• Title/Summary/Keyword: Gas Chromatography/mass spectrometry

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Changes of Volatiles from Apple Fruits during Maturity and Storage -Part. I. Identification and Determination of Volatiles in the Fruits- (사과 성숙(成熟) 및 저장중(貯藏中) 향기성분(香氣成分)의 변화(變化) -제일보(第一報). 과실(果實) 성숙중(成熟中) 향기성분(香氣成分)의 동정(同定) 및 정량(定量)-)

  • Shim, Ki-Hwan;Sohn, Tae-Hwa;Kim, Myung-Chan;Kang, Shin-Kwoen;Park, Seok-Kyu
    • Applied Biological Chemistry
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    • v.27 no.1
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    • pp.14-20
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    • 1984
  • Volatiles from Mallus pumila Miller Var. Fuji, Ralls Janet and Jonathan during maturity were examined. The volatiles of apples were collected by the headspace trapping method using. Tenax GC and identified by gas liquid chromatography and GC-mass spectrometry. Among over 34 GLC peaks, 23 esters, 9 alcohols and 2 aldehydes were identified. The quantity of volatiles produced was increased in proportion to the degree of maturity, and 1-butanol, isobutyl butyrate, 2-pentanol, ethyl valerate and hexanal were major.

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Quantitative Speciation of Selenium in Human Blood Serum and Urine with AE- RP- and AF-HPLC-ICP/MS

  • Jeong, Ji-Sun;Lee, Jonghae;Pak, Yong-Nam
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3817-3824
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    • 2013
  • Various separation modes in HPLC, such as anion exchange (AE), reversed-phase (RP), and affinity (AF) chromatography were examined for the separation of selenium species in human blood serum and urine. While RP- and AE-HPLC were mainly used for the separation of small molecular selenium species, double column AF-HPLC achieved the separation of selenoproteins in blood serum efficiently. Further, the effluent of AF-HPLC was enzymatically hydrolyzed and then analyzed with RP HPLC for selenoamino acid study. The versatility of the hybrid technique makes the in-depth study of selenium species possible. For quantification, post column isotope dilution (ID) with $^{78}Se$ spike was performed. ORC ICP/MS (octapole reaction cell inductively coupled plasma/mass spectrometry) was used with 4 mL $min^{-1}$ Hydrogen as reaction gas. In urine sample, inorganic selenium and SeCys were identified. In blood serum, selenoproteins GPx, SelP and SeAlb were detected and quantified. The concentration for GPx, SelP and SeAlb was $22.8{\pm}3.4\;ng\;g^{-1}$, $45.2{\pm}1.7\;ng\;g^{-1}$, and $16.1{\pm}2.2\;ng\;g^{-1}$, respectively when $^{80}Se/^{78}Se$ was used. The sum of these selenoproteins ($84.1{\pm}4.4\;ng\;g^{-1}$) agrees well with the total selenium concentration measured with the ID method of $87.0{\pm}3.0\;ng\;g^{-1}$. Enzymatic hydrolysis of each selenium proteins revealed that SeCys is the major amino acid for all three proteins and SeMet is contained in SeAlb only.

Antimicrobial efficacy of endophytic Penicillium purpurogenum ED76 against clinical pathogens and its possible mode of action

