• Title/Summary/Keyword: liquid chromatography mass spectrometry

Search Result 888, Processing Time 0.024 seconds

Analysis of Hypoxia-Inducible Factor Stabilizers by a Modified QuEChERS Extraction for Antidoping Analysis

  • Kim, Si Hyun;Lim, Nu Ri;Min, Hophil;Sung, Changmin;Oh, Han Bin;Kim, Ki Hun
    • Mass Spectrometry Letters
    • /
    • v.11 no.4
    • /
    • pp.118-124
    • /
    • 2020
  • An analytical method was developed for hypoxia-inducible factor (HIF) stabilizers based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) sample preparation and liquid chromatography-high resolution mass spectrometry analysis. HIF stabilizers potentially enhance the performance of athletes, and hence, they have been prohibited. However, the analysis of urinary HIF stabilizers is not easy owing to their unique structure and characteristics. Hence, we developed the QuEChERS preparation technique for a complementary method and optimized the pH, volume of extraction solvent, and number of extractions. We found that double extraction with 1% of formic acid in acetonitrile provided the highest recovery of HIF stabilizers. Moreover, the composition of the mobile phase was also optimized for better separation of molidustat and IOX4. The developed method was validated in terms of its precision, detection limit, matrix effect, and recovery for ISO accreditation. To the best of our knowledge, this is the first demonstration of the application of the QuEChERS method, which is suitable as a complementary analytical method, in antidoping.

Thermal Stability Improvement of Liquid Fuel by Using Some Additives (첨가제를 이용한 액체연료의 열안정성 향상)

  • Park, Sun-Hee;Kim, Joong-Yeon;Chun, Byung-Hee;Han, Jeong-Sik;Jeong, Byung-Hun;Kim, Sung-Hyun
    • Proceedings of the Korean Society of Propulsion Engineers Conference
    • /
    • 2010.11a
    • /
    • pp.294-299
    • /
    • 2010
  • Thermal stability of exo-tetrahydrodicyclopentadiene (exo-THDCP) were investigated in a batch-type reactor perfectly coated with quartz. The 1 ml liquid product, which was a sufficiently small amount so as not to affect the reaction pressure, was sampled at 90 min intervals during the reaction and determined by gas chromatography-mass spectrometry (GC-MS) to measure thermal decomposition products of exo-THDCP and specify mechanism for additives (thermal stabilizer). Hydrogen donors (thermal stabilizer) such as 1,2,3,4-tetrahydroquinoline (THQ), benzyl alcohol (BnOH) increased thermal stability of exo-THDCP. These materials donated hydrogen to radical of exo-THDCP produced after initiation of exo-THDCP to decrease activity of primary products of exo-THDCP.

  • PDF

Study on the Development and Functional Characteristics of Salted Egg with Liquid Smoke

  • Putri Widyanti Harlina;Tri Yuliana;Fetriyuna;Raheel Shahzad;Meihu Ma
    • Food Science of Animal Resources
    • /
    • v.43 no.3
    • /
    • pp.471-490
    • /
    • 2023
  • In this study, the duck eggs were salted with none or 2.5% and 5.0% (v/v) of liquid smoke (LS), respectively. As a control, samples salted without LS were used. The 2-thiobarbituric acid (TBA) values, 1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging ability, and reducing power of the three groups were tested at 0, 7, 14, and 21 and 28 days to determine the effects of LS on the antioxidant activity of treated eggs. In addition, gas chromatography-mass spectrometry (GC-MS) and electronic nose (E-Nose) were used to analyze the volatile flavor components of fresh duck eggs, LS, control, and salted duck eggs enriched with 2.5% (v/v) LS after 28 days of salting. The TBA value considerably increased with an increase in salting period, and the treated egg's TBA value significantly associated with LS concentration. The TBA value decreased as the LS concentration increased. The amount of LS present was highly associated with their capacity to scavenge DPPH radicals. The reducing power of the samples was substantially correlated with the LS concentration, and the reducing power increased with increasing LS concentration. The GC-MS data revealed that phenols and ketones were the predominant chemicals present in the LS, and they were also found in the eggs added to the LS even though they were absent in the fresh eggs and control. The flavor of the control group and treated eggs with LS differed significantly, according to the principal component analysis and radar map of the E-nose. The texture study results revealed that the LS significantly impacted the hardness, cohesiveness, and chewiness of eggs.

