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Studies on Solvent Extraction and Analytical Application of Metal-dithizone Complexes(I). Separation and Determination of Trace Heavy Metals in Urine (Dithizone 금속착물의 용매추출 및 분석적 응용(제1보). 뇨중 흔적량 중금속 원소의 분리 정량)

  • Jeon, Moon-Kyo;Choi, Jong-Moon;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.9 no.4
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    • pp.336-344
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    • 1996
  • The extraction of trace cobalt, copper, nickel, cadmium, lead and zinc in urine samples of organic and alkali metal matrix into chloroform by the complex with a dithizone was studied for graphite furnace AAS determination. Various experimental conditions such as the pretreatment of urine, the pH of sample solution, and dithizone concentration in a solvent were optimized for the effective extraction, and some essential conditions were also studied for the back-extraction and digestion as well. All organic materials in 100 mL urine were destructed by the digestion with conc. $HNO_3$ 30 mL and 30% $H_2O_2$ 50 mL. Here, $H_2O_2$ was added dropwise with each 5.0 mL, serially. Analytes were extracted into 15.0 mL chloroform of 0.1% dithizone from the digested urine at pH 8.0 by shaking for 90 minutes. The pH was adjusted with a commercial buffer solution. Among analytes, cadmium, lead and zinc were back-extracted to 10.00 mL of 0.2 M $HNO_3$ from the solvent for the determination, and after the organic solvent was evaporated, others were dissolved with $HNO_3-H_2O_2$ and diluted to 10.00 mL with a deionized water. Synthetic digested urines were used to obtain optimum conditions and to plot calibration-eurves. Average recoveries of 77 to 109% for each element were obtained in sample solutions in which given amounts of analytes were added, and detection limits were Cd 0.09, Pb 0.59, Zn 0.18, Co 0.24, Cu 1.3 and Ni 1.7 ng/mL, respectively. It was concluded that this method could be applied for the determination of heavy elements in urine samples without any interferences of organic materials and major alkaline elements.

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The Study on Geology and Volcanism in Jeju Island (II): Petrochemistry and $^{40}Ar/^{39}Ar$ Absolute Ages of the Volcanic Rocks in Gapado-Marado, Jeju Island (제주도의 지질과 화산활동에 관한 연구 (II): 가파도와 마라도 화산암류의 암석화학 및 $^{40}Ar/^{39}Ar$ 절대연대)

  • Koh, Gi-Won;Park, Jun-Beom
    • Economic and Environmental Geology
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    • v.43 no.1
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    • pp.53-66
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    • 2010
  • We report petrologic characteristics including $^{40}Ar-^{39}Ar$ absolute ages of the subsurface lavas recovered from borehole cores in two islets, Marado and Gapado, off the southwestern coast of Jeju in southernmost Korea and discuss on the volcanism in the region. The lavas in Gapado are apparently divided into one unit with bright colored, aphanitic texture and sheet jointed, and another unit with dark colored and massive. The outcrops often show differentially weathered pattern due to textural difference. While, the lavas in Marado have vesicular and glomerporphyric texture, even though each lava flow unit in Marado has slight unique texture with variation of vesicularity and phenocrysts. The chemical composition of rock core samples from Gapa borehole and Mara borehole shows that the lavas from Gapado and Marado are classified into basaltic trachyandesite($SiO_2$ 52.6-53.6 wt%, $Na_2O+K_2O$ 7.3-7.5 wt%) and tholeiitic andesite($SiO_2$ 51.7-52.8 wt%, $Na_2O+K_2O$ 3.6-4.1 wt%), respectively. The measured $^{40}Ar-^{39}Ar$ plateau ages range from $824{\pm}32\;Ka$(MSL -69 m) to $758{\pm}\;Ka$(MSL 19 m) for core samples of Gapa borehole and $259{\pm}168\;Ka$(MSL -26 m) for a core sample of Mara borehole, respectively. The absolute age of Gapado basaltic trachyandesite is well correlated with that of Sanbangsan trachyte(Won et al., 1986). Meanwhile, the age of a sample in Marado has $259{\pm}168\;Ka$(MSL -26 m) with poor plateau age formation and high error range. We report the data in caution but the rock composition and absolute age of Marado tholeiitic andesite are relatively correlated with those of lava units from Duksu and Sangmo-2 boreholes, indicating the volcanism during 260-150 Ka. On the basis of interpretation of occurrences of exposed and subsurface volcanic rocks of the study area, stratigraphic relationship with adjacent borehole cores and the bathymetry chart of surrounding area, it indicates that the lavas in Gapado were formed around 800 Ka during relatively early stage of volcanic activity in Jeju Island. Meanwhile, Marado may have originated around 260-150 Ka during relatively young stage of volcanism in Jeju Island. It is inferred that the volcanisms have originated in land and these islets were individual ancient volcanoes. The apparent topography has been re-shaped by tidal erosion due to transgression.

