• 제목/요약/키워드: liquid chromatography mass spectrometry

검색결과 891건 처리시간 0.031초

Analysis and Exposure Assessment of Perchlorate in Korean Dairy Products with LC-MS/MS

  • Oh, Sung-Hee;Lee, Ji-Woo;Mandy, Pawlas;Oh, Jeong-Eun
    • Environmental Analysis Health and Toxicology
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    • 제26권
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    • pp.12.1-12.7
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    • 2011
  • Objectives: Perchlorate is an emerging contaminant that is found everywhere, including various foods. Perchlorate is known to disturb the production of thyroid hormones and leads to mental disorders in fetuses and infants, as well as metabolic problems in adults. In this study, we attempted to establish an LC-MS/MS method for measuring perchlorate in dairy products and used this developed method to investigate perchlorate levels in Korean milk and yogurt samples. Methods: The developed method of perchlorate analysis requires a shaker and 1% acetic acid/acetonitrile as the extracting solvent. Briefly, the samples were extracted and then centrifuged (4000 rpm, 1hour), and the supernatant was then passed through a $Envi^{TM}$ Carb SPE cartridge that had been prewashed sequentially with 6 mL of acetonitrile and 6 mL of 1% acetic acid in water. The final volume of the sample extract was adjusted to 40 mL with reagent water and the final sample was filtered through a 0.20-${\mu}m$ pore size PTFE (Polytetrafluoroethylene) syringe filter prior to LC-MS/MS. Results: The average levels of perchlorate in milk and yogurt samples were $5.63{\pm}3.49\;{\mu}g/L$ and $3.65{\pm}2.42\;{\mu}g/L$, respectively. The perchlorate levels observed in milk samples in this study were similar to those reported from China, Japan, and the United States. Conclusions: The exposure of Koreans to perchlorate through the consumption of dairy products was calculated based on the results of this study. For all age groups, the calculated exposure to perchlorate was below the reference of dose (0.7 ${\mu}g/kg$-day) proposed by the National Academy of Science, USA, but the perchlorate exposure of children was higher than that of adults. Therefore, further investigation of perchlorate in other food samples is needed to enable a more exact assessment of exposure of children to perchlorate.

HPLC를 이용한 이중탕 중 3종 활성성분의 동시분석법 확립 (Simultaneous Determination of Three Compounds in Ejung Tang by HPLC-DAD and LC-ESI-MS)

  • 이보형;마진열;원진배;양혜진;윤보라;마충제
    • 생약학회지
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    • 제43권1호
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    • pp.10-15
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    • 2012
  • An accurate and sensitive analysis method was established for simultaneous determination of three bioactive compounds (glycyrrhizin, 6-gingerol and ginsenoside Rg3) in the Ejung Tang with high-performance liquid chromatography (HPLC)-photodiode array detection (DAD)-electrospray ionization (ESI)-Mass spectrometry (MS). The optimizing chromatographic separations a were acquired by an $C_{18}$ column ($5{\mu}m$, $4.6I.D{\times}250mm$, SHISHEDO) using gradient elution with water comprising 0.1% TFA(trifluoroacetic acid) and acetonitrile at a performing temperature of $35^{\circ}C$. Flow rate was 1.0 ml/min. A detection UV wavelength set at 205 nm and 250 nm. The three compounds were identified by electrospray ionization mass spectrometry. All calibration curves indicated great linear regression within test ranges ($R^2>0.9997$). The established method provided acceptable precision and accuracy. The relative standard deviations (RSDs) of intra-day and inter-day were less than 2.00% and 3.00%, respectively. The recoveries were found to range from 94.49 to 101.10% for the three compounds analyzed. These results showed that this method was effective and reliable for quality control of Eiung-Tang.

