• Title/Summary/Keyword: 칼럼실험

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Simultaneous Determination of Aflatoxins and Ochratoxin A in Pork by LC-MS/MS (LC-MS/MS를 이용한 돼지고기 중 총아플라톡신 및 오크라톡신 A 동시분석법 확립)

  • Paek, Ockjin;Park, Songyi;Park, Ki Hun;Kim, Sheen-Hee;Suh, Saejung;Yoon, Hae Jung
    • Journal of Food Hygiene and Safety
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    • v.31 no.3
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    • pp.194-200
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    • 2016
  • Aflatoxins and ochratoxin A (AFTs and OTA) are secondary fungal metabolites produced by several moulds, mainly by Aspergillus flavus by Aspergillus ochraceus and Penicillium verrucosum, and these toxins can be transferred to animals and humans through the ingestion of contaminated feed and food. This study was to develop the analytical method for determination the levels of AFTs ($B_1$, $B_2$, $G_1$ and $G_2$) and OTA in pork. The AFTs and OTA were analyzed simultaneously by electrospray ionization in positive ion mode and mass reaction monitoring (MRM) after solid phase extract (SPE) columns clean-up. Performance characteristics, such as accuracy, precision, linear range, limit of detection (LOD) and quantification (LOQ), were also determined. Matrix-matched standard calibration was used for quantification, obtaining the recoveries in the range of 67.3~108.2% with the relative standard deviations of < 20%. Limits of detection and quantification were also estimated, obtaining the limits of quantification ranged in $0.7{\sim}1.3{\mu}g/kg$. The results of the inter-day study, which was performed with pork samples for 3 days, showed an accuracy of 92.0~109.9%. The precisions (expressed as relative standard deviation values) for the inter day variation were 2.6~17.8%. The method developed in this study was able to carry out the analysis with the satisfactory intensity and accuracy.

Influence of Acid and Heat Treatment on the Removal of Fluoride by Red Mud (Red Mud의 산처리 및 열처리가 불소 제거에 미치는 영향)

  • Kang, Ku;Nyakunga, Expedito;Kim, Young-Kee;Park, Seong-Jik
    • Journal of Korean Society of Environmental Engineers
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    • v.37 no.4
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    • pp.210-217
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    • 2015
  • Fluoride removal by acid and heat treated red mud were studied in batch and column system regarding contact time, initial concentration, pH, adsorbent dose, and filter depth. The results showed that acid treated with 0.8 M HCl, had highest adsorption capacity of fluoride and adsorption capacity decreased as heat treatment temperature increased. Sorption equilibrium reached in 30 min at a initial concentration of 50 mg-F/L but 1 h was required to reach the sorption equilibrium at the initial concentration of 500 mg-F/L by 0.8 M acid treated red mud (0.8 M-ATRM). Equilibrium adsorption data were fitted well to Langmuir isotherm model with maximum fluoride adsorption capacity of 23.162 mg/g. The fluoride adsorption decreased as pH increased due to the fluoride competition for favorable adsorption site with $OH^-$ at higher pH. Removal percentage was increased but the amount of adsorption per unit mass decreased by adding the amount of 0.8 M-ATRM. It was concluded that the 0.8 M-ATRM could be used as a potential adsorbent for the fluoride removal from aqueous solutions because of its high fluoride adsorption capacity and low cost.

Evaluation of Oil Infiltration Behavior in Porous Media Using Dielectric Response (유전율에 의한 지반 매질내 유류침투거동 분석)

  • Kim Man-Il;Jeong Gyo-Cheol
    • The Journal of Engineering Geology
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    • v.15 no.1
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    • pp.29-39
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    • 2005
  • For detecting a ground contamination survey, soil sampling method have been used a drilling or coring technique in general. However these methods are very difficult to systematically real-time monitoring of variation of contamination degree in field. ]'n this research frequency Domain Reflectometry (FDR) system was suggested and carried out to experimental approaches for determination of oil contamination on surface and underground. Experimental method using FDR method was discussed with feasibility of measurement in the laboratory column test. It is determined to degree of oil contamination due to response of dielectric constant re-lated with volumetric water content(θ/sub w/) and volumetric oil content( θ/sub al/ ) of saturated and unsaturated soil media. And physical properties such as effective porosity and oil residual ratio of saturated soil media were also measured through real-time monitoring works using installed FDR measurement sensors, which are defected characteristics of oil movement in the saturated soil media under the soil column tests. In the results of these experiments, a range of effective porosity was estimated to about 0.35 compared with initial porosity 0.40 of manufactured saturated soil media, which is also calculated to about 87.5% to the ratio of initial porosity to effective porosity. Finally oil residual ratio which is compared with volumetric water content and volumetric oil content was calculated about 62.5%.

