• Title/Summary/Keyword: chromatography test

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An Inter-Laboratory Comparison Study on Chlorophyll a Determination in Seawater (해수 중 엽록소 a 측정방법에 대한 실험실 간 비교연구)

  • Moon, Cho-Rong;Kang, Dong-Jin;Park, Mi-Ok;Noh, Jae Hoon;Yoo, In-Jae;Moon, Jeong-Eon;Shin, Kyung-Hoon;Kim, Yun Sook;Choi, Joong-Ki;Suh, Young Sang
    • The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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    • v.19 no.1
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    • pp.76-87
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    • 2014
  • Chlorophyll a in seawater which is an indicator of phytoplankton biomass and primary production is determined by High Performance Liquid Chromatography (HPLC), Fluorometry and Spectrophotometry. In this study, various methods for chlorophyll a determination in seawater are compared using in situ seawater samples from Korean seas. Three inter-laboratory comparison campaigns were carried out using chlorophyll a standard samples (R0) and in situ seawater samples, collected from the East China Sea (R1) and the East Sea (R2). 6 laboratories by HPLC methods, 4 laboratories by fluorometry, and 3 laboratories by spectrophotometry participated. Precisions, defined as the coefficient of variation (CV) were within 9% in standard samples, 0.8~20% (average: 6.1%) in R1, 4~21% (average: 13.2%) in R2. Discrepancy in three methods was approximately 20% within the range of the sample homogeneity intended the laboratory precision (R1: 8%, R2: 15%). The discrepancy in laboratories was greater than the discrepancy in methods. The chlorophyll a concentrations can be produced within 20% discrepancy in spite of using different methods. It is recommended to consider this 20% discrepancy when using the chlorophyll a data produced by different laboratories and different methods.

Study on Reesterification of Rice Bran Oil Containing High Free Fatty Acids and Glycerol (유리지방산을 많이 함유한 미강유와 글리세린의 에스테르화 반응에 관한 연구)

  • Moon, Sung-Hoon;Rhee, Joon-Shick
    • Korean Journal of Food Science and Technology
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    • v.12 no.3
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    • pp.193-199
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    • 1980
  • A series of tests were conducted on the reesterification of rice bran oil containing high free fatty acids (acid value=119.7) with theoretical equivalent of glycerol. Test results showed that reaction rate (in terms of decrease in acid value) was increased as the reaction temperature was increased regardless of the presence of the catalyst and reaction time (42.7, 21.5 and 10.0 at $170^{\circ}C,\;210^{\circ}C\;and\;250^{\circ}C$, respectively) and as the reaction time was increased regardless of the temperature and the presence of the catalyst (31.1 vs 18.3 for 3 hrs vs 6 hrs). The presence of the catalyst (0.2% tin chloride) also accelerated the rate regardless of the reaction temperature and time (36.9 vs 12.5). Analysis by column chromatography showed that content of triglyceride in the oil was increased to 72.9% and 61.1% from 10.4% and content of free fatty acids in the oil was decreased to 1.4% and 6.1% from 60.2%, when the degummed oil was esterified at $250^{\circ}C$ for 6 hrs in the presence of and in the absence of the catalyst, respectively. The results estimated from the iodine values indicate that polymer formation was not significant, when the oil was esterified for 6 hrs at temperatures up to $210^{\circ}C$. However, it was somewhat significant for the oil esterified at $250^{\circ}C$ for 6 hrs. The catalyst did not affect the polymer formation. Analysis by high performance liquid chromatography showed that oleic acid (42.5%), linoleic acid (29.0%) and palmitic acid (20.3%) were the major fatty acid components of the rice bran oil.

