• Title/Summary/Keyword: high performance liquid chromatography/mass spectrometry

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Detection of 1,4-Dihydroxy-2-Naphthoic Acid from Commercial Makgeolli Products

  • Eom, Ji-Eun;Kwon, Sang-Chul;Moon, Gi-Seong
    • Preventive Nutrition and Food Science
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    • v.17 no.1
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    • pp.83-86
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    • 2012
  • To support beneficial effects of makgeolli for human health, we investigated for the presence of 1,4-dihydroxy-2-naphthoic acid (DHNA), a bifidogenic growth stimulator (BGS), from commercial makgeolli products. Among eleven makgeolli products (A~K), four showed positive peaks for DHNA in high performance liquid chromatography analysis. Makgeolli product A in particular contained the highest concentration of DHNA (0.44 ppm), as confirmed by liquid chromatography-mass spectrometry. Furthermore, BGS activity of the makgeolli product A was higher than those of products in which DHNA was not detected. These results indicate that makgeolli can be a good source for DHNA and that DHNA-enriched makgeolli could be developed by modifying manufacturing procedures and controlling its microbiota.

Studies on Microbial Transformation of Meloxicam by Fungi

  • Shyam Prasad, G.;Girisham, S.;Reddy, S.M.
    • Journal of Microbiology and Biotechnology
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    • v.19 no.9
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    • pp.922-931
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    • 2009
  • Screening-scale studies were performed with 26 fungal cultures for their ability to transform the anti-inflammatory drug meloxicam. Among the different fungi screened, a filamentous fungus, Cunninghamella blakesleeana NCIM 687, transformed meloxicam to three metabolites in significant quantities. The transformation of meloxicam was confirmed by high-performance liquid chromatography (HPLC). Based on the liquid chromatography-tandem mass spectrometry (LC-MS/MS) data, two metabolites were predicted to be 5-hydroxymethyl meloxicam and 5-carboxy meloxicam, the major mammalian metabolites reported previously. A new metabolite was produced, which is not detected in mammalian systems. Glucose medium, pH of 6.0, temperature of $27^{\circ}C$, 5-day incubation period, dimethylformamide as solvent, and glucose concentration of 2.0% were found to be suitable for maximum transformation of meloxicam when studied separately. It is concluded that C. blakesleeana can be employed for biotransformation of drugs for production of novel metabolites.

Genetic and Functional Analyses of the DKxanthene Biosynthetic Gene Cluster from Myxococcus stipitatus DSM 14675

  • Hyun, Hyesook;Lee, Sunjin;Lee, Jong Suk;Cho, Kyungyun
    • Journal of Microbiology and Biotechnology
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    • v.28 no.7
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    • pp.1068-1077
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    • 2018
  • DKxanthenes are a class of yellow secondary metabolites produced by myxobacterial genera Myxococcus and Stigmatella. We identified a putative 49.5 kb DKxanthene biosynthetic gene cluster from Myxococcus stipitatus DSM 14675 by genomic sequence and mutational analyses. The cluster consisted of 15 genes (MYSTI_06004-MYSTI_06018) encoding polyketide synthases, non-ribosomal peptide synthases, and proteins with unknown functions. Disruption of the genes by plasmid insertion resulted in defects in the production of yellow pigments. High-performance liquid chromatography and liquid chromatography-tandem mass spectrometry analyses indicated that the yellow pigments produced by M. stipitatus DSM 14675 might be novel DKxanthene derivatives. M. stipitatus did not require DKxanthenes for the formation of heat-resistant viable spores, unlike Myxococcus xanthus. Furthermore, DKxanthenes showed growth inhibitory activity against the fungi Aspergillus niger, Candida albicans, and Rhizopus stolonifer.

Characterization of a New Antidementia $\beta$-Secretase Inhibitory Peptide from Rubus coreanus

  • Lee, Dae-Hyoung;Lee, Dae-Hyung;Lee, Jong-Soo
    • Food Science and Biotechnology
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    • v.17 no.3
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    • pp.489-494
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    • 2008
  • In order to develop a potent antidementia $\beta$-secretase inhibitor from phytochemicals, $\beta$-secretase inhibitory activities of extracts from many medicinal plants and herbs were determined. Water extracts from Rubus coreanus showed the highest $\beta$-secretase inhibitory activity of 84.5%. After purification of the $\beta$-secretase inhibitor from R. coreanus using systematic solvent extraction, ultrafiltration, Sephadex G-10 column chromatography, and reverse-phase high performance liquid chromatography (HPLC), a purified $\beta$-secretase inhibitor with $IC_{50}$ inhibitory activity of $6.3{\times}10^3\;ng/mL$ ($1.56{\times}10^{-6}\;M)$ was obtained with a 0.08% solid yield. The molecular mass of the purified $\beta$-secretase inhibitor was estimated to be 576 Da by liquid chromatography-mass spectrometry (LC-MS) and $\beta$-secretase inhibitor also is a new tetrapeptide with the sequence Gly-Trp-Trp-Glu. The purified $\beta$-secretase inhibitory peptide inhibited $\beta$-secretase non-competitively and also show less inhibition on trypsin, however no inhibition on other proteases such as $\alpha$-secretase, chymotrypsin, and elastase.