  • Yenn, Tong Woei;Ibrahim, Darah;Chang, Lee Kok;Ab Rashid, Syarifah;Ring, Leong Chean;Nee, Tan Wen;Noor, Muhamad Izham bin Muhamad
    • Korean Journal of Microbiology
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    • v.53 no.3
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    • pp.193-199
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    • 2017
  • This study was aimed to evaluate the antimicrobial activity of Penicillium purpurogenum ED76 on several clinically important microorganisms. The endophytic fungus P. purpurogenum ED76 was previously isolated from Swietenia macrophylla leaf. The antimicrobial efficacy of P. purpurogenum ED76 dichloromethane extract was determined via disc diffusion and broth microdilution assay. A kill curve study was conducted and the morphology of extract treated bacterial cells were viewed under scanning electron microscope. The dichloromethane extract showed significant inhibitory activity on 4 test bacteria and 2 test yeasts. The minimal inhibitory concentration of the extract ranged from 125 to $1,000{\mu}g/ml$, which indicates the different susceptibility levels of the test microorganisms to the fungal extract. The kill curve study has revealed a concentration-dependent inhibition for all test microorganisms. With the increase of the extract concentration, the microbial growth was significantly reduced. The scanning electron micrograph of dichloromethane extract-treated Staphylococcus aureus cells showed the total damage of the cells. The cell wall invagination of the bacterial cells also indicates the loss of cellular materials and metabolic activity. The gas chromatography mass spectrometry analysis of the extract also showed that the major compound was stigmasterol, which constitutes 45.30% of the total area. The dichloromethane extract of P. purpurogenum ED76 exhibited significant inhibitory activity on several clinically important bacteria and yeasts. The study proposed a possible mode of action that the extract cause significant damage to the morphology of S. aureus cells.

Effects of NaOH and Humic Acid on the UV Photolysis of PCBs (PCBs의 광화학적 연구: NaOH 및 휴믹산 (humic acid, HA)에 의한 분해특성)

  • Shin, Hae Seung;Kim, Jae Hyoun
    • Journal of Environmental Health Sciences
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    • v.40 no.2
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    • pp.147-156
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    • 2014
  • Objectives: This study was carried out to examine whether the apparent photolysis with or without sensitizers [NaOH and humic acid (HA)] was prompted photodegradation of polychlorinated biphenyl (PCB) in aqueous solution. Methods: PCBs photodegradation occurred using fluorescence black lamps at ${\lambda}_{max}=300nm$. PCB congeners were exposed in 10 ppm HA or 0.05N NaOH solutions, to investigate the decreasing profile of PCB concentration with time. The PCBs were then analyzed by gas chromatography/mass spectrometry (GC-MS). Reductive degradation profile of PCB congeners in the presence of both sensitizers under oxygen-saturated protic conditions was described using the wind-rose diagrams. Results: Use of HA or NaOH decreased PCB concentration with time in the dark and on irradiation, indicating that photolysis underwent through reductive dechlorination through energy transfer and possibly with reactive oxygens. The dechlorination was marked by a chromatographic shift, observed in the GC-MS plots. Therefore it is logical to assume that increasing the dose of sensitizers would increase the photodegradation rates of PCBs. The half-lives of pentachloro-PCB (penta-3) in 0.05N NaOH and 10 ppm HA were estimated at about 47 hours and 39 hours, respectively, under the same experimental conditions of photolysis. It was found that the rate of photolysis of pentachloro-PCB in aqueous solution followed apparent first-order kinetics compared to other congeners. Conclusion: Photochemical degradation (using 328 nm UV light) of penta- and hexa-PCBs in HA or alkaline solution is a viable method for pretreatment method. The results are helpful for the further comprehension of the reaction mechanism for photolytic dechlorination of PCBs in aquatic system.

Evaluation of sewage-derived organic matter using fecal sterols in the sediments from Ulsan Bay and adjacent areas (Fecal sterol을 이용한 울산만과 주변해역 퇴적물내 하수기인 유기물 평가)

  • Choi Minkyu;Choi Hee-Gu;Kim Sang-Soo;Moon Hyo-Bang
    • Journal of Environmental Science International
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    • v.14 no.1
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    • pp.23-32
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    • 2005
  • Surface sediments (0$\~$4 cm) were sampled at 40 stations from Ulsan Bay and its adjacent areas of Korea, to evaluate the contamination by sewage-derived organic matters using fecal sterols. Some sterols were quantified by gas chromatography coupled to mass spectrometry (GC/MS). Total concentrations of eight sterols (co­prostanol, cholesterol, cholestanol, epicholestanol, epicoprostanol, ${\beta}-sitosterol,$ brassicasterol, and stigmasterol) in the sediments from Ulsan Bay and its vicinity varied from 929 to 23,444 ng/g dry weight. The most predom­inant sterols were cholesterol and coprostanol, accounting for $33\~72{\%}$ of total sterols. The concentration of coprostanol known as the indicator of human feces ranged from 141 to 8,257 ng/g dry weight. In particular, the coprostanol concentrations in the sediments from Jansaengpo Harbor and Taehwa River exceeded the value of 1,000 ng/g dry weight, suggesting that these areas could be considered as the hot-spot zones by municipal sewage contamination. Some molecular indices and multivariate data analysis were used to assess the origin of these sterols in the sediments. Results showed that the major routes of sewage contamination in Ulsan Bay and its vicinity were the input through Jansaengpo Harbor and Taehwa River.

