• Title/Summary/Keyword: MS analysis

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Analysis of Phenolic Acids in Tobacco Leaf by GC/MS (GC/MS에 의한 잎담배중 Phenolic Acid의 분석)

  • 박진우
    • YAKHAK HOEJI
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    • v.26 no.2
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    • pp.129-132
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    • 1982
  • A GC/MS method was developed to analyze phenolic acid extract from tobacco leaf. Extracted acids were converted to their methyl esters by refluxing with 3M hydrogen chloride in methanol, and the esters were reacted with his (trimethylsilyl) trifluoroacetamide plus 10% trimethylchlorosilane to silylate the phenolic groups. Derivatives of standard salicylic, p-hydroxybenzoic, vanillic, gentisic, p-coumaric, syringic, ferulic, and sinapic acids prepared by this procedure were analyzed by GC/MS on $20m{\times}0.2mm$ column of SE-54 glass capillary. GC/MS analysis of the extract from tobacco leaf revealed the presence of salicylic, p-hydtoxybenzoic, vanillic, gentisic, protocatechuic, p-coumaric, syringic, gallic, ferulic, caffeic, sinapic, and quinic acids, respectively. The quantitative analysis of these phenolic acids were achieved by using multiple ion selection technique.

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Food safety analytical techniques used in food industry (식품산업에서 활용되는 식품안전 분석기술의 현황)

  • Kim, Young-Jun
    • Food Science and Industry
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    • v.51 no.1
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    • pp.16-25
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    • 2018
  • Recently, the importance of analytical techniques related to food safety is emerging in the food industry due to changes in diet patterns, environmental changes, climate change and consumer's interest in food safety. In particular, food safety accidents in the food industry may cause economic losses such as media reports, product recalls, consumer distrust, and so on. Therefore, a systematic, proactive and comprehensive food safety management system is increasingly required to prevent food safety issues. Efforts to ensure the reliability of food safety are essential by introducing various analysis instruments such as LC, GC, ICP, LC/MS/MS, GC/MS/MS, ICP/MS, PCR, and RT-PCR. In addition, recent food safety analytical techniques used in food industry should be shifted paradigm by developing multi-component simultaneous analytical method, low cost with high efficient analytical method, and eco-friendly method.

Analysis of germanium in rock and sediment by ICP/MS after ammonium bifluoride(NH4HF2) digestion (이플루오린화 암모늄 시료분해 및 ICP/MS에 의한 암석 및 퇴적물 중 게르마늄 분석)

  • Eum, Chul Hun;Choi, Won Myung
    • Analytical Science and Technology
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    • v.26 no.6
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    • pp.375-380
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    • 2013
  • Ammonium biflouride ($NH_4HF_2$) digestion was studied for germanium analysis in rock and sediment by inductively coupled plasma mass spectrometry (ICP/MS). QLO-1 and SDO-1 are used for reference materials from USGS. Sediment, basalt and ball clay for GeoPT were chosen as real samples. The loss of germanium in open vessel digestion was well known which can be caused by easy transformation to volatile compounds. But ammonium bifluoride digestion could suppress loss of germanium in open vessel digestion. Germanium recovery was not influenced by hydrogen peroxide with ammonium bifluoride digestion. Furthermore, the new method was simple and rapid in germanium analysis by ICP/MS. MDL(method detection limit) was 0.015 ${\mu}g/g$ and germanium recovery was 106~128%.

Quantitative Determination of the Bioactive Marker Components in Gyeji-tang Using LC-ESI-MS/MS (LC-ESI-MS/MS를 이용한 계지탕 중 주요 성분 분석)