Determination and Monitoring of Grayanotoxins in Honey Using LC-MS/MS (LC-MS/MS를 이용한 벌꿀 중 grayanotoxin 분석법 연구 및 실태조사)

  • Lee, Sook-Yeon;Choi, Youn-Ju;Lee, Kang-Bong;Cho, Tae-Yong;Kim, Jin-Sook;Son, Young-Wook;Park, Jae-Seok;Im, Sung-Im;Choi, Hee-Jung;Lee, Dong-Ha
    • Korean Journal of Food Science and Technology
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    • v.40 no.1
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    • pp.8-14
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    • 2008
  • This study was performed to establish analysis methods, and evaluated for grayanotoxin in domestic/foreign honey and wild honey. The molecular weight of grayanotoxins I, II and III, excluding grayanotoxin III that has been commercialized, were analyzed by LC-MS/MS. Then, the molecular structure of grayanotoxins I and II were analyzed by NMR. A total 111 samples (25 Korean honey, 21 Korean wild honey, 13 Korean honeycomb honey, 44 foreign honey, 8 foreign wild honey) were examined to determined whether or not each sample contained grayanotoxins I, II, and III. The honey samples were mixed with methanol and loaded into a tC18 cartridge, the filtrate was diluted with water, and the mixture was then analyzed by ESI triple-quadrupole LC-MS/MS. Grayanotoxins were only found in the foreign wild honey and were not detected in Korean honey, Korean honeycomb honey, or Korean wild honey. Three of the samples contained grayanotoxin I, II, and III, and one sample contained only grayanotoxins I and III. The lowest level for grayanotoxin I was 3.13 ${\pm}$ 0.00 mg/kg, and the highest level was 12.93 ${\pm}$ 0.01 mg/kg. The levels of grayanotoxin II were 0.84 ${\pm}$ 0.01 mg/kg, 0.92 ${\pm}$ 0.00 mg/kg and 1.08 ${\pm}$ 0.01 mg/kg, respectively. The lowest level of grayanotoxin III was 0.25 ${\pm}$ 0.01 mg/kg and the highest level was 3.29 ${\pm}$ 0.74 mg/kg. Through this study, safety management for foreign wild honey has been enabled.

Physicochemical characteristics of lactic acid fermented Seomaeyaksuk (Artemisia argyi H) Sikhye added with different addition ratio of MSG (MSG 첨가 비율을 달리한 섬애약쑥(Artemisia argyi H) 식혜의 유산균 발효에 따른 이화학적 특성)

  • Shin, Jeong Yeon;Shin, Jung Hye;Kang, Min Jung;Choi, Myung Hyo;Park, Hee Rin;Choi, Jine Shang;Bae, Won Yeol;Seo, Won Tak
    • Food Science and Preservation
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    • v.24 no.2
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    • pp.254-265
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    • 2017
  • For the production of ${\gamma}-aminobutyric$ acid (GABA) contents increased Seomaeyaksuk fermentant, 0, 0.25, 0.5 and 1.0% of monosodium galutamate (MSG) was added in Seomaeyaksuk water extract 15% contained Sikhye and inoculated with Lactobacillus brevis (KI271266). Physicochemical properties were sampling and analyzed at each 1 day during 3 days fermentation. Goes on fermentation periods, the turbidity was gradually reduced, but lightness and the yellowness was increased, redness was decreased. Soluble solid was also decreased. The reducing sugars content were also decreased during fermentation. pH was 4.65-4.83 before fermentation but it was lower 3.15-3.68 after three days fermentation. The GABA contents increased by fermentation periods and it was the highest in MSG 1.0% added sample (354.38 mg/L). Fructose, glucose and sucrose contents were 50-67% decreased at three days fermentation than before fermentation. Among the organic acids, propionic acid, oxalic acid, citric acid and fumaric acid contents were decreased and lactic acid, acetic acid and succinic acid were increased during fermentation periods. Contents of total polyphenol and DPPH radical scavenging activity were the highest in MSG 0.5% added sample. From these results, we confirmed that increasing of GABA content when the manufacturing of Seomaeyaksuk lactic acid fermentation product, is possibile by addition of MSG without affecting physicochemical characteristics.