The Study on the Analysis Method of Tetrodotoxin in Puffer Fish (복어 중 테트로도톡신 분석법에 관한 연구)

  • Kang, Young-Woon;Lee, Yoon-Suk;Park, Sung-Kug;Seo, Jung-Heok;Kim, Mee-Hye
    • Journal of Food Hygiene and Safety
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    • v.27 no.1
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    • pp.37-41
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    • 2012
  • The current standard for testing tetrodotoxin (TTX) in foodstuffs is the mouse bioassay (MBA) in Korea as in many other countries. However, this test suffers from potential ethical concerns over the use of live animals. In addition, the mouse bioassay does not test for a specific toxin thus a sample resulting in mouse incapacitation would need further confirmatory testing to determine the exact source toxin (e.g., TTX, STX, brevotoxin, etc.). Furthermore, though the time of death is proportional to toxicity in this assay, the dynamic range for this proportional relationship is small thus many samples must be diluted and new mice be injected to yield a result that falls within the quantitative dynamic range. Therefore, in recent years, there have been many efforts in this field to develop alternative assays. High performance liquid chromatography (HPLC) coupled with mass spectrometry (MS) has been emerged as one of the most promising options. A LC-MS-MS method involves solid-phase extraction (SPE) and followed by analysis using an electrospray in the positive ionization mode and multiple reactions monitoring (MRM). To adopt LC-MS-MS method as alternative standard for testing TTX, we performed a validation study for the quantification of TTX in puffer fish. This LC-MS-MS method showed good sensitivity as limits of detection (LOD) of $0.03{\sim}0.08{\mu}g/g$ and limits of quantification (LOQ) of $0.10{\sim}0.25{\mu}g/g$. The linearity ($r^2$) of tetrodotoxin were 0.9986~0.9997, the recovery were 80.9~103.0% and the relative standard deviations (RSD) were 4.3~13.0%. The correlation coefficient between the mouse bioassay and LC/MS/MS method was higher than 0.95.

Solid-Phase Refolding Technology in Recombinant Proteins Recovery: Application Examples to Various Biopharmaceutical Proteins (유전자재조합 단백질 회수 공정에서의 고체상 재접힘 기술: 여러 바이오의약 단백질에의 적용 사례)

  • Kim, Min Young;Suh, Chang Woo;Kim, Chang Sung;Jo, Tae Hoon;Park, Sang Joong;Choi, Won Chan;Lee, Eun Kyu
    • Korean Chemical Engineering Research
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    • v.43 no.2
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    • pp.187-201
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    • 2005
  • Bioprocessing technologies utilizing 'biorecognition' between a solid matrix and a protein is being widely experimented as a means to replacing the conventional, solution-based technology. Frequently the matrices are chromatographic resins with specific functional groups exposed outside. Since the reactions of and interactions with the proteins occur as they are attached to the solid matrix, this 'solid-phase' processing has distinct advantages over the solution-phase technology. Solid-phase refolding of inclusion body proteins uses ion exchange resins to adsorb denaturant-dissolved inclusion body. As the denaturant is slowly removed from the micromoiety around the protein, it is refolded into a native, three-dimensional structure. Once the refolding is complete, the folded protein can be eluted by a conventional elution technique such as the salt-gradient. This concept was successfully extended to 'EBA (expanded bed adsorption)-mediated refolding,' in which the denaturant-dissolved inclusion body in whole cell homogenate is adsorbed to a Streamline resin while cell debris and other impurity proteins are removed by the EBA action. The adsorbed protein follows the same refolding steps. This solid-phase refolding process shows the potential to improve the refolding yield, reduce the number of processing steps and the processing volume and time, and thus improve the overall process economics significantly. In this paper, the experimental results of the solid-phase refolding technology applied to several biopharmaceutical proteins of various types are presented.

Recovery of Aglycone of Daidzein and Genistein in Soybeans (콩에 포함된 비배당체 다이드제인과 제니스테인의 회수)

  • Lee, Kwang Jin;Jin, Long Mei;Kim, Young Sik;Row, Kyung Ho
    • Korean Chemical Engineering Research
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    • v.43 no.5
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    • pp.641-645
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    • 2005
  • Using aqueous solution of 60% ethanol, the isoflavones contained in the Soybean (Chungsun, Korea), Tawon (Suwon, Korea), Jackbean (Hongsung, Korea), Soybean (Jilin, China), Black Soybean (Jilin, China), Kidneybean (Jilin, China) and Soybean (California, U.S.A.) were extracted. In this work, the pretreatment step was composed of agitation extraction, filtration, concentration, ultracentrifuge, and membrane filtration. The analysis by $C_{18}$ column was performed, and the mobile phase applied was linearly changed with A/B of 85/15-65/35 vol% for 50 min (A water/acetic acid, 99.9/0.1 vol%, B acetonitrile/acetic acid, 99.9/0.1 vol%). Among the soybeans tested, the total amounts of the four isoflavones (daidzin, genistin, daidzein, and genistein) extracted by the soybeans from Korea, China and U.S.A. were 1.37, 1.60, and 2.25 mg/g, respectively. It was also found that the total amount of aglycone of daidzein and genistein from soybean (American California) was $144{\mu}g/g$, which was the largest for the soybeans experimented.