Multi-class, Multi-residue Analysis of 59 Veterinary Drugs in Livestock Products for Screening and Quantification Using Liquid Chromatography-tandem Mass Spectrometry

  • Yu Ra Kim;Sun Young Park;Tae Ho Lee;Ji Young Kim;Jang-Duck Choi;Guiim Moon
    • Korean Journal of Environmental Agriculture
    • /
    • v.41 no.4
    • /
    • pp.288-309
    • /
    • 2022
  • BACKGROUND: The objective of this study was to develop a comprehensive and simple method for the simultaneous determination of 59 veterinary drug residues in livestock products for safety management. METHODS AND RESULTS: For sample preparation, we used a modified liquid extraction method, according to which the sample was extracted with 80% acetonitrile followed by incubation at -20℃ for 30 min. After centrifugation, an aliquot of the extract was evaporated to dryness at 40℃ and analyzed using liquid chromatography combined with tandem mass spectrometry. The method was validated at three concentration levels for beef, pork, chicken, egg, and milk in accordance with the Codex Alimentarius Commission/Guidelines 71-2009. Quantitative analysis was performed using a matrix-matched calibration. As a results, at least 52 (77.6%) out of 66 compounds showed the proper method validation results in terms of both recovery of the target compound and coefficient of variation required by Codex guidelines in livestock products. The limit of quantitation of the method ranged from 0.2 to 1119.6 ng g-1 for all matrices. CONCLUSION(S): This method was accurate, effective, and comprehensive for 59 veterinary drugs determination in livestock products, and can be used to investigate veterinary drugs from different chemical families for safety management in livestock products.

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
    • /
    • v.17 no.1
    • /
    • pp.83-86
    • /
    • 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
    • /
    • v.19 no.9
    • /
    • pp.922-931
    • /
    • 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
    • /
    • v.28 no.7
    • /
    • pp.1068-1077
    • /
    • 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.

Transesterification of O, N -bistrifluoroacetyl, n-butyl esters of some hydroxylated amino acids into O-carbethoxy, N-trifluoroacetyl, n-butyl esters during N-carbethoxy derivatization of histidine and histamine (Histidine 및 Histamine의 N-carbethoxy 유도체 형성시 수종의 수산기함유 아미노산의 치환 에스터화작용에 대하여)

  • Jo, Do-Hyun;Desgres, J.;Paideu, P.
    • Applied Biological Chemistry
    • /
    • v.20 no.1
    • /
    • pp.130-135
    • /
    • 1977
  • The transesterifcation of some hydroxylated amino acids derivatives was studied by gas-liquid chromatography and combined gas-liquid chromatography-mass spectrometry and the fragmentation of these two different O-derivatives was discussed.

  • PDF

Integration of Headspace Solid Phase Micro-Extraction with Gas Chromatography for Quantitative Analysis of Formaldehyde

  • Lo, Kong Mun;Yung, Yen Li
    • Bulletin of the Korean Chemical Society
    • /
    • v.34 no.1
    • /
    • pp.139-142
    • /
    • 2013
  • A study was carried out to evaluate the solid phase micro-extraction (SPME) for formaldehyde emission analysis of uncoated plywood. In SPME, formaldehyde was on-fiber derivatized through headspace extraction and analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The SPME was compared with desiccators (DC-JAS 233), small-scale chamber (SSC-ASTM D6007) and liquid-liquid extraction (LLE-EPA 556) methods which were performed in accordance with their respective standards. Compared to SSC (RSD 4.3%) and LLE (RSD 5.0%), the SPME method showed better repeatability (RSD 1.8%) and not much difference from DC (RSD 1.4%). The SPME has proven to be highly precise (at 95% confidence level) with better recovery (REC 102%). Validation of the SPME method for formaldehyde quantitative analysis was evidenced. In addition, the SPME by air sampling directly from plywood specimens (SPME-W) correlated best with DC ($r^2$ = 0.983), followed by LLE ($r^2$ = 0.950) and SSC ($r^2$ = 0.935).

Preserving Reliability of Evidence Containers for Fire Debris Containing Ignitable Liquids (유류화재증거물 보관용기의 신뢰성에 관한 연구)

  • Han, Dong-Hun;Lee, Sung-Ryong
    • Fire Science and Engineering
    • /
    • v.27 no.2
    • /
    • pp.70-74
    • /
    • 2013
  • It is very important for the collected samples at fire scenes to be properly preserved for laboratory analysis. Preserving abilities of four type containers, metal cans, glass jars, zipper and heat sealed polymer bags, with the five ignitable liquids (toluene, n-octane, o-xylene, n-decane and n-hexadecane) were examined with gas chromatography-mass spectrometry. The glass jars with Teflon (PTFE) liner were the best ability to prevent the evaporation of the ignitable liquids.