Association of Fatty Acid Ethyl Esters in Meconium of Neonates with Growth Deficits at Birth: a Prospective, Single-Centre Cohort Study

  • Lee, Hyun-Seung;Kim, Yeon Hee;Kwak, Ho-Seok;Han, Jung-Yeol;Jo, Sun-Jin;Lee, Hae Kook
    • Journal of Korean Medical Science
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    • 제33권50호
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    • pp.318.1-318.10
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    • 2018
  • Background: In this prospective cohort study, we investigated the association between fatty acid ethyl esters (FAEEs) in meconium as biomarkers of prenatal ethanol exposure and growth deficits, as birth outcomes, that constitute several of the key cardinal features of fetal alcohol syndrome. Methods: A total of 157 meconium samples were collected from enrolled infants within 24 hours of birth, and nine FAEEs were quantified using liquid chromatography/tandem mass spectrometry. The relationships between cumulative concentrations of nine species of FAEEs in meconium and birth parameters of growth (age-sex-specific centiles of head circumference [HC], weight, and length) and respective and combined birth outcomes of growth deficits (HC ${\leq}10th$ centile, weight ${\leq}10th$ centile, and length ${\leq}10th$ centile) were determined. Results: Multivariate logistic regression analysis demonstrated that higher cumulative concentrations of meconium FAEEs correlated with elevated risks for HC and length, both, 10th percentile or less (adjusted odds ratio [aOR], 2.94; 95% confidence interval [CI], 1.12-7.74; P = 0.029) and HC and weight and length, all of them, 10th percentile or less (aOR, 3.27; 95% CI, 1.12-9.59; P = 0.031). Conclusion: The elevated cumulative FAEEs in meconium were associated with combined growth deficits at birth, specifically HC and length, both, 10th percentile or less, which might be correlated with detrimental alcohol effects on fetal brain and bone development, suggesting a plausible alcohol-specific pattern of intrauterine growth restriction.

Profiling of differentially expressed proteins between fresh and frozen-thawed Duroc boar semen using ProteinChip CM10

  • Yong-Min Kim;Sung-Woo Park;Mi-Jin Lee;Da-Yeon Jeon;Su-Jin Sa;Yong-Dae Jeong;Ha-Seung Seong;Jung-Woo Choi;Shinichi, Hochi;Eun-Seok Cho;Hak-Jae Chung
    • Journal of Animal Science and Technology
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    • 제65권2호
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    • pp.401-411
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    • 2023
  • Many studies have been conducted to improve technology for semen cryopreservation in pigs. However, computer-assisted analysis of sperm motility and morphology is insufficient to predict the molecular function of frozen-thawed semen. More accurate expression patterns of boar sperm proteins may be derived using the isobaric tags for relative and absolute quantification (iTRAQ) technique. In this study, the iTRAQ-labeling system was coupled with liquid chromatography tandem-mass spectrometry (LC-MS/MS) analysis to identify differentially expressed CM10-fractionated proteins between fresh and frozen-thawed boar semen. A total of 76 protein types were identified to be differentially expressed, among which 9 and 67 proteins showed higher and lower expression in frozen-thawed than in fresh sperm samples, respectively. The classified functions of these proteins included oxidative phosphorylation, mitochondrial inner membrane and matrix, and pyruvate metabolic processes, which are involved in adenosine triphosphate (ATP) synthesis; and sperm flagellum and motile cilium, which are involved in sperm tail structure. These results suggest a possible network of biomarkers associated with survival after the cryopreservation of Duroc boar semen.

Secretome Analysis of Host Cells Infected with Toxoplasma gondii after Treatment of Human Epidermal Growth Factor Receptor 2/4 Inhibitors

  • Kim, Hye-Jung;Ahn, Hye-Jin;Kang, Hyeweon;Park, Jaehui;Oh, Seul gi;Choi, Saehae;Lee, Won-Kyu;Nam, Ho-Woo
    • Parasites, Hosts and Diseases
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    • 제58권3호
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    • pp.249-255
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    • 2020
  • Toxoplasma gondii, a ubiquitous, intracellular parasite of the phylum Apicomplexa, infects an estimated one-third of the human population as well as a broad range of warm-blooded animals. We have observed that some tyrosine kinase inhibitors suppressed the growth of T. gondii within host ARPE-10 cells. Among them, afatinib, human epithermal growth factor receptor 2 and 4 (HER2/4) inhibitor, may be used as a therapeutic agent for inhibiting parasite growth with minimal adverse effects on host. In this report, we conducted a proteomic analysis to observe changes in host proteins that were altered via infection with T. gondii and the treatment of HER2/4 inhibitors. Secreting proteins were subjected to a procedure of micor basic reverse phase liquid chromatography, nano-liquid chromatography-mass spectrometry, and ingenuity pathway analysis serially. As a result, the expression level of heterogeneous nuclear ribonucleoprotein K, semaphorin 7A, a GPI membrane anchor, serine/threonine-protein phosphatase 2A, and calpain small subunit 1 proteins were significantly changed, and which were confirmed further by western blot analysis. Changes in various proteins, including these 4 proteins, can be used as a basis for explaining the effects of T. gondii infections and HER2/4 inhibitors.