Quantitative Analysis of Marker Compounds and Matabolic Profiling of Zanthoxylum piperitum (Chopi) according to Different Parts and Harvest T imes

  • Hyejin Hyeon;Eunbi Jang;Yoonji Lee;Sung Hye Han;Baek Kwang Yeol;Su Young Jung;Ki Sung Shin;Weon-Jong Yoon
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2023.04a
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    • pp.62-62
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    • 2023
  • Zanthoxylum piperitum ("chopi" in Korean) has been used as traditional medicinal plants with high anti-inflammatory, antioxidant, and antifungal activities. The aims of the study were to identify marker compounds and to investigate metabolites variation of chopi according to different parts and harvest times. Every month from June to September, chopi were harvested with three different parts: leaves, leaf-twig mixtures, twigs. Using liquid chromatography-tandem mass spectrometry (LC-MS/MS), two main marker compounds (quercitrin and quercetin-3-O-glucoside) were characterized in 70% ethanol extracts of chopi. Quantification of the two marker compounds were subsequently conducted by high performance liquid chromatography (HPLC), representing that contents of these compounds were higher in leaves and leaf-twig mixtures rather than twigs. For the comprehensive analysis of metabolites associated with production of marker compounds, 35 primary metabolites were identified using gas chromatography-mass spectrometry (GC-MS). Multivariate analysis results represented that plant parts were main contributors to the separation of chopi. However, significant differences were not observed between leaves and leaf-twig mixtures samples. The partial least square (PLS) predictive model revealed that monosaccharides (fructose, galactose, glucose, mannose, xylose) and branched-chain amino acids (isoleucine, valine, leucine) were important determinants for the production of marker compounds together with alanine, inositol, GABA, and theronic acid. This study could be extended to stabilize and utilize chopi as an industrial material, as well as to find good candidates with various nutritional traits.

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Rational and efficient approach to the preparation of the active fractions of Scutellaria baicalensis (황금(Scutellaria baicalensis) 유효분획물 제조의 합리적이고 효율적인 접근방법)

  • Kim, Doo-Young;Kim, Won Jun;Kim, Jung-Hee;Oh, Sei-Ryang;Ryu, Hyung Won
    • Journal of Applied Biological Chemistry
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    • v.62 no.1
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    • pp.31-38
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    • 2019
  • Scutellaria baicalensis Georgi (Scutellariae Radix) has been widely used as a dietary ingredient and traditional herbal medicine such as diuretic, hyperlipidemia, antibacterial, anti-allergy, anti-inflammatory and anticancer properties. In this study, the isolation of biomarkers or bioactive compounds from complex S. baicalensis extracts represents an essential step for de novo identification and bioactivity assessment. The bioactive fraction consisted of eight compounds which was chromatographed on an analytical high performance liquid chromatography column using two different gradient runs. A simulative replacement of the analytical column with a medium pressure liquid chromatography and open column allowed the determination of gradient profile to allow sufficient separation in the preparative scale. From the optimized method, eight standard compounds have been identified in the fractions. In addition, MS, UV, HRMS detection was provided by ultraperformance liquid chromatographyequadrupole time-of-flight mass spectrometry (UPLC-QTof-MS) of all fractions. Therefore, this scale up procedure was successfully applied to a S. baicalensis extract.