  • Seo, Chang-Seob;Ha, Hyekyung
    • Korean Journal of Pharmacognosy
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    • v.49 no.1
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    • pp.76-83
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    • 2018
  • A traditional herbal formula, Gyeji-tang has been used to treat the early colds, headache, chills, and fever in Asian countries. In this study, we were performed simultaneous determination of the 14 bioactive marker compounds, gallic acid, spinosin, paeoniflorin, albiflorin, liquiritin apioside, liquiritin, 6'''-feruloylspinosin, liquilitigenin, coumarin, cinnmamic acid, benzoylpaeoniflorin, cinnamaldehyde, glycyrrhizin, and 6-gingerol in Gyeji-tang using an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS). Analytical column was used a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) and maintained at $45^{\circ}C$ with a flow rate of 0.3 mL/min. The mobile phase consists of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was conducted using multiple reaction monitoring in the positive and negative modes by a Waters ACQUITY TQD LC-MS/MS system. The calibration curves of 14 bioactive marker compounds showed linearity with correlation coefficients ${\geq}0.9798$. The limits of detection and quantification values were in the range of 0.11-6.66 ng/mL and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the established LC-MS/MS method, the amounts of tested 14 compounds in the lyophilized Gyeji-tang sample were detected up to $85.7{\mu}g/g$. These results may be useful for quality assessment of a traditional herbal formulas.

Analysis of Carbonyl Compounds using DNPH Cartridge with LC-MS (DNPH cartridge/LC-MS 방법에 의한 카르보닐화합물 분석에 관한 연구)

  • Cho Deok-Hee;Song Il-Seok
    • Journal of Korean Society for Atmospheric Environment
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    • v.22 no.2
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    • pp.201-208
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    • 2006
  • Several carbonyl compounds are important because of their irritant and toxic properties, mutagenicity and carcinogenicity. Therefore, they are regulated in korean odor emission standard. In this study, atmospheric pressure ionization-mass spectrometry(API-MS) is used for the analysis of carbonyl compounds after derivatization with 2, 4-dinitrophenylhydrazine (DNPH) and liquid chromatographic separation. In the negative ion mode, the $[M-H]^-$ pseudomolecular ions are most abundant for the carbonyls. Analytical parameters such as linearity, repeatability and minimum detection limit were evaluated. The linearities ($r^2$) for carbonyls were $0.9977{\sim}0.9999$ when analyte concentration ranges from $25\;to\;250{\mu}g/L$(n=6). The relative standard deviations (%RSD) for carbonyls were $0.55{\sim}3.51%$ for concentration of $100{\mu}g/L$(n=5). The minimum detection limit (MDL) was $1.88{\mu}g/L$(0.27 ppb) for i-valeraldehyde. It was shown that LC-MS method has a great potential for carbonyl compounds analysis.

Biotransformation of Valdecoxib by Microbial Cultures

  • Srisailam, K.;Veeresham, C.
    • Journal of Microbiology and Biotechnology
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    • v.20 no.4
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    • pp.809-816
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    • 2010
  • Microbial biotransformations can be used to predict mammalian drug metabolism. The present investigation deals with microbial biotransformation of valdecoxib using microbial cultures. Thirty-nine bacterial, fungal, and yeast cultures were used to elucidate the biotransformation pathway of valdecoxib. A number of microorganisms metabolized valdecoxib to various levels to yield nine metabolites, which were identified by HPLC-DAD and LC-MS-MS analyses. HPLC analysis of biotransformed products indicated that a majority of the metabolites are more polar than the substrate valdecoxib. Basing on LC-MS-MS analysis, the major metabolite was identified as a hydroxymethyl metabolite of valdecoxib, whereas the remaining metabolites were produced by carboxylation, demethylation, ring hydroxylation, N-acetylation, or a combination of these reactions. The hydroxymethyl and carboxylic acid metabolites were known to be produced in metabolism by mammals. From the results, it can be concluded that microbial cultures, particularly fungi, can be used to predict mammalian drug metabolism.

Qualitative Analysis of Phenolic Substances in Artemisia capillaris by LC-MS (LC-MS에 의한 사철쑥에 존재하는 페놀성 화합물의 정성분석)

  • Nugroho, Agung;Lim, Sang-Cheol;Park, Hee-Juhn
    • Korean Journal of Pharmacognosy
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    • v.43 no.4
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    • pp.302-307
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    • 2012
  • The herb of Artemisia capillaris in Chinese medicine is used to treat hepatic diseases. In this research, qualitative analysis was performed using a UPLC/Q-TOF-ESI-MS/MS method for rapid identification of phenolic substances from A. capillaris: three caffeoylquinic acids (chlorogenic acid, 3,5-di-O-caffeoylquinic acid, and 4,5-di-O-caffeoylquinic acid), three flavonoids (hyperoside, isorhamnetin 3-O-robinobioside and quercetin) and three prenylated coumarins (6,8-diprenylumbelliferone, cedrelopsin and osthol) were identified. The three prenylated coumarins have not been reported from A. capillaris.