GC-MS Analysis of Organophosphorus Pesticide Residue in Seawater From the Kwangyang Bay, Korea (광양만 해수 중 유기인 잔류 농약성분의 GC-MS 분석)

  • Park, Mi-Ok;Park, Jeom-Sook
    • Journal of Environmental Science International
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    • v.15 no.4
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    • pp.293-304
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    • 2006
  • Sea water samples collected in August, 1994 from 20 stations in the Kwangyang Bay were analyzed by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) to investigate persistence and distribution pattern of four organophosphorus pesticides (DDVP, Diazinon, IBP, EDDP). Except for IBP, the contamination by DDVP, Diazinon, and EDDP in marine aquatic environment in Korea has not been reported previously. In this study, however, all these four pesticides were detected in all stations (except DDVP) and their concentrations were in ng/L level. The concentrations ranged from detection limit to 15.3ng/L for DDVP, 1.8-27.7ng/L for Diazinon, 7.3-63.5ng/L for IBP, and 22.2-1100.1ng/L for EDDP. It is noteworthy that the measured concentrations of IBP and EDDP in this study would be much lower than usual, since the use of IBP and EDDP was less than 50% of average annual consumption due to unusually dry and hot weather condition in the summer of 1994. It was very surprising to find that the highest concentrations of organophosphorus pesticides were observed at stations near Daesa Streamlet instead of Seomjin River, which has more point source of the pesticides. This result suggests that the small river discharge during heavy ram period in summer can give harmful effect on marine biota (both wild and aqua-cultured) with its organophosphorus pesticide residue, despite of their short residence time in aquatic environment. In order to protect the marine life properly from acute toxicity of the organophosphorus pesticides, it needs to be emphasized that monitoring the level of agricultural pesticides in river run-off should be done during active consumption period rather at regular intervals.

Autoxidative Stability of Triglyceride Molecular Species (트리글리세리드 분자종의 산화안정성에 관한 연구)

  • Yoon, Hyeung-Sik;Kim, Seon-Bong;Park, Yeung-Ho
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.18 no.2
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    • pp.205-210
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    • 1989
  • The influence of triglyceride molecular species on autoxidation was investigated by determining the residual molecular species after incubating soybean oil triglycerides. The molecular species of soybean oil triglycerides were analyzed by capillary column gas chromatography and electron impact ionization mass spectrometry utilizing selected ion monitoring. The autoxidative stability of each molecular species in soybean oil triglycerides appeared to decrease in proportion to the increase in the number of double bonds present in the acyl residues, and it was affected by degree of unsaturation of fatty acid when the number of double bonds in triglyceride were the same. And it appeared to be enhanced by a decreases in the length of the saturated acyl chain present in the glycerides.

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Chemical and Textural Properties in Commercial Fermented Soybean Curds of Sufu

  • Kim, Joo-Shin;Lu, Ying;Chung, Hau-Yin
    • Preventive Nutrition and Food Science
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    • v.16 no.1
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    • pp.55-61
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    • 2011
  • A survey aiming to find out the chemical and textural properties of commercial fermented soy bean curd called sufu was conducted. Sixteen brands of plain sufu produced in the Northern or the Southern part of China were collected and examined for their crude protein, crude fat, texture profiles, free amino acids, and free fatty acid contents. Twenty-one free amino acids were extracted and derivatized using a commercial kit followed by separation and analyzed by the gas chromatography-mass spectrometry (GC-MS). Similarly, ten free fatty acids were extracted using alumina, eluted, separated and analyzed. The content ranges of crude fat and protein were 22~36% and 31~38%, respectively. In texture profile analysis, ranges of the texture parameters were 131~493 g (hardness), 0.4~0.5 (cohesiveness), -137 to -50 gs (adhesiveness), 0.6~1 (springiness), 47~220 g (gumminess) and 32~177 g (chewiness). Twenty-one different free amino acids, especially alanine, glycine, $\alpha$-aminobutyric acid, valine, leucine, allo-isoleucine, aspartic acid, glutamic acid and lysine in large amount, as well as ten fatty acids in total, notably linoleic acid (9-octadecanoic acid), oleic acid (9,12-octadecadienoic acid), linolenic acid (9,12,15-octadecadienoic acid), hexadecanoic acid and octadecanoic acid were found. This information provides important quality reference ranges for product developers and manufacturers to optimize and produce the plain sufu.

