation of the analytes was performed on ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 ㎛). The elution gradient was conducted with 5 mM ammonium formate (pH 3.0) in distilled water and 0.1% formic acid in acetonitrile at a flow rate of 0.25 mL/min. The selected reaction monitoring (SRM) mode was used for drug screening with multiple transitions in the positive ionization mode. The specificity, limit of detection, recovery, and stability was evaluated for validation. The method was found to be sensitive and reproducible for drug screening. The method was applied to plasma sample analysis for the proficiency test from the Association of Racing Chemist.

Comparative Studies on the Analysis of Pesticide Residues. in Rice, Barley and Wheat (주곡중의 잔류농약분석에 관한 연구)

  • Park Seung Heui
    • Korean journal of applied entomology
    • /
    • v.13 no.4 s.21
    • /
    • pp.235-243
    • /
    • 1974
  • Recenty, the pesticides Pollutions in connection with the maintenance of dietary life are poised as serious sanitary problems. Author have established an appropriate analysis method in this connection and, at the same time, analysed the levels of pesticides residues, such as organochloride pesticides and organic mercurials, contained in main cereals (rice, barley, and wheat) collected throughout the country. Using gas liquid chromatography method, comparative analyses were made of organochloride Pesticides with electron capture detector, and organic mercurials with electron capture detector and the Dithizone Method. As a result, the organic mercurials analysis using gas liquid chromatography is believed to hold out an especially good method for both in terms of its sensitivity and its Practical applications. The summary obtained from these results is as follows; The detectable limit of organochloride pesticides is $5\times10^{-10}$ grams and that of organic mecurials is $5\times10^{-9}$ grams. The detections using the Dithizone Method are difficult. The gas liquid chromatographic analysis of organic mercurials is very simple in its operation and high in its sensitivity, compare with the analysis using the Dithizone Method. Therefore, this analysis is expected to be a good method applicable to the pesticide residues analysis. The levels of pesticide residues contained in samples are very little for tolerance and, therefore, no problem i.: foreseen for eating. The appropriate conditions of gas liquid chromatographic analysis obtained from these results are expected very useful for the date establishing an officially authorized analysis method.

  • PDF

Phenolic Glycosides Isolated from Safflower (Carthamus tinctorius L.) Seeds Increase the Alkaline Phosphatase (ALP) Activity of Human Osteoblast-like Cells

  • Kim, Dong-Hyun;Lee, Jin-Hee;Ahn, Eun-Mi;Lee, Youn-Hyung;Baek, Nam-In;Kim, In-Ho
    • Food Science and Biotechnology
    • /
    • v.15 no.5
    • /
    • pp.781-785
    • /
    • 2006
  • The chemical compositions of the seeds of the safflower (Carthamus tinctorius L.) plant were evaluated to determine possible compound having proliferative effects on human osteoblast cells. Three-[4,5-dimethylthiazole-2-yl]-2,5-diphenyltetrazolium bromide (MTT) test and alkaline phosphatase (ALP) activity were used to assess the effects of the isolates on the human osteoblast-like line (Saos-2). Activity guided fractionation led to the isolation of ALP activating lignin and alkaloid glycosides through the extraction of the seeds, solvent partitioning and repeated silica gel and octadecyl silica (ODS) column chromatographic separations. The data from Nuclear Magnetic Resonance (NMR), Mass (MS), and Infrared (IR) analyses enabled the determination of the chemical structure and characterization of two compounds as a tracheloside and an N-(p-coumaroyl)-serotonin mono-${\beta}$-D-glucopyranoside. These two compounds showed respectively $149.2{\pm}4.2$ and $138.9{\pm}3.5%$ ALP activity compared to the control when evaluated at a concentration of $100\;{\mu}g/mL$.

A Putative Histone Deacetylase Modulates the Biosynthesis of Pestalotiollide B and Conidiation in Pestalotiopsis microspora

  • Niu, Xueliang;Hao, Xiaoran;Hong, Zhangyong;Chen, Longfei;Yu, Xi;Zhu, Xudong
    • Journal of Microbiology and Biotechnology
    • /
    • v.25 no.5
    • /
    • pp.579-588
    • /
    • 2015
  • Fungi of the genus Pestalotiopsis have drawn attention for their capability to produce an array of bioactive secondary metabolites that have potential for drug development. Here, we report the determination of a polyketide derivative compound, pestalotiollide B, in the culture of the saprophytic fungus Pestalotiopsis microspora NK17. Structural information acquired by analyses with a set of spectroscopic and chromatographic techniques suggests that pestalotiollide B has the same skeleton as the penicillide derivatives, dibenzodioxocinones, which are inhibitors of cholesterol ester transfer protein (CETP), and as purpactins A and C', inhibitors of acyl-CoA:cholesterol acyltransferase (ACAT). Strain NK17 can make a fairly high yield of pestalotiollide B (i.e., up to 7.22 mg/l) in a constitutive manner in liquid culture. Moreover, we found that a putative histone deacetylase gene, designated as hid1, played a role in the biosynthesis of pestalotiollide B. In the hid1 null mutant, the yield of pestalotiollide B increased approximately 2-fold to 15.90 mg/l. In contrast, deletion of gene hid1 led to a dramatic decrease of conidia production of the fungus. These results suggest that hid1 is a modulator, concerting secondary metabolism and development such as conidiation in P. microspora. Our work may help with the investigation into the biosynthesis of pestalotiollide B and the development for new CETP and ACAT inhibitors.