Characterization of Canthaxanthin Isomers Isolated from a New Soil Dietzia sp. and Their Antioxidant Activities

  • Venugopalan, Vijayalatha;Tripathi, Subhash K.;Nahar, Pradip;Saradhi, P. Pardha;Das, Rakha H.;Gautam, Hemant K.
    • Journal of Microbiology and Biotechnology
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    • 제23권2호
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    • pp.237-245
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    • 2013
  • Canthaxanthin (cx) is a potent antioxidant that is chemically synthesized at the industrial scale and has imperative applications in the cosmetic and feed industries. An orange pigmented mesophilic bacterium, designated as K44, was isolated from soil samples of Kargil, India. Biochemical tests, 16S rRNA gene sequencing, and FAME analysis of the bacterium indicated it to belong in the genus Dietzia and is distinct from human isolates. The strain showed 98% 16S rRNA gene sequence homology with Dietzia maris DSM 43102. High-performance liquid chromatography profile of the pigments isolated from K44 showed two major peaks absorbing at 465.3 and 475 nm. The liquid chromatography-mass spectrometry (LC-MS) analysis of both these peaks revealed their m/z to be 564. The molecular weights, LC-MS/MS fragmentation patterns, and ${\lambda}_{max}$ of these fractions corresponded to all-trans- (475 nm) and 9-cis-(465.3 nm) cx isomers. The antioxidant activities of cis- and trans-cx isomers isolated from this bacterium were found to differ, where the cis-isomer showed higher free radical, superoxide radical, and reactive oxygen species scavenging activities than the alltrans- isomer, suggesting that 9-cis-cx is more effective as an antioxidant than the all-trans-cx.

Study on Chemical Components of the Aerial Parts and the Roots of Buckwheat

  • Ham, Young-Min;Hyun, Ho-Bong;Yoon, Seon-A;Yoon, Weon-Jong;Yang, Woo-Sam;Oh, Dae-Ju
    • 한국자원식물학회:학술대회논문집
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    • 한국자원식물학회 2018년도 춘계학술발표회
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    • pp.61-61
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    • 2018
  • Buckwheat is a important vegetable in asia for long time. Recently, Buckwheat has attracted attention to its potential for health benefit and especially as a gluten-free food. Conventional buckwheat studies have focused on seeds and sprouts, but we studied the components of the aerial parts and roots of buckwheat after harvesting. Therefore, we hope that this research will be a basic study to expand the application range of buckwheat plants which are discarded after harvesting. The ethanol extracts of aerial part and roots of buckwheat (Daegwan, Yangjul) were analysed using high performance liquid chromatography (HPLC). Rutin was detected as the major compound in Daegwan, Yangjul aerial part and Daegwan root extracts, except yangjul root extract. So we analysed Yangjul root extract using liquid chromatography-mass spectrometry (LC-MS) and then obtained the informations about the components in Yangjul root extract. Yangjul root extract was analysed by $LC-MS^n$ in negative ESI mode within the range m/z 150-2000 amu. Totally, four components was found in the Yangjul root extract and obtained the fragments ion patterns of ones. Further study, we have to confirm the structure of components in Yangjul root extract and try to more biological activity test the components for development as useful food or cosmetic ingredients.

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역삼투압 시스템으로 처리한 포도주의 향기성분 변화 (The Changes of Aroma in Wine Treated with Reverse Osmosis System)

  • 이승룡;이규회;장규섭;이석건
    • 한국식품과학회지
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    • 제32권1호
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    • pp.17-24
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    • 2000
  • 본 연구에서는 날로 그 생산 및 소비량이 중대 되어가는 추세에 있는 포도주의 품질향상을 이루고자 역삼투 처리기술을 이에 적용하여 시도하였는데, 포도주의 제조공정에서 필요로하는 보당과정 없이 역삼투 처리에 의해 포도 착즙액중의 순수(純水)를 제거함으로써 자체 당도를 농인 상태에서 포도주를 제조하여 일반적인 제법으로 제조한 포도주와의 비교 분석 실험을 행하였다. 또한 GC-O(Gas chromatography-Olfactometry)와CC-MS(Gas chromatography-Mass spectrometry) 그리고, 훈련된 검사자들을 통한 관능검사의 실시로 그 차이점을 구명하였는데, 관능검사 결과 RO 28 시료가 General D사(社)의 제품에 비해 전체적인 선호도면에서 월등한 것으로 나타났다. GC-O및 GC-MS를 이용한 분석결과 RO 28시료가 General 및 D사(社) 제품에 비하여 훨씬 긍정적인 향기성분의 함량이 높은 것으로 나타났으며, 비교적 긍정적인 향기성분으로 사료되어지는 ethanol, ethyl acetate 등의 chemical compound를 동정해 낼 수 있었다.