Levels of PBDEs in Pig Feed (축산물 사료중의 Polybrominated Diphenyl Ethers(PBDEs) 평가)

  • Shin, Jeoung-Hwa;Ahn, Yun-Gyong
    • The Korean Journal of Community Living Science
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    • v.23 no.3
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    • pp.255-263
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    • 2012
  • Polybrominated diphenyl ethers (PBDEs) are a group of brominated flame retardants (BFRs), which are used in a variety of consumer products. Several of those are produced in large quantities. Their chemical structure similarities to polychlorinated dibenzo-p-dioxins and polychlorinated biphenyls (PCBs), as well as their toxicity, has been studied. PBDEs are persistent and lipophilic, which results in their bioaccumulation in the fatty tissues of organisms and enrichment throughout food chains. In addition, a number of studies also reported high levels of PBDEs in animals and food resulting from the use of contaminated animal feed Public concern about PBDEs levels in animals and food has been raised. Feed contamination by toxic chemicals has been the cause of the contamination of poultry products. The purpose of this study was to evaluate PBDEs in pig feed to search the origin chase of POPs in pigs. Feed samples were obtained wheat from East Europe, corn from South America and America, soybean meal from Korea, America, South America and India and tallow from Korea. The preparation of samples was based on the EPA method 1614. Instrumental analysis was based on the use of high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC/HRMS). Quantification was carried out by the isotopic dilution method. The analysis of ${\Sigma}PBDEs$ involved 22 PBDE congeners, including BDE-17, 28, 47, 49, 66, 71, 77, 85, 99, 100, 119, 126, 138, 153, 154, 156, 183, 184, 190, 191, 196 and 197.

Evaluation for Concentration of Residual PCDD/Fs in Pig Feed (돼지사료 중의 다이옥신 잔류 평가)

  • Ahn, Yun-Gyong;Shin, Jeoung-Hwa
    • The Korean Journal of Community Living Science
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    • v.23 no.2
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    • pp.129-136
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    • 2012
  • Dioxins are chemical substances that are not properly decomposed degradation under natural photochemical, biological and chemical conditions in the environment, and bio-accumulate through the food chain, so pose a risk of causing adverse effects to human health and the environment. Ninety seven percent of human exposure to dioxins comes through meat, fish, dairy consumption and so on. Pork is the largest proportion meat aspect of daily intake in the Korean food. Pigs are three times more than Cattle in terms of breeding population and production amount in the world, and the amount is increasing every year. Therefore, it is necessary to monitor the exposure level of dioxins in pig's body. Also, it is required to evaluate the presence of these chemical substances in the pig's feed grain such as corn, soybeans, and tallow. The purpose of this study was to evaluate PCDD/Fs in pig's feed to search the origin of PCDD/Fs. Feed samples obtained were wheat from East Europe, corn from South America and America, soybean meal from Korea, America, South America and India and tallow from Korea. The preparation of samples was based on the EPA method 1613. Instrumental analysis was based on the use of high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC/HRMS). The concentrations of 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) and 1,2,3,7,8-pentachlorodibenzo-p-dioxin (PCDD), which are the most toxic potent dioxins, were not observed in any of the samples. However OCDD was detected in most of the samples. The TEQs in the feed samples were ranged from 0 pg TEQ/g to 0.09841 pg TEQ/g. Especially, the high level of TEQs was observed in the samples of wheat from East Europe and soybean meal from Korea.