Comparative Analyses of Bioactive Constituents from Forsythia suspensa and Forsythia viridissima by HPLC-DAD

  • Won, Tae-Hyung;Liao, Lijuan;Lee, Seung-Ho;Son, Jong-Keun;Shin, Jong-Heon
    • Natural Product Sciences
    • /
    • v.17 no.4
    • /
    • pp.328-336
    • /
    • 2011
  • A high-performance liquid chromatography (HPLC) with diode array detector (DAD) method was established for the discrimination of a folk medicine Forsythia suspensa and Forsythia viridissima. Five and three representative metabolites of the lignan and phenolic glycoside classes were selected for the analysis from F. suspensa and F. viridissima, respectively. The optimal chromatographic conditions were obtained on an ODS column (5 ${\mu}m$, $4.6{\times}250$ mm) with the column temperature at $40^{\circ}C$. The mobile phase was composed of methanol and 0.3% acetic acid using an isocratic elution with the flow rate 1 mL/min. Detection wavelength was set at 280 nm. All calibration curves showed good linear regression ($r^2$ > 0.996) within test ranges. Limits of detection (LOD) and limits of quantitation (LOQ) values were lower than 0.096 and 0.291 ${\mu}g/mL$, respectively. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.07-0.63% and 0.14-0.62%, respectively, and the overall recoveries of 97.79-102.46% for all of the compounds analyzed. In addition, effectiveness of diverse extraction methods was compared to each other for the development of standard analytical method. The verified method was successfully applied to the quantitative determination of representative metabolites in fifty-three commercial F. suspensa samples and fifteen commercial F. viridissima samples from diverse sources. The overall analytical results showed the unequivocal differences in bioactive constituents between F. suspensa and F. viridissima.

Isolation and Characterization of Mucous Exopolysaccharide (EPS) Produced by Vibrio furnissii Strain VB0S3

  • Bramhachari P.V.;Kishor P.B. Kavi;Ramadevi R.;Kumar Ranadheer;Rao, B. Rama;Dubey Santosh Kumar
    • Journal of Microbiology and Biotechnology
    • /
    • v.17 no.1
    • /
    • pp.44-51
    • /
    • 2007
  • Marine bacterial strains were isolated trom coastal regions of Goa and screened for the strains that produce the highest amount of mucous expolysaccharide (EPS). Our screening resulted in the identification of the strain Vibrio furnissii VB0S3 (hereafter called VB0S3), as it produced the highest EPS in batch cultures during the late logarithmic growth phase. The isolate was identified as VB0S3 based on morphological and biochemical properties. Growth and EPS production were studied in mineral salts medium supplemented with NaCl (1.5%) and glucose (0.2%). The exopolymer was recovered from the culture supernatant by using three volumes of cold ethanol precipitation and dialysis procedure. Chemical analyses of EPS revealed that it is primarily composed of neutral sugars, uronic acids, and proteins. Fourier-transform infrared (FT-IR) spectroscopy revealed the presence of carboxyl, hydroxyl, and amide groups, which correspond to a typical heteropolymeric polysaccharide, and the EPS also possessed good emulsification activity. The gas chromatographic analysis of an alditol-acetate derivatized sample of EPS revealed that it was mainly composed of galactose and glucose. Minor components found were mannose, rhamnose, fucose, ribose, arabinose, and xylose. EPS was readily isolated from culture supernatants, which suggests that the EPS was a slime-like exopolysaccharide. This is the first report of exopolysaccharide characterization that describes the isolation and characterization of an EPS expressed by Vibrio surnissii strain VB0S3. The results of the study contribute significantly and go a long way towards an understanding of the correlation between growth and EPS production, chemical composition, and industrial applications of the exopolysaccharide in environmental biotechnology and bioremediation.