Anticholinesterase activity of Cinnamomum zeylanicum L. leaf extract

  • Dalai, Manoj Kumar;Bhadra, Santanu;Chaudhary, Sushil Kumar;Chanda, Joydeb;Bandyopadhyay, Arun;Mukherjee, Pulok K.
    • CELLMED
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    • v.4 no.2
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    • pp.11.1-11.6
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    • 2014
  • Cinnamomum zeylanicum (C. zeylanicum) is a tropical evergreen tree of Lauraceae family. It is one of the oldest culinary spices known and used traditionally in many cultures for centuries. In addition to its culinary uses, cinnamon also possesses as a folk remedy of many health disease condition including analgesic, antiseptic, antispasmodic, aphrodisiac, astringent, carminative, haemostatic, insecticidal, and parasiticide and memory enhancing property. This study was aimed to assess the acetylcholinesterase and butyrylcholinesterase inhibitory activity of standardized methanol extract of the C. zeylanicum. Gas chromatography - mass spectrometry (GC-MS) and high performance liquid chromatography (HPLC) analysis were done to identify the presence of eugenol as chemical component and support the neuroprotective activity in the extract. Anticholinesterase inhibitory activity of crude methanol extract of C. zeylanicum leaves and cinnamon oil were evaluated by 96-well microtiter plate assay and thin layer chromatography bioassay detection methods. This study revealed that cinnamon oil ($IC_{50}:45.88{\pm}1.94{\mu}g/ml$) has better anticholinesterase activity than methanol extract ($IC_{50}:77.78{\pm}0.03{\mu}g/ml$). In HPLC analysis, retention time of eugenol in cinnamon oil was found to be 15.81 min which was comparable with the retention time (15.99 min) of the reference standard, eugenol. Seven chemical compounds were identified by GC-MS analysis, in which eugenol as an important phytoconstituents. Thus the phytochemicals from C. zeylanicum methanol leaves extract could be developed as potential source of anticholinesterase activity, with particular benefit in the symptomatic treatment of Alzheimer's disease.

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
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    • v.43 no.2
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    • pp.224-229
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    • 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.

A Survey of Zearalenone in Beans Using High Performance Liquid Chromatography-Fluorescence Detector (HPLC-FLD) and Ultra Performance Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS) (HPLC-FLD 및 LC-MS/MS에 의한 두류 중 제랄레논 오염실태 조사)

  • Jang, Mi-Ran;Lee, Chang-Hui;Lee, Hyo-Jeong;Kim, Ji-Yeon;Son, Sang-Hyeok;Sin, Chun-Sik;Kim, So-Hui;Kim, Dae-Byeong
    • Korean Journal of Food Science and Technology
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    • v.40 no.3
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    • pp.354-359
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    • 2008
  • A survey for zearalenone contamination was conducted on 27 soy bean samples, 27 red bean samples, 16 black bean samples, 19 seoritae samples, 14 seomoktae samples, for a total of 127 commercial Korean samples. Zearalenone was quantified by the immunoaffinity column clean-up method with high performance liquid chromatography-fluorescence detection (HPLC-FLD), and was confirmed by liquid chromatography tandem mass spectrometry(LC-MS/MS). The limits of detection and quantification were $2.0{\mu}g/kg$ and $6.0{\mu}g/kg$, respectively. The recovery in the beans ranged from 82.2 to 98.4%. According to HPLC-FLD, zearalenone was detected in 13 samples (10.2% incidence), including 1 soybean and 12 red bean samples. The zearalenone contamination levels were in the range of 8.01${\sim}38.98{\mu}g/kg$. Finally, LC-MS/MS analysis was conducted in the contaminated samples to verify the results of HPLC-FLD. The LC-MS/MS results confirmed the presence of zearalenone in all 13 samples. The contamination level was lower than that of EU, which is below $100{\mu}g/kg$ for raw grains.

Identification of Natural dyes used in 16th pink Dallryeong (Official's robe in Joseon Dynasty) Excavated from Cheonan, Chungnam (충남 천안시 출토 16세기 분홍 단령에 사용된 염재 동정)

  • Chae, Jeongmin;Ryu, Hyo-Seon
    • Journal of Conservation Science
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    • v.31 no.3
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    • pp.299-308
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    • 2015
  • Aim of this study is to identify dyestuff of the Dallryeong(official's robe in Joseon Dynasty, 16th century) excavated from Yuryang-dong, Cheonan, in 1996. For this purpose, extracted dyestuffs from Dallryeong fabric and from natural dyestuffs for red color(safflower, Sapanwood, Madder) which are presumed to have been used in the Dallryeong, are analyzed and compared by high performance liquid chromatography(HPLC). As a result, HPLC chromatogram of extracts of the Dallryeong's dyestuff and safflower are showed a peak at 17.5 minutes. The UV/Vis spectra of the samples are showed the maximum absorption wavelength at 519nm. This result is identical with the analysis of the previous studies on red dyestuff of safflower. In addition, the analysis of Mass Spectrometry(MS) showed the identical result of the peak with m/z 910. Following these results, excavated pink Dallryeong were considered to have been dyed with safflower.