Changes in Physicochemical Composition of Sea Urchin Roe by Steaming Treatment (열처리 조건에 따른 성게 알의 이화학적 성분 변화)

  • Lee, Sung-Uk;Lee, Hye-Young;Kim, Seong-Ho;Kim, Duk-Jin
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.41 no.4
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    • pp.550-560
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    • 2012
  • This study was performed to investigate the physicochemical properties of sea urchin ($Anthocidaris$ $crassispina$, $Pseudocentrotus$ $depressus$, $Hernicentrotus$ $pulcherrimus$) roe as a processed or canned food by steaming treatment. Proximate compositions of $A.$ $crassispina$ roe and $P.$ $depressus$ roe were similar, but water, crude ash, and carbohydrate contents of $H.$ $pulcherrimus$ roe showed little differences. Proximate compositions of sea urchin roe showed slight differences with steaming time, raw samples showed no differences. Glycine content of the three raw sea urchin roe samples showed the highest concentration among free amino acids, followed by arginine, alanine, and lysine, in order. Total free amino acid contents of raw sea urchin roe were 754.70 mg% ($A.$ $crassispina$), 567.75 mg% ($P.$ $depressus$), and 449.44 mg% ($H.$ $pulcherrimus$). Total free amino acid content of 5 min steaming sample was highest among steaming and canning conditions. ATP, ADP, and AMP contents of raw $P.$ $depressus$ roe sample was higher than those of $A.$ $crassispina$and $H.$ $pulcherrimus$ roe. Major fatty acids of the three raw sea urchin roe samples were myristic acid, palmitic acid, and EPA. S.F.A. content of raw samples of $A.$ $crassispina$and $H.$ $pulcherrimus$ roe was higher than U.F.A content, whereas U.F.A. content of $P.$ $depressus$ roe was highest among the three raw samples. For minerals K, P, Fe, and Zn contents were highest in $A.$ $crassispina$roe while Ca, Mg, Na, and Cu contents were highest in $H.$ $pulcherrimus$ roe. For heavy metals, Cd, Pb and As were detected in all samples in trace amounts under the criteria of the Korea food codex.

Effect of extract temperature and duration on antioxidant activity and sensory characteristics of Ulmus pumila bark extract (추출온도 및 시간에 따른 유백피 추출물의 항산화 활성과 음료의 관능적 특성)

  • Cho, Myoung Lae;Oh, Yu-Na;Ma, Jin-Gyeong;Lee, Su-Jin;Choi, Young-Hee;Son, Dong-Hwa;Jang, Eun Hee;Kim, Jong-Yea
    • Food Science and Preservation
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    • v.23 no.7
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    • pp.995-1003
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    • 2016
  • Ulmus pumila L. bark underwent distilled water extraction under three temperature condition ($4^{\circ}C$, room temperature, or $80^{\circ}C$) and two extraction times (1, or 5 min) in order to develop a functional beverage products. Changes in yield, pH, color, total phenolic (TP) content, tannin content and antioxidant activity of the aqueous extracts were evaluated for each extraction temperature and duration. Extraction conditions did not affect yield or pH value of the extracts; however CIE $b^*$ values were high in extracts prepared under high extraction temperature ($80^{\circ}C$) and long extraction duration (5 min) conditions. Both extraction temperature and duration affected the TP and tannin contents of the extracts; however, all extraction conditions resulted in ${\geq}450\;mg\;GAE/g$ TP content and ${\geq}80\;mg\;CE/g$ tannin content. All extracts exhibited ABTS and DPPH radical scavenging ability similar to that of vitamin C. Nitric oxide inhibition activity was lower in the 5 min duration sample than in the 1 min sample. The $4^{\circ}C$ extraction temperature produced an extract with the highest reducing power and hydrogen peroxide values. Extraction temperature also affected sensory evaluation results with the $80^{\circ}C$ extraction temperature producing significantly higher flavor, bitterness, and color score, than those obtained under $4^{\circ}C$ and room temperature extraction conditions.

Determination of Petroleum Aromatic Hydrocarbons in Seawater Using Headspace Solid-Phase Microextraction Coupled to Gas Chromatography/Mass Spectrometry (HS-SPME-GC/MS를 이용한 해수 내 유류계 방향족탄화수소 분석법)

  • An, Joon Geon;Shim, Won Joon;Ha, Sung Yong;Yim, Un Hyuk
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.17 no.1
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    • pp.27-35
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    • 2014
  • The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.

Enzymatic Method for Measuring ATP Related Compounds in Fish Sauces (효소법에 의한 액젓중의 ATP 관련물질 측정)