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Characterization and Purification of the Bacteriocin Produced by Bacillus licheniformis Isolated from Soybean Sauce (간장에서 분리한 Bacillus licheniformis가 생산하는 박테리오신의 특성 및 정제)

  • Jung, Sung-Sub;Choi, Jung-I;Joo, Woo-Hong;Suh, Hyun-Hyo;Na, Ae-Sil;Cho, Yong-Kweon;Moon, Ja-Young;Ha, Kwon-Chul;Paik, Do-Hyeon;Kang, Dae-Ook
    • Journal of Life Science
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    • v.19 no.7
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    • pp.994-1002
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    • 2009
  • A bacteriocin-producing bacterium identified as Bacillus licheniformis was isolated from soybean sauce. Antibacterial activity was confirmed by paper disc diffusion method, using Micrococcus luteus as a test organism. The bacteriocin also showed antibacterial activities against Bacillus sphaericus, Lactobacillus bulgaricus, Lactobacillus planiarum, Paenibacillus polymyxa, and Pediococcus dextrinicus. Optimal culture conditions for the production of bacteriocin was attained by growing the cells in an MRS medium at a pH of 6.5~ 7.0 and a temperature of 37$^\circ$C for 36$\sim$48 hr. Solvents such as chloroform, ethanol, acetone, and acetonitrile had little effect on bacteriocin activity. However, about 50% of bacteriocin activity diminished with treatment of methanol and isopropanol at the final concentration of 50% at 25$^\circ$C for 1 hr. It was stable against a pH variation range from 3.0 and 7.0, but the activity reduced to 50% at a pH range from 9.0 to 11.0. It's activity was not affected by heat treatment at 100$^\circ$C for 30 min and 50% of activity was retained after heat treatment at 100$^\circ$C for 60 min, showing high thermostability. The bacteriocin was purified to a homogeneity through ammonium sulfate precipitation, SP-Sepharose ion-exchange chromatography, and reverse-phase high-performance liquid chromatography (HPLC). The entire purification protocol led to a 75-fold increase in specific activity and a 13.5% yield of bacteriocin activity. The molecular weight of purified bacteriocin was estimated to be about 2.5 kDa by tricine-SDS-PAGE.

Classification and identification of organic aerosols in the atmosphere over Seoul using two dimensional gas chromatography-time of flight mass spectrometry (GC×GC/TOF-MS) data (GC×GC/TOF-MS를 이용한 서울 대기 중 유기 에어로졸의 분류 및 동정)

  • Jeon, So Hyeon;Lim, Hyung Bae;Choi, Na Rae;Lee, Ji Yi;Ahn, Yun Kyong;Kim, Yong Pyo
    • Particle and aerosol research
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    • v.14 no.4
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    • pp.153-169
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    • 2018
  • To identify a variety of organic compounds in the ambient aerosols, the two-dimensional gas chromatography-time of flight mass spectrometry (GCxGC) system (2DGC) has been applied. While 2DGC provides more peaks, the amount of the generated data becomes huge. A two-step approach has been proposed to efficiently interpret the organic aerosol analysis data. The two-dimensional 2DGC data were divided into 6 chemical groups depending on their volatility and polarity. Using these classification standards, all the peaks were subject to both qualitative and quantitative analyses and then classified into 8 classes. The aerosol samples collected in Seoul in summer 2013 and winter 2014 were used as the test case. It was found that some chemical classes such as furanone showed seasonal variation in the high polarity-volatile organic compounds (HP-VOC) group. Also, for some chemical classes, qualitative and quantitative analyses showed different trends. Limitations of the proposed method are discussed.

A Study on Replay Experiments and Thermal Analysis for Autoignition Phenomenon of Shredded Waste Tires (폐타이어 분쇄물의 자연발화현상에 대한 재연실험 및 열분석에 관한 연구)

