• 한국지역사회생활과학회지
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• 제23권2호
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• pp.199-206
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• 2012

In order to evaluate the aroma compounds in Korean traditional alcoholic beverages, volatile compounds of the commercial wines, Makgeolli were analyzed and quantified using the conventional method. Eight volatile compounds including three kinds of alcohols, two kinds of organic acids and three kinds of ether were extracted by Liquid-Liquid Extraction with Dichloromethane. For the separation and quantification, Gas chromatography coupled with mass spectrometry (GC/MS) was used to analyze these compounds. Also, the separation efficiency of these compounds was performed and compared with GC column. The results of this study were as follows ; Eight kinds of volatile compounds were separated well on the HP-88 column better than on the DB-5MS column. Short chain fatty acids, butyric acid and isovaleric acid were not detected in two brands of makgeolli samples. The higher alcohols were detected in the range of 0.86~225.68 ${\mu}g/mL$ and ethyl esters were detected in the range of 0.86~225.68 ${\mu}g/mL$, respectively. There compounds are known to be associated with sensory and odorant.

• 한국식품과학회지
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• 제41권3호
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• pp.326-333
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• 2009

국내에서 주로 섭취되는 어패류(고등어, 삼치, 조기, 대합, 바지락, 꼬막, 백합)를 가열조리 하였을 때 형성되는 HCAs를 분리, 동정하여 그 함량을 모니터링 하였다. 추출 및 정제는 고체상 추출 방법을 사용하였고 정성, 정량을 위한 분석장비는 LC/MS를 사용하였다. 모니터링 결과 생선류에서는 고등어(2.2-1,1117.7 ng/g), 삼치(9.1-443.6 ng/g), 조기(17.5-179.5 ng/g)순으로 HCAs가 많이 검출되었으며 특히 고등어 muscle에서 많은 양(1,1117.7 ng/g, Harman)이 검출되었다. 조개류 중에서는 대합(12.2-196.4 ng/g), 꼬막(2.2-76.2 ng/g), 바지락(1.7-25.8 ng/g), 백합(1.5-2.7 ng/g)순으로 많이 검출되었으며 대합의 Norharman(196.4 ng/g)이 가장 많이 검출되었다. 15종의 HCAs 중 ${beta}$-carbolines에 속하는 Norharman과 Harman이주로 검출되었으며 그 밖에 PhIP, Trp-P-1. Trp-P-2 등의 발암가능성이 있는 물질들이 검출되었다. 조리방법 측면에서 보면 간장을 이용한 조림방법보다는 직접적인 가열을 통한 구이방법이 많은 양의 HCAs를 형성시켰으며 구이 중에서도 muscle만 있는 부위에서의 검출함량보다는 muscle과 skin이 함께 있는 부위에서 검출함량이 더 많았다. 가열 조리한 어패류 분석방법에 대한 유효성을 확인해 본 결과 정량한계는 0.8-23.9 ng/mL, 검출한계는 0.2-7.2 ng/mL이었으며 회수율은 15.7-74.7%이었다.

• 한국어병학회지
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• 제34권1호
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• pp.71-80
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• 2021

세팔로스포린계열의 반합성 항생제인 세팔렉신은 법적 허가를 받은 여러 나라의 양식장에서 사용되어 왔다. 따라서 이 항생제는 갑각류 중 흰다리새우와 같은 어류를 제외한 다른 수생 생물 종에서 광범위하게 사용할 수 있다. 본 연구는 흰다리새우에서 세팔렉신의 잔류기간 설정을 위해 잔류분석법을 개발하였고, 이를 바탕으로 잔류실험을 수행하였다. 분석법 개발을 위하여 이미 존재하고 있는 여러 식용동물 조직에서의 분석법을 바탕으로 반복 시도하여 고성능 액체 크로마토그래피와 질량분석기(high-performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)를 이용한 분석법을 개발하였다. 그 결과, 0.1 mg/kg의 농도에서 회수율이 81.79%, C.V.값은 8.2%로 Codex guideline에서 권장하는 회수율 및 C.V.에 충족하는 결과를 나타내었다. 개발한 분석법의 적정성을 검증 후, 흰다리새우에 세팔렉신을 경구투여 한 뒤 잔류량을 분석하여 흰다리새우 조직에서의 적용 가능성을 확인하였다. 그 결과, 투여 종료 3일 후에 대부분의 근육 시료에서 정량한계(0.05 mg/kg)이하로 검출되었고, 투여 종료 14일 후에 대부분의 간췌장 시료에서 정량한계 이하로 검출되었다. 특히 본 연구에서 개발한 분석법에서 설정된 정량한계(0.05 ppm)는 어류에서 법적으로 설정된 잔류허용 기준 0.2 mg/kg에 대해 충분한 감도를 나타낸다.

