• 한국자연치유학회지
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• 제10권2호
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• pp.108-113
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• 2021

배경: 속새 줄기와 뿌리의 추출물에서 항산화 물질의 작용에 관한 결과를 이미 보고하였으나 항산화 성분은 분석되지 않았다. 목적: 속새 줄기와 뿌리 부분의 성분을 추출한 물질들이 항산화 물질의 분자 구조를 확인하는 것이었다. 방법: 성분분석은 열수와 에틸알코올로 추출하여 HPLC와 LC-MS로 분석하였다. 결과: 속새 줄기와 뿌리 추출물의 HPLC 크로마토그램은 파장 205 nm에서 4개의 중요한 peak가 나타났다. 280 nm에 있는 peak 1번은 전형적인 단순 페놀릭형이고, 모두 280 nm와 370 nm 근처에 있는 peak 2~4는 전형적인 플라보노이드 배당체의 형태임을 알 수 있었다. HPLC 분석에 의한 추출물의 항산화도는 740 nm에서 peak의 합은 100% 에탄올 추출물이 3,669 mAU로 제일 높았고, 70% 에탄올 추출물은 3,096 mAU, 열수추출물은 2,868 mAU로 제일 낮았다. 항산화성 추출 물질을 LC-MS 분석한 결과는 peak 3에서는 분자량이 772 da인 kaempferol-3-sophoroside-7-glucoside, peak 4에서는 분자량이 788과 772인 물질 kaempferol-3- sophoroside- 8-glucoside가 확인되었다. 결론: 속새의 항산화 추출물에 항산화 성분이 존재하는 것이 확인되어 속새가 기능성 화장품의 원료로서 가능성이 높아 졌다고 본다.

• Mass Spectrometry Letters
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• 제5권2호
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• pp.52-56
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• 2014

Glycated hemoglobin (HbA1c) is used as an index of mean glycemia over prolonged periods. This study describes an optimization of enzyme digestion conditions for quantification of non-glycated hemoglobin (HbA0) and HbA1c as diagnostic markers of diabetes mellitus. Both HbA0 and HbA1c were quantitatively determined followed by enzyme digestion using isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) with synthesized N-terminal hexapeptides as standards and synthesized isotope labeled hexapeptides as internal standards. Prior to quantification, each peptide was additionally quantified by amino acid composition analysis using ID-LC-MS/MS via acid hydrolysis. Each parameter was considered strictly as a means to improve digestion efficiency and repeatability. Digestion of hemoglobin was optimized when using 100 mM ammonium acetate (pH 4.2) and a Glu-C-to-HbA1c ratio of 1:50 at $37^{\circ}C$ for 20 h. Quantification was satisfactorily reproducible with a 2.6% relative standard deviation. These conditions were recommended for a primary reference method of HbA1c quantification and for the certification of HbA1c reference material.

• Mycobiology
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• 제38권4호
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• pp.302-309
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• 2010

Formic acid is a representative carboxylic acid that inhibits bacterial cell growth, and thus it is generally considered to constitute an obstacle to the reuse of renewable biomass. In this study, Saccharomyces cerevisiae was used to elucidate changes in protein levels in response to formic acid. Fifty-seven differentially expressed proteins in response to formic acid toxicity in S. cerevisiae were identified by 1D-PAGE and nano-liquid chromatography-tandem mass spectrometry (nano-LC-MS/MS) analyses. Among the 28 proteins increased in expression, four were involved in the MAP kinase signal transduction pathway and one in the oxidative stress-induced pathway. A dramatic increase was observed in the number of ion transporters related to maintenance of acid-base balance. Regarding the 29 proteins decreased in expression, they were found to participate in transcription during cell division. Heat shock protein 70, glutathione reductase, and cytochrome c oxidase were measured by LC-MS/MS analysis. Taken together, the inhibitory action of formic acid on S. cerevisiae cells might disrupt the acidbase balance across the cell membrane and generate oxidative stress, leading to repressed cell division and death. S. cerevisiae also induced expression of ion transporters, which may be required to maintain the acid-base balance when yeast cells are exposed to high concentrations of formic acid in growth medium.