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Development of a Label-Free LC-MS/MS-Based Glucosylceramide Synthase Assay and Its Application to Inhibitors Screening for Ceramide-Related Diseases

  • Fu, Zhicheng;Yun, So Yoon;Won, Jong Hoon;Back, Moon Jung;Jang, Ji Min;Ha, Hae Chan;Lee, Hae Kyung;Shin, In Chul;Kim, Ju Yeun;Kim, Hee Soo;Kim, Dae Kyong
    • Biomolecules & Therapeutics
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    • 제27권2호
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    • pp.193-200
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    • 2019
  • Ceramide metabolism is known to be an essential etiology for various diseases, such as atopic dermatitis and Gaucher disease. Glucosylceramide synthase (GCS) is a key enzyme for the synthesis of glucosylceramide (GlcCer), which is a main ceramide metabolism pathway in mammalian cells. In this article, we developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to determine GCS activity using synthetic non-natural sphingolipid C8-ceramide as a substrate. The reaction products, C8-GlcCer for GCS, could be separated on a C18 column by reverse-phase high-performance liquid chromatography (HPLC). Quantification was conducted using the multiple reaction monitoring (MRM) mode to monitor the precursor-to-product ion transitions of m/z $588.6{\rightarrow}264.4$ for C8-GlcCer at positive ionization mode. The calibration curve was established over the range of 0.625-160 ng/mL, and the correlation coefficient was larger than 0.999. This method was successfully applied to detect GCS in the human hepatocellular carcinoma cell line (HepG2 cells) and mouse peripheral blood mononuclear cells. We also evaluated the inhibition degree of a known GCS inhibitor 1-phenyl-2-decanoylamino-3-morpholino-1-propanol (PDMP) on GCS enzymatic activity and proved that this method could be successfully applied to GCS inhibitor screening of preventive and therapeutic drugs for ceramide metabolism diseases, such as atopic dermatitis and Gaucher disease.

Improved HPLC-UV method for determination of five synthetic dyes in Typha orientalis

  • Ko, Kyung Yuk;Choi, Eun Young;Jeong, Se Hee;Paek, Ock jin;Lee, Chan;Heo, Huijin;Oh, She-Wook;Lee, Chulhyun;Kang, Juhye;Cho, Sooyeul
    • 분석과학
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    • 제34권4호
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    • pp.160-171
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    • 2021
  • Synthetic azo dyes are used extensively in herbal medicines to render the medicines more visually attractive to consumers. This study developed and validated a rapid high-performance liquid chromatography (HPLC) method to determine whether synthetic colorants such as Tartrazine, Auramine O, Metanil yellow, Sunset yellow, and Orange II are used extensively in Typha orientalis. To increase the recovery of the synthetic dyes, this method employed containing 50 mM ammonium acetate in 70 % methanol at first extraction and 100 mM HCl in 70 % methanol at second extraction. Five synthetic pigments in Typha orientalis were separated by gradient elution with a mobile phase consisting of acetonitrile and 50 mM ammonium acetate in distilled water at ultra-violet (UV) detection 428 nm or 500 nm. Additionally, this study established the liquid chromatography tandem mass spectrometry (LC-MS/MS) method to confirm positive samples suspected by HPLC results. The HPLC-UV method had good linearity, indicating r2> 0.999. The recoveries of the samples spiked with three different concentration ranged from 73.8~91.5 %, and relative standard deviation values indicated 0.2~5.2 %. The established LC-MS/MS could successfully identify the synthetic pigments in herbal medicine samples. The study demonstrates that Typha orientalis adulterated by yellowish synthetic dyes can be successfully distinguished when using the HPLC-UV method.