  • Koh, Jae Sun;Jang, Man Joon
    • Fire Science and Engineering
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    • v.26 no.6
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    • pp.99-108
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    • 2012
  • These days, spontaneous ignition phenomena by oxidizing heat frequently occur in the circumstances of processing and storing waste tires. Therefore, to examine the phenomena, in this work, this researcher conducted the tests of fires of fragmented waste tires (shredded tire), closely investigated components of the fire residual materials collected in the processing and storing place, and analyzed the temperature of the starting of the ignition, weight loss, and heat of reaction. For the study, this researcher conducted fire tests with fragmented waste tires in the range of 2.5 mm to 15 mm, whose heat could be easily accumulated, and performed heat analysis through DSC and TGA, DTA, DTG, and GC/MS to give scientific probability to the possibility of spontaneous ignition. According to the tests, at the 48-hour storage, rapid increase in temperature ($178^{\circ}C$), Graphite phenomenon, smoking were observed. And the result from the DTA and DTG analysis showed that at $166.15^{\circ}C$, the minimum weight loss occurred. And, the result from the test on the waste tire analysis material 1 (Unburnt) through DSC and TGA analysis revealed that at $180^{\circ}C$ or so, thermal decomposition started. As a result, the starting temperature of ignition was considered to be $160^{\circ}C$ to $180^{\circ}C$. And, at $305^{\circ}C$, 10 % of the initial weight of the material reduced, and at $416.12^{\circ}C$, 50 % of the intial weight of the material decreased. The result from the test on oxidation and self-reaction through GC/MS and DSC analysis presented that oxidized components like 1,3 cyclopentnadiene were detected a lot. But according to the result from the heat analysis test on standard materials and fragmented waste tires, their heat value was lower than the basis value so that self-reaction was not found. Therefore, to prevent spontaneous ignition by oxidizing heat of waste tires, it is necessary to convert the conventional process into Cryogenic Process that has no or few heat accumulation at the time of fragmentation. And the current storing method in which broken and fragmented materials are stored into large burlap bags (500 kg) should be changed to the method in which they are stored into small burlap bags in order to prevent heat accumulation.

Inhibitory Effect of Hot-Water Extract of Paeonia japonica on Oxidative Stress and Identification of Its Active Components (백작약 열수추출물의 산화적 스트레스 억제효과 및 유효성분 동정)

  • Jeong, Ill-Yun;Lee, Joo-Sang;Oh, Heon;Jung, U-Hee;Park, Hae-Ran;Jo, Sung-Kee
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.5
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    • pp.739-744
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    • 2003
  • This study was carried out to investigate the antioxidative activity and to identify the active components of hot-water extract of Paeoniajaponica (PJ), which was a main ingredient of a herb mixture preparation recently established as a potent candidate of radioprotector in our laboratory. The water extract was fractionated with CHCl$_3$, EtOAc and n-BuOH. The extract and its fractions showed very low activity in hydroxyl radical scavenging test. In lipid peroxidation test, the extract, EtOAc and water fractions showed moderate inhibition with the ratio above 50%. In DPPH radical scavenging test, the extract, EtOAc and water fraction showed high activity with the ratio above 80%, especially. EtOAc fraction scavenged the radicals as much as synthetic antioxidant (BHA), even at low concentration. It is suggested that mai or partition for antioxidative activity of Paeonia japonica was EtOAc fraction. Subsequently, two active compounds (PJE021-1 and JE024-1) from EtOAc fraction were isolated by using MCI gel and silica gel column chromatography The two compounds inhibited remarkedly the $H_2O$$_2$-induced DNA damage in human peripheral blood lymphocytes, measured by single-cell gel electrophoresis (SCGE). PJE021-1 protected the cells to almost negative control level, dose-dependently. PJE024-1 exhibited a potent inhibition with the ratio of 71% at even low concentration (0.5 $\mu\textrm{g}$/$m\ell$). Finally, their chemical structures were identified as gallic acid (PJE021-1) and (+)-catechin (PJE024-1), respectively, on the basis of the speculation of spectral and physical data.

Neuroprotective Effects of Modified Yuldahanso-tang (MYH) in a Parkinson's Disease Mouse Model (MPTP로 유도된 Parkinson's disease 동물 모델에서 열다한소탕 가감방 (MYH)의 신경 세포 보호 효과)