  • CHO Young Je;IM Yeong Sun;KIM Sang Moo;CHOI Young Joon
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.32 no.4
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    • pp.385-390
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    • 1999
  • HPLC method usually has been used for the determination of ATP and its related compounds in fish muscle and fish sauce. But, total amount of ATP related compounds in fish sauce is determined less than that of fish muscle. In order to establish the extract analysis method for ATP related compounds in fish sauce, a new enzymatic method was developed and compared with existing HPLC method. Fish sauce was extracted with chilled perchloric acid and neutralized to Ph 7.0 with potassium hydroxide solution, the extract was used as sample analyzed by HPLC as usual. On the other hand, for sample analyzed by enzymatic method, 1 ml extract solution was pipetted into test tube. To the tube, 0.5ml of mixed suspension adenosinedeaminase (4U), nucleosidephosphorylase (0.02U) and xanthineoxidase (0.03U) suspended in 2.0ml of 1/15 M sodium phosphate buffer solution pH 7.6 and 1.5ml deionized water wereadded for the decomposition of IMP, HxR and Hx to uric acid at $37^{\circ}C$ for 40 minutes. Total uric acid was determined by measuring optical density at 290nm. In HPLC method, salt decreased the total amount of ATP related compounds by $13.6\~16.2\%$ at $2.5\%$ concentration, but no effect in enzymatic method. IMP, HxR and Hx were detected at 254nm, while uric acid at only 290nm. The ratio of the total amount of ATP related compounds by HPLC method was about $45\%$ of that by enzymatic method in fish sauce. Form these results, enzymatic method is more accurate and simple than HPLC method for analysis of ATP related compounds in fish sauce.

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Textural and Sensory Properties of Beef Jerky replaced Salt with Soybean Paste, Soy Sauce or Red Pepper Paste (소금(NaCl)을 된장, 간장 또는 고추장으로 대체한 우육포의 조직적 및 관능적 특성)

  • Lim, Hyun-Jung;Jung, Eun-Young;Kim, Gap-Don;Joo, Seon-Tea;Yang, Han-Sul
    • Journal of agriculture & life science
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    • v.46 no.6
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    • pp.97-104
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    • 2012
  • The aim of this study was to investigate the quality properties of beef jerky replaced salt (NaCl) with red pepper paste, soy sauce and soybean paste. The quality properties of beef jerky including water activity ($a_w$), pH, moisture content, protein content, color, shear force, texture profile analysis and sensory evaluations were investigated. The sliced beef samples were marinated at salt (control), soybean paste (T1), soy sauce (T2) and red pepper paste (T3) for 24 h and then dried at $70^{\circ}C$ for 8 h. The $a_w$ and moisture content varied from 0.88 to 0.79 and from 28.87% to 22.98%, respectively. All treatment samples showed higher final $a_w$ and moisture content than the control sample after drying for the 8 h (p<0.05). The protein content of T2 and T3 samples were lower than the control. Also, shear force and hardness value of all treatment samples had lower than the control (p<0.05). However, all treatment samples showed lower saltiness intensity than the control sample. Sensory panelists recorded greater flavor and texture scores to the samples with soy sauce replacement. Therefore, sensory panels found that the T2 samples had better overall acceptability scores than the other beef jerky samples (p<0.05).

Evaluation of microplastic in the inflow of municipal wastewater treatment plant according to pretreatment methods (전처리 방법에 따른 하수처리장 유입수에서의 미세플라스틱 성상분석 평가)

  • Kim, Sungryul;Gil, Kyungik
    • Journal of Wetlands Research
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    • v.24 no.2
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    • pp.83-92
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    • 2022
  • The amount of the plastic waste has been increasing according to global demand for plastic. Microplastics are the most hazardous among all plastic pollutants due to their toxicity and unknown physicochemical properties. This study investigates the optimal methodology that can be applied to sewage samples for detecting microplastics before discussing reducing microplastics in MWTPs. In this study, the effect of different pretreatment methods while detecting microplastic analysis of MWTP influent samples was investigated; the samples were collected from the J sewage treatment plant. There are many pretreatment methods but two of them are widely used: Fenton digestion and hydrogen peroxide oxidation. Although there are many pretreatment methods that can be applied to investigate microplastics, the most widely used methods for sewage treatment plant samples are Fenton digestion and H2O2 oxidation. For each pretreatment method, there were factors that could cause an error in the measurement. To overcome this, in the case of the Fenton digestion pretreatment, it is recommended to proceed with the analysis by filtration instead of the density separation method. In the case of the H2O2 oxidation method, the process of washing with distilled water after the reaction is recommended. As a result of the analysis, the concentration of microplastics was measured to be 2.75ea/L for the sample using the H2O2 oxidation method and 3.2ea/L for the sample using the Fenton oxidation method, and most of them were present in the form of fibers. In addition, it is difficult to guarantee the reliability of measurement results from quantitative analysis performed via microscope with eyes. A calibration curve was created for prove the reliability. A total of three calibration curves were drawn, and as a result of analysis of the calibration curves, all R2 values were more than 0.9. This ensures high reliability for quantitative analysis. The qualitative analysis could determine the series of microplastics flowing into the MWTP, but could not confirm the chemical composition of each microplastic. This study can be used to confirm the chemical composition of microplastics introduced into MWTP in the future research.