• 한국식품영양학회지
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• 제35권6호
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• pp.543-551
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• 2022

There has been increased interest in lignans due to their potential effect in reducing the risk of developing several diseases. To evaluate lignan contents, sensitive and accurate methods should be developed for their quantification in food. The present study aimed to validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantification of 5 lignans: lariciresinol (Lar), matairesinol (Mat), pinoresinol (Pin), secoisolariciresinol (Seco), and syringaresinol (Syr). The validation included selectivity, linearity, recovery, accuracy, and precision. The method was proved to be specific, with a linear response (R²≥0.99). The limits of detection were 0.040~0.765 ㎍/100 g and the limits of quantification were 0.114~1.532 ㎍/100 g. Recoveries were 90.588~109.053% for black sesame powder. Relative standard deviations of repeatability and reproducibility were below 5%. Total lignan contents of roasted coffee bean, oat, and blacksoy bean were 105.702 ㎍/100 g, 78.965 ㎍/100 g, and 165.521 ㎍/100 g, respectively. These results showed that LC-MS/MS analysis would be effective in producing acceptable sensitivity, accuracy, and precision in five lignan analyses.

• Bulletin of the Korean Chemical Society
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• 제33권5호
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• pp.1681-1685
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• 2012

A sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed to determine valproic acid in human red blood cell (RBC). It is important to measure the drug concentration of the RBC as well as that of the plasma because of drug partitioning for pharmacokinetic and pharmacodynamic study. The method was linear over the dynamic range of 1-100 ${\mu}g$/mL with a correlation coefficient $r$ = 0.9997. The linearity of this method was established from 1 to 100 ${\mu}g$/mL for valproic acid in red blood cell with accuracy and precision within 15% at all concentrations. The intra-run and inter-run assay accuracy and coefficient of variations are all within 15% for all QC samples prepared in plasma and red blood human samples. Then, valproic acid amount by protein precipitation in plasma was quantified by LC-MS/MS mass spectrometry. The distribution ratio of VPA in RBC and plasma was analyzed by clinical samples. Based on measurement of the valproic acid in human red blood cell, this method has been applied to clinical research for study of distribution ratio of valproic acid in blood.

• 한국동물위생학회지
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• 제30권1호
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• pp.13-21
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• 2007

An atmospheric pressure chemical ionization (APcI) LC/MS/MS method was developed for the simultaneous analysis of fluoroquinolones (norfloxacin, ciprofloxacin, enrofloxacin, danofloxacin) residues in eggs. The spiked and blank samples were extracted from whole eggs using 50mM phosphate buffer (pH 7.4). The extract was cleaned up by passage though $Oasis^{(R)}$ MAX extraction cartridge for solid-phase extraction followed by elution with 4% formic acid in methanol. The extract of sample was separated on a Waters $Atlantis^{TM}$ $dC_{18}$ reversed-phase column ($4.6{\times}150mm,\;5{\mu}m$) and analyzed by APcI positive mode mass spectrometry. The mobile phase consists of aqueous 0.2% nonafluoropentanoic acid (NFPA) and methanol. Multiple reaction monitoring (MRM) using the precursor to product ion combinations of m/z $320\;{\dashrightarrow}\;302,\;332\;{\dashrightarrow}\;314,\;360\;{\dashrightarrow}\;342$ and m/z $358\;{\dashrightarrow}\;340$ were used to quantify norfloxacin (NOR), ciprofloxacin (CIP), enrofloxacin (ENR) and danofloxacin (DAN), respectively. The limits of quantification (LOQ) were 7.8ppb for NOR, 8.5ppb for CIP, 8.9ppb for ENR, and 4.8ppb for DAN. Average recoveries of fortified sample at levels of 0.025 to 0.1 ppm were estimated 71.29% for NOR, 75.27% for CIP, 85.51% for ENR and 81.22% for DAN. These results could be applied for the confirmation and quantification in eggs.

• Asian Pacific Journal of Cancer Prevention
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• 제16권3호
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• pp.1011-1018
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• 2015