  • Go, Ga-Yeon;Kim, Yoon-Ha;Ahn, Taek-Won
    • Journal of Sasang Constitutional Medicine
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    • v.27 no.2
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    • pp.270-287
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    • 2015
  • Objectives To evaluate the neuroprotective effects of modified Yuldahanso-tang (MYH) in a Parkinson's disease mouse model. Methods 1) Four groups (each of 8 rats per group) were used in this study. 2) The neuroprotective effect of MYH was examined in a Parkinson's disease mouse model. C57BL/6 mice treated with 1-methyl-4-phenyl-1,2,3,6-tetrahydropyridine (MPTP, 30 mg/kg/day), intraperitoneal (i.p.) for 5 days. 3) The brains of 2 mice per group were removed and frozen at $-20^{\circ}C$, and the striatum-substantia nigra part was seperated. The protein volume was measured by Bradford method following Bio-Rad protein analyzing kit. Using mouse/Rat Dopamine ELISA Assay Kit. 4) The brains of 2 mice per group were separated and removed. TH-immunohistochemical was examined in the MPTP-induced Parkinson's disease mice to evaluate the neuroprotective effects of MYH on ST and SNpc. 5) Two mice out of each group were anesthetized and skulls were opened from occipital to frontal direction to take out the brains. The brains added TTC solution for 20 minutes for staining. 6) The water tank used for morris water maze test was filled with $28^{\circ}C$ water, and a round platform of 10cm in diameter was installed for mice to step on. The study was carried out once a day within 30 seconds, keep exercising to step on the platform in the pool. 7) The brains of two mice out of each group were fixed in 10% formaldehyde solution and paraphillin substance was infiltrated. They were fragmented by microtome, and observed under an optical microscope after Hematoxylin & Eosin staining. 8) A round acrylic cylinder with its upper side open was filled with clean water and depressive mouse models were forced to swim for 15 minutes. After 24 hours the animals were put in the same equipment for 5 minutes and were forced to swim. 9) The convenient, simple, and accurate high-performance liquid chromatography (HPLC) method was established for simultaneous determination of Neurotransmitters in MPTP-MYH group. Results 1) MYH possess Dopamine cell protective effect on MPTP-induced injury in striatum and substantia nigra pars compacta. 2) MYH inhibits the loss of tyrosine hydroxylase-immunoreacitive (TH-IR) cells in the striatum and substantia nigra pars compacta on MPTP-induced injury in C57BL/6 mice. 3) MYH possesses improvement effect on MPTP-induced memory deterioration in C57BL/6 mice through the reduction of prolongated Sort of lost time by MPTP injection using the Morris water maze test. 4) MYH possesses hippocampal neuron protective effect on MPTP-induced injury in C57BL/6 mice. 5) MYH possesses improvement effect on MPTP-induced motor behaviour deficits and depression in C57BL/6 mice through the reduction of prolongated losing motion by MPTP injection using the Forced swimming test. 6) MYH increases serotonin product amount on MPTP-induced injury in C57BL/6 mice. Conclusions This experiment suggests that the neuroprotective effect of MYH is mediated by the increase in Dopamin, TH-ir cell, Hippocampus and Serotonin. Furthermore, MYH essential oil may serve as a potential preventive or therapeutic agent regarding Parkinson's disease.

Quantitatation of Benzoic and Sorbic Acids in Some Processed Foods of Korea (일부 한국 가공식품의 벤조산과 소르빈산의 함량 조사)

  • Mitra, Sanika;Han, Jang-Il;Lee, Ki-Teak;Kim, Seong-Ai
    • Food Science and Preservation
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    • v.16 no.6
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    • pp.789-796
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    • 2009
  • Benzoic acid (BA) and sorbic acid (SA) are the preservatives most commonly used in food. Although BA and SA are generally safe, some previous studies have shown that consumption of excessive amounts of these food additives can be a health hazard. The aim of this study was to determine the amounts of BA and SA in processed foods in Korea. Different brands of fruit juice, yogurt, cheese, dried fruits, jam, and margarine were purchased at a local market in Daejeon, Korea. Samples were analyzed by high-performance liquid chromatography (HPLC) using a UV detector. Chromatographic separation was achieved with a C18 column. Methanol acetate buffer (pH 4.4) at a 35:65 v/v ratio was used as the initial mobile phase to elute BA and SA. The detector wavelength was set at 254 nm. The average test results observed for BA concentrations in fruit juice, yogurt, cheese, dried fruits, jam, and margarine were $40.26{\pm}0.02$, $2.07{\pm}0.06$, $0.02{\pm}0.09$, $0.36{\pm}08$, $265.30{\pm}0.02$, and $27.34{\pm}0.08\;mg/kg$, respectively. Average concentrations of SA in these samples were $0.92{\pm}0.06$, $1.06{\pm}0.07$, $7.30{\pm}0.01$, $14.14{\pm}0.08$, $25.65{\pm}0.06$, and $4.81{\pm}0.07\;mg/kg$, respectively. Thus, the average levels of BA and SA in the studied food items were lower than the KFDA-permitted limits. Moreover, the estimated daily intake of both BA and SA by a typical consumer were below the maximum recommended daily values.