• Journal of Pharmaceutical Investigation
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• 제41권2호
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• pp.91-94
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• 2011

The purpose of this study was to investigate the effect of peptide charge on the interaction between peptide and poly(D,L-lactide-co-glycolide) (PLGA) for evaluating mechanism of acylated peptide formation in PLGA matrix. As a model peptide, octreotide, a synthetic somatostatin analogue and active ingredient of commercial PLGA product, was used. The disulfide group of octreotide was reduced with dithiothreitol and the sulfhydryl groups were modified with N-${\beta}$-maleimidopropionic acid (BMPA) to neutralize octreotide with positive charge in physiological conditions. The BMPA-conjugated octreotide was identified by measuring the molecular mass with liquid chromatography-mass spectrometry. In the interaction study with PLGA, native octreotide showed initial adsorption to PLGA and substantial production of acylated peptides (56% of overall peptide), whereas BMPA-conjugated octreotide showed minimal adsorption to PLGA and no acylation products for 42 days. Consequently, the neutralization of octreotide completely inhibited the peptide acylation by preventing interaction of peptide with PLGA. In conclusion, this study demonstrates that the initial polymer interaction of peptide is important step for peptide acylation in PLGA matrix and suggests the modulation of peptide charge as strategy for inhibiting the formation of acylated peptide impurities.

• Bulletin of the Korean Chemical Society
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• 제32권2호
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• pp.524-530
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• 2011

In the present study, we demonstrate that SRM LC-MS/MS method developed by Luo et al. (ref. 10) can be successfully applied to the quantitative analysis of intracellular metabolites in E. coli that are collected at the exponential and stationary growth phases. A focus is given on measuring the changes in the concentrations of intracellular metabolites in batch cultures, which were induced during both the dynamically changing exponential and stationary growth phases. The following intracellular metabolites are quantified in the exponential and stationary phases of E. coli growth, using the SRM mode of a triple quadrupole mass spectrometer: glucose-1-phosphate, fructose-1,6-bisphosphate, phosphoenolpyruvate, pyruvate, acetyl-coenzyme A, 6-phosphogluconate, ribulose-5-phosphate, xylulose-5-phosphate, erythrose-4-phosphate. The determined intracellular metabolite concentration profiles are shown to be in a good agreement with the growth profiles of E. coli, which clearly indicates that SRM LC-MS/MS can be successfully used for following the metabolite changes induced at different growth stages.

• 한국산업보건학회지
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• 제26권4호
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• pp.396-403
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• 2016

Objectives: The study is to evaluate biological monitoring and risk assessment for epichlorohydrin-bisphenol A resin exposed from waterproofing or finishing work in the apartment building construction. Methods: Subjected workers were working on spray-painting and waterproofing work for 8 hours per day every 20 days. The urine samples were collected at the end of 20 days working period. For urinary bisphenol A as metabolite from epichlorohydrin-bisphenol A exposure, urine samples were analyzed with liquid chromatography mass-mass spectrometry(HPLC-MS/MS). Results: Geometric means of urinary bisphenol A(BPA) with no hydrolysis and with enzymic hydrolysis(BPA-EH) in the workers were $1.10{\mu}g/L$ and $2.90{\mu}g/L$. BPA-EH was 4 times higher than that of control group. The factors for working period and ages did not affect the variation of BPA and BPA-EH. The levels for BPA and BPA-EH were not higher than 95th percentile for exposure on human-life environment. Conclusions: The BPA and BPA-EH were therefore effective biological markers for epichlorohydrin-bisphenol A exposure workers, but not seem to hazardous exposure level. Waterproofing work in construction workshop is required to measuring work environment and health care management for the workers.

• Bulletin of the Korean Chemical Society
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• 제35권1호
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• pp.158-164
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• 2014

Substance P and neuropeptide Y were discovered as early diagnostic biomarkers of acute myocardial infarction in Korean patients and confirmed using enzyme-linked immunosorbent assay (ELISA). We screened 12 peptides from the sera of Korean acute myocardial infarction (AMI) patients and detected 3 peptides (neuropeptide Y, substance P, and N-terminal pro-B-type natriuretic peptide) to be elevated from patients' sera by liquid chromatography mass/mass spectrometry. The elevated concentration of 3 peptides was confirmed by ELISA. The screening results revealed the substance P, neuropeptide Y, and pro-B-type natriuretic peptide (47-76) concentrations were higher in patients' sera than in healthy controls. The sensitivity and specificity of substance P for AMI diagnostic marker were 80% and 83%, respectively, and those of neuropeptide Y were 87% and 90%, respectively compared to healthy controls. These results suggest that substance P and neuropeptide Y could be used as early diagnostic biomarkers in patients with AMI.