This study was conducted to investigate the plasma phosphoproteome and differential plasma phosphoproteins in cases of of Opisthorchis viverrini (OV)-related cholangiocarcinoma (CCA). Plasma phosphoproteomes from CCA patients (10) and non-CCA subjects (5 each for healthy subjects and OV infection) were investigated using gel-based and solution-based LC-MS/MS. Phosphoproteins in plasma samples were enriched and analyzed by LC-MS/MS. STRAP, PANTHER, iPath, and MeV programs were applied for the identification of their functions, signaling and metabolic pathways; and for the discrimination of potential biomarkers in CCA patients and non-CCA subjects, respectively. A total of 90 and 60 plasma phosphoproteins were identified by gel-based and solution-based LC-MS/MS, respectively. Most of the phosphoproteins were cytosol proteins which play roles in several cellular processes, signaling pathways, and metabolic pathways (STRAP, PANTHER, and iPath analysis). The absence of serine/arginine repetitive matrix protein 3 (A6NNA2), tubulin tyrosine ligase-like family, member 6, and biorientation of chromosomes in cell division protein 1-like (Q8NFC6) in plasma phosphoprotein were identified as potential biomarkers for the differentiation of healthy subjects from patients with CCA and OV infection. To differentiate CCA from OV infection, the absence of both serine/threonine-protein phosphatase 2A 56 kDa regulatory subunit beta isoform and coiled-coil domain-containing protein 126 precursor (Q96EE4) were then applied. A combination of 5 phosphoproteins may new alternative choices for CCA diagnosis.

• 한국수산과학회지
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• 제44권1호
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• pp.45-49
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• 2011

As a first step toward identifying a new method for testing sea snail tissue for toxins, and thus prevent food poisoning due to the ingestion of contaminated snails, we measured the tetramine [$(CH_3)_4N^+$] contents of sea snails from the Korean coast using both liquid chromatography-tandem mass spectrometry (LC-MS/MS) and ion chromatography. For tetramine tested, good linearity ($r^2$ = 0.9996) was observed between the amounts in the injected samples and the peak areas of standard toxins, which ranged from 0.1 to 100 ng. The recovery (%) of tetramine from spiked tissue and mid-gut gland samples ranged from 84.0 to 95.3%. The quantitative results for tetramine using this method were in good agreement with the theoretical values. LC-MS/MS has both high sensitivity and selectivity, which makes it possible to measure trace quantities of tetramine in samples.

• 약학회지
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• 제60권3호
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• pp.112-117
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• 2016

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of caffeine in forensic aqueous sample. The centrifuged sample ($100{\mu}l$) was diluted 50-fold with distilled water. The diluted sample ($400{\mu}l$) was then diluted further with $200{\mu}l$ of 0.1% formic acid solution and $400{\mu}l$ of acetonitrile containing 500 ng of caffeine-(3-methyl-$^{13}C_3$) prior to LC-MS/MS analysis. The mobile phase was composed of 0.1% formic acid in distilled water (A) and acetonitrile (B). Chromatographic separation was performed by using a Zorbax SB-C18 ($100mm{\times}2.1mm$ i.d., $3.5{\mu}m$) column and caffeine was eluted within 1.1 min. Linear least-squares regression with a 1/x weighting factor was used to generate a calibration curve with the coefficients of determination ($r^2=0.9983$). The lower limit of quantification was $25ng/ml$ for the analyte. The process efficiency was 98.6~100.1%. Intra- and inter-day precisions were not more than 2.1% and 1.7%, while intra- and inter-day accuracies were ranged from -6.8 to 4.5%, respectively. The suitability of the method was examined by analyzing unknown forensic aqueous samples.

• KSBB Journal
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• 제31권1호
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• pp.1-7
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• 2016

Changes in the concentrations of glucosinolates and related compounds in different extracts of Dolsan leaf mustard kimchi (DLMK) and Dolsan leaf mustard pickles (DLMP) were during storage investigated. Samples were kept at 0oC for 35 days and collected at 7 day intervals. The leaves and stems of DLMK and DLMP were refluxed for 24 h with 50% acetonitrile, and the extracts were analyzed by LC-PDA/MS/MS. The main glucosinolates detected in DLMK were sinigrin, gluconapoleiferin, glucobrassicanapin, and gluconapin, whereas those in DLMP were sinigrin, gluconapoleiferin, glucobrassicanapin, glucobrassicin, and glucoerucin. Sinigrin concentrations were quantified by UV absorption at 228 nm. Sinigrin concentrations in the leaves and stems of DLMK on the day of preparation were 2.14 mg/g and 2.25 mg/g, respectively, and those on day 35 after preparation were 1.25 mg/g and 1.00 mg/g, respectively. DLMP showed a similar trend: the concentrations in the leaves and stems on the day of preparation were 2.04 mg/g and 0.29 mg/g, respectively, whereas those on day 35 after preparation were 0.59 mg/g and 0.41 mg/g, respectively. Thus, sinigrin concentrations decreased during storage.