Simultaneous Determination of Cholesterol, Bile Acids and Sterols in Human Bile Juices and Gallstones Using GC/MS (GC/MS에 의한 담석과 담즙내의 Cholesterol, Bile Acids 및 Sterols의 동시 Profiling)

  • Yang, Yoon Jung;Lee, Seon Hwa;Kim, Hyun Joo;Chung, Bong Chul
    • Journal of the Korean Chemical Society
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    • v.42 no.3
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    • pp.266-276
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    • 1998
  • Cholesterol supersaturation in bile, which causes gallstone formation, is the result of low bile acid secretion or high cholesterol secretion. The quantitative analysis of cholesterol, bile acids and sterols which are precursors of cholesterol have been used to examine the changes in bile component. We described a simple, sensitive and reproducible method for simultaneous determination of cholesterol, five bile acids and seven sterols in human bile juices and gallstones by capillary column gas chromatography-mass spectrometry (GC/MS). Clinical samples were hydrolyzed by alcoholic KOH, extracted twice (pH 14 and 1) and derivatized to trimethylsilyl (TMS) ether with $MSTFA/NH_4I$ (N-methyl-N-trimethylsilyltrifluoroacetamide/ammonium iodide) mixture in order to be detected on the GC/MS. The good quality control data were obtained through within-a-day and day-to-day test (RSD values were 1.72-13.79, 0.68-14.10, respectively) and the recovery range of them was 73.56-96. 95 Using this method, biliary and gallstone compositions in the patients with intrahepatic stones were analyzed. The amounts and its relative distribution of cholesterol, bile acids and sterols showed different pattern in bile juices and gallstones.

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A Diagnostic Algorithm after Newborn Screening for 21-hydroxylase Deficiency (선천성 부신 과형성증(21-hydroxylase 결핍)의 신생아 선별 검사 후 진단 알고리즘)

  • Cho, Sung Yoon;Ko, Jung Min;Lee, Kyung-A
    • Journal of The Korean Society of Inherited Metabolic disease
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    • v.16 no.2
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    • pp.70-78
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    • 2016
  • 21-hydroxylase deficiency (21-OHD), most common form of congenial adrenal hyperplasia, is categorized into classical forms, including the salt-wasting (SW) and the simple virilizing (SV) types, and nonclassical (NC) forms based on the severity of the disease. Newborn screening for 21-OHD has been performed in Korea since 2006. $17{\alpha}$-hydroxyprogesterone (17-OHP) is a marker for 21-OHD and is measured using a radioimmunoassay or a fluoroimmunoassay. Premature and low birth weight infants are likely to give false positive 17-OHP findings, therefore, cutoff values for these infants should be determined based on gestational weeks or birth weight. ACTH simulation test is helpful when the 17-OHP shows equivocal increase, and it is gold standard for diagnosis of NC type. Recently, liquid chromatography linked with tandem mass spectrometry was developed for rapid, highly specific, and sensitive analysis of multiple analytes. Molecular analysis of CYP21A2 is useful for confirming diagnosis of mild SV or NC type, predicting prognoses, and genetic counseling. In order to make newborn screening for 21-OHD more efficient, early detection of boy with SW type, early determination of girl with ambiguous genitalia, detection of NC type, and overcoming of false positive in premature and low birth weight infants should be considered. Above all, early treatment should be started when the patient is suspected as having 21- OHD clinically before confirming the diagnosis to prevent adrenal crisis. Here, author reviewed recent articles of guideline and proposed guideline for 21-OHD.

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