LC-MS/MS-Based Comparative Investigation on Chemical Constituents of Six Aster Species Occurring in Korea

  • Kang, Kyo Bin;Lee, Dong Young;Sung, Sang Hyun
    • Natural Product Sciences
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    • v.27 no.4
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    • pp.257-263
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    • 2021
  • Aster species (Asteraceae) are widely distributed edible and medicinal plants, known to contain various specialized metabolites including polyphenols and saponins. However, systemic analysis on the chemical profiles of these plants have rarely been made. Here we analyzed the phytochemical constituents in leaves of 6 Aster species occurring in Korea, A. ageratoides, A. altaicus var. uchiyamae, A. glehnii, A. hispidus, A. incisus, and A. yomena, by applying a LC-MS/MS-based untargeted metabolomics approach. The analysis revealed that A. ageratoides, A. hispidus, and A. yomena are relatively rich in saponins most of which are expected to be previously unknown.

Development of mass spectrometric analysis of $\alpha_1$(I) and $\alpha_2$(I) chain Collagen ($\alpha_1$(I)및 $\alpha_2$(I)사슬 콜라겐의 질량분석법 개발 연구)

  • Kim, Kwang-Yon;Cho, Seon-Young;Lee, Sang-Han;Nnm, Hae-Seon;Kim, Sung-Ho
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.6 no.2
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    • pp.134-143
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    • 2005
  • Collagen is the important structural proteins in mammals with various peptide composition and cross-linkings. The direct analysis of collagen protein was not suitable because of its structural complexity and diversity. In this study, we suggest the simple way of collagen analysis by introducing matrix-assisted laser desorption/ionization time-of flight mass spectrometry (MALDI-TOF MS) to identify the collagen and its trypsin-digested fragments, and by subsequent time-of-flight tandem mass spectrometry(Q-TOF MS/MS) to analyze the amino acid sequences of identified fragments. Using the collagen samples extracted from the tail of mouse, 10 separated bands were found in SDS-PAGE, and the masses of most bands could be more finely determined by MALDI-TOF MS. When each 10 separated proteins was tryptic digested and introduced to MALDI-TOF, the Gly1056-Arg1073 fragment from $\alpha_1$-chain was identified in four bands, and the Gly1056-Arg1073 fragment from $\alpha_2$-chain was identified in five bands, both in type I collagen. Although few fragments were found because of the cross-linkings left in digested collagen sample, it could be determined that the type I collagen existed at least in 7 separated bands. When the amino acid sequences of two identified fragments were analyzed by Q-TOF MS/MS, both sequences were identical with those determined by MALDI-TOF MS. It suggested that the two peaks in MALDI-TOF MS caused by the fragments identified in this work could be used as the fingerprint to simply identify type I collagen in protein samples.

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Accurate Metabolic Flux Analysis through Data Reconciliation of Isotope Balance-Based Data

  • Kim Tae-Yong;Lee Sang-Yup
    • Journal of Microbiology and Biotechnology
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    • v.16 no.7
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    • pp.1139-1143
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    • 2006
  • Various techniques and strategies have been developed for the identification of intracellular metabolic conditions, and among them, isotope balance-based flux analysis with gas chromatography/mass spectrometry (GC/ MS) has recently become popular. Even though isotope balance-based flux analysis allows a more accurate estimation of intracellular fluxes, its application has been restricted to relatively small metabolic systems because of the limited number of measurable metabolites. In this paper, a strategy for incorporating isotope balance-based flux data obtained for a small network into metabolic flux analysis was examined as a feasible alternative allowing more accurate quantification of intracellular flux distribution in a large metabolic system. To impose GC/MS based data into a large metabolic network and obtain optimum flux distribution profile, data reconciliation procedure was applied. As a result, metabolic flux values of 308 intracellular reactions could be estimated from 29 GC/ MS based fluxes with higher accuracy.