An Efficient Method for Synthesis of PEO-Based Macromonomer and Macroinitiator

  • Kim, Jung-Ahn;Choi, Song-Yee;Kim, Kyung-Min;Go, Da-Hyeon;Jeon, Hee-Jeong;Lee, Jae-Yeol;Park, Hyeong-Soo;Lee, Cheol-Han;Park, Heung-Mok
    • Macromolecular Research
    • /
    • v.15 no.4
    • /
    • pp.337-342
    • /
    • 2007
  • The n-butyllithium-initiated ring-opening polymerization of ethylene oxide, in a mixture of benzene and dimethylsulfoxide (DMSO), between $25-45^{\circ}C$, with potassium tert-butoxide, is a useful and powerful method to control the molecular weight as well as achieve a quantitative chain-end functionalization yield of the resulting polymeric alkoxide via a one pot synthesis. The molecular weight of the product could be controlled by adjusting the ratio of grams of monomer to moles of initiators, such as n-butyllithium ([n-BuLi]) and potassium t-butoxide ([t-BuOK]). The yields for the macromonomer and ${\omega}-brominated$ poly(ethylene oxide) (PEO) were quantitative in relation to the chain-end functionalizations of the polymeric alkoxide formed. The resulting products were characterized by a combination of $^1H-NMR$ spectroscopic and size exclusion chromatographic analyses.

Regions in China identification and quality control of radix Codonopsis by chemical fingerprint: Evaluation of lobetyolin from different cultivated

  • Chou, Gui X;Gao, Qiu T;Li, Jun;Duan, Ran;Cheung, Anna WH;Chu, Glanice KY;Jiang, Zhi Y;Dong, Tina TX;Tsim, Karl WK
    • Advances in Traditional Medicine
    • /
    • v.6 no.4
    • /
    • pp.293-299
    • /
    • 2006
  • By using high-performance liquid chromatography-photodiode array detection, a simple and accurate chromatographic fingerprint method was developed for the identification of Radix Codonopsis (roots of Codonopsis) from different sources. Eighteen herbs of Codonopsis at different habitats in China, including roots from Codonopsis pilosula, Codonopsis pilosula var. modesta and Codonopsis tangshen were analyzed by the fingerprint. The amount of lobetyolin was calibrated, which was found to be more consistent in roots of Codonopsis pilosula as compared to that of Codonopsis pilosula var. modesta and Codonopsis tangshen. Having the fingerprint results, hierarchical clustering analyses were performed to classify the eighteen herbs into three groups: Codonopsis pilosula, Codonopsis pilosula var. modesta and Codonopsis tangshen. This clustering analysis agrees very well with the pharmacognostic identification result, and which could be used as a tool in the quality control of Radix Codonopsis.

Production of Polyhydroxybutyrate from Crude Glycerol and Spent Coffee Grounds Extract by Bacillus cereus Isolated from Sewage Treatment Plant

  • Lee, Gi Na;Choi, So Young;Na, Jonguk;Youn, HaJin;Jang, Yu-Sin
    • KSBB Journal
    • /
    • v.29 no.6
    • /
    • pp.399-404
    • /
    • 2014
  • Production of biodegradable polymer polyhydroxyalkanoates (PHAs) from industrial wastes exhibits several advantages such as recycle of waste and the production of high valuable products. To this end, this study aimed at isolating from the sewage treatment plant a PHA producing bacterium capable of utilizing wastes generated from biodiesel and food industries. A Bacillus cereus strain capable of producing poly(3-hydroxybutyrate) [P(3HB)] was isolated, which was followed by confirmation of P(3HB) accumulation by gas-chromatographic analyses. Then, the effects of nutrient limitation on P(3HB) production by B. cereus was first examined. Cells cultured in a minimal medium under the limitation of nitrogen, potassium and sulfur suggested that nitrogen limitation allows the highest P(3HB) accumulation. Next, production of P(3HB) was examined from both waste of biodiesel production (crude glycerol) and waste from food industry (spent coffee grounds). Cells cultured in nitrogen-limited minimal medium supplemented crude glycerol and waste spent coffee grounds extract accumulated P(3HB) to the contents of 2.4% and 1.0% of DCW. This is the first report demonstrating the capability of B. cereus to produce P(3HB) from waste raw materials such as crude glycerol and spent coffee grounds.

Characteristics of Coal/Polypropylene Coliquefaction (석탄과 폴리프로필렌의 공동액화 특성)

  • Jeong, Dae-Heui;Lee, Jin-Young;Jeong, Tae-Jin;Han, Choon
    • Journal of Energy Engineering
    • /
    • v.7 no.1
    • /
    • pp.138-145
    • /
    • 1998
  • Synergistic effect and characteristics of coliquefaction with Alaskan subbituminous coal and polypropylene (PP) were investigated in a tubing-bomb reactor. Coliquefaction results showed considerable synergistic effect on conversions for various coal/PP compositions and tetralin addition. Therefore, coliquefactions conversions at 430$^{\circ}$C and 450$^{\circ}$C with (coal 2 g+PP 2g) and 4 ml tetralin appeared 20.0 and 11.6 per cent higher respectively compared to the conversion of (coal+tetralin) and (PP+tetralin) liquefactions. According to gas chromatographic analyses, hydrogen was not needed during PP liquefactions. On the other hand, 0.70~0.83 part of tetralin per part of coal was converted into naphthalene by donoring hydrogen to free radicals during liquefaction. Also, extraction results by decalin proved that synergistic effect of coliquefaction were mainly due to PP decomposition catalysed be coal.

  • PDF