• 한국축산식품학회지
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• 제36권2호
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• pp.254-261
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• 2016

The purpose of this study was to analyze oxidized methionines in the myosin isoforms of porcine longissimus thoracis, psoas major, and semimembranosus muscles by liquid chromatography (LC) and mass spectrometry (MS). A total of 836 queries matched to four myosin isoforms (myosin-1, -2, -4, and -7) were analyzed and each myosin isoform was identified by its unique peptides (7.3-13.3). Forty-four peptides were observed from all three muscles. Seventeen peptides were unique to the myosin isoform and the others were common peptides expressed in two or more myosin isoforms. Five were identified as oxidized peptides with one or two methionine sulfoxides with 16 amu of mass modification. Methionines on residues 215 (215), 438 (438), 853 (851), 856 (854), 1071 (1069), and 1106 (1104) of myosin-1 (myosin-4) were oxidized by the addition of oxygen. Myosin-2 had two oxidized methionines on residues 215 and 438. No queries matched to myosin-7 were observed as oxidized peptides. LC-MS/MS allows analysis of the oxidation of specific amino acids on specific residue sites, as well as in specific proteins in the food system.

• 대한화학회지
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• 제68권3호
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• pp.139-145
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• 2024

This study aims to elucidate the mechanism involved in the hydrolysis of the hexacyanoferrate(III) complex ion (Fe(CN)₆^3-) and the mechanism leading to the formation of Prussian blue (Fe^III₄[Fe_II(CN)₆]₃·xH₂O, PB) in acidic aqueous solutions at moderately elevated temperatures. Hydrolysis constitutes a crucial step in generating PB through the widely used single-source or precursor method. Recent PB syntheses predominantly rely on the single-source method, where hexacyanoferrate(II/III) is the exclusive reactant, as opposed to the co-precipitation method employing bare metal ions and hexacyanometalate ions. Despite the widespread adoption of the single-source method, mechanistic exploration remains largely unexplored and speculative. Utilizing UV-vis spectrophotometry, negative-ion mode liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS), and a devised reaction, this study identifies crucial intermediates, including aqueous Fe^2+/3+ ions and hydrocyanic acid (HCN) in the solution. These two intermediates eventually combine to form thermodynamically stable PB. The findings presented in this research significantly contribute to understanding the fundamental mechanism underlying the acid-catalyzed hydrolysis of the hexacyanoferrate(III) complex ion and the subsequent formation of PB, as proposed in the sequential mechanism introduced herein. This finding might contribute to the cost-effective synthesis of PB by incorporating diverse metal ions and potassium cyanide.

• Journal of Pharmaceutical Investigation
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• 제38권4호
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• pp.269-275
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• 2008

The purpose of the present study was to evaluate the bioequivalence of two levofloxacin tablets, Jeil $Cravit^{TM}$ tablet (Jeil Pharm. Co., Ltd., Korea, reference drug) and $Lesacin^{TM}$ tablet (Ilhwa. Co., Ltd., Korea, test drug), according to the guidelines of Korea Food and Drug Administration (KFDA). Twenty-four healthy male Korean volunteers received two tablets containing levofloxacin 200 mg in a $2{\times}2$ crossover study. There was a one-week washout period between the doses. Plasma concentrations of levofloxacin were monitored for over a period of 24 hr after administration by using a high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The area under the plasma concentration-time curve from time zero to 24 hr ($AUC_t$), maximum plasma drug concentration ($C_{max}$) and time to reach $C_{max}\;(T_{max})$ were complied from the plasma concentration-time data. Analysis of variance (ANOVA) test was utilized for the statistical analysis of the parameters using logarithmically transformed $AUC_t$ and $C_{max}$. The 90% confidence intervals of the $AUC_t$ ratio and the $C_{max}$ ratio for $Lesacin^{TM}$/Jeil $Cravit^{TM}$ were $\log\;0.9527{\sim}\log\;0.9981$ and $\log\;0.8712{\sim}\log\;1.0556$, respectively. These values were within the acceptable bioequivalence intervals of $\log\;0.80{\sim}\log\;1.25$, recommended by KFDA. In all of these results, we concluded that $Lesacin^{TM}$ tablet was bioequivalent to Jeil $Cravit^{TM}$ tablet, in terms of rate and extent of absorption.