Structure Determination of the Extractives from the Taxus Cuspidata Fruits (주목열매 추출물 구조분석)

  • Park, Se-Yeong;Choi, In-Gyu;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.41 no.6
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    • pp.566-575
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    • 2013
  • The fruits of Taxus cuspidata were collected, divided into seeds and fruits, and extracted with 95% EtOH. The extracts were evaporated under the reduced vacuum pressure, concentrated, then successively fractionated with a series of n-hexane, dichloromethane, ethyl acetate and water on a separatory funnel to get some freeze dried samples. A portion of the EtOAc (arils:1.65 g, seeds:1.04 g) and $H_2O$ (arils:7 g, seeds:10 g) soluble samples were chromatographed on a Sephadex column using MeOH-$H_2O$ (1:1, 1:3, 1:5, v/v), EtOH-hexane (3:1, v/v) mixture and 100% $H_2O$ as eluting solvents to isolate pure compounds from the fractions. The isolates were developed by cellulose TLC using t-BuOH-HOAc-$H_2O$ (TBA; 3:1:1, v/v/v) and 6% aqueous HOAc. Visualization was done under ultraviolet light and by spraying the vanillin-HCl-EtOH reagent (4.8:12:480, v/v/v). followed by heating. The structures of the isolates were characterized by $^1H$- and $^{13}C$-NMR, DEPT, 2D-NMR, LC/MS and EI-MS spectra. In addition to the NMR and MS spectra, acid hydrolysis and permethylation were used to determine the correct structure of the isolated sugar compound. Their structures were elucidated as (+)-catechin (1), (-)-epicatechin (2), (+)-gallocatechin (3), (-)-epigallocatechin (4) and ${\beta}$-D-fructofuranose-($2{\rightarrow}4$)-O-${\beta}$-D-glucopyranose($1{\rightarrow}4$)-O-${\alpha}$-D-glucopyranose ($1{\rightarrow}2$)-O-${\beta}$-D-fructofuranose (5) on the basis of the above experimental evidences.

A Study on the Condition Analysis and Improvement of Domestic Medical 99Mo/99mTc Generators Self-disposal (국내 의료용 99Mo/99mTc Generator 자체 처분 지침 현황 분석 및 개선 방향에 대한 연구)

  • Ryu, Chan-Ju;Hong, Seong-Jong
    • Journal of the Korean Society of Radiology
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    • v.13 no.2
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    • pp.297-303
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    • 2019
  • The nuclear medicine department of a domestic medical institution uses $^{99m}TcI$, a radionuclide, from $^{99}Mo/^{99m}TcI$ Generator, to inject radioactive drugs into patients. Among the expired generators, imported from foreign countries, the medical institution implements its own disposal. Each medical institution shall satisfy the permitted in-house disposal concentration of radioactive wastes. The guidelines for self-disposal presented in Korea suggested that self-disposal can be performed 80 days after the generator is used. The purpose of these guidelines is to analyze them by comparing them with the data measured directly with the generator and to study if they are feasible. As a result, the generator with a capacity of 1,000 mCi has the longest half-life, and when tested with a high-radiation Mo(molybdenum) column, the number of days that are below the permitted concentration of body disposal with radioactive waste was 72 days and 71 days that were derived from direct column measurement. The results of the direct study confirmed that the guidelines for in-house disposal in Korea were reasonable, as there were 8 to 9 days of storage compared to the number of in-house disposal days provided in the guidelines.

Cryptoporus volvatus (Peck) Shear: Mycelial characteristics under different culture conditions (한입버섯 균사체 특성과 배양 적정 조건)

  • Kyung-Hwa, Shin;Tae-Min, Park;Kyung-Gu, Min;Soon-Ja, Seok;Myung-Jun, Jang
    • Journal of Mushroom
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    • v.20 no.4
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    • pp.263-269
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    • 2022
  • This study investigated the culture characteristics of Cryptoporus volvatus, whichis grow naturally in Korea, to determine the suitable environmental conditions for its cultivation. The physiological characteristics of the mycelia were assessed according to the cultivation conditions, to determine the optimal conditions for artificial cultivation. The visual characteristics of the hyphae of Cryptoporus volvatus KACC52303 included an irregular and uneven surface and a fuzzy or cotton-like texture. Under the microscope, its microstructure showed pre-chlamydospore formation, but no clamps were seen. The appropriate culture temperature was found to be a medium/high temperature of approximately 25-30℃, and the optimal pH was found to have a wide range from weakly acidic (pH 4) to neutral (pH 7). In the optimal nutrient source experiment, hyphal growth was shown to be fair in a mixed medium with 2.5% dextrin as the carbon source and 0.1% yeast extract as the organic nitrogen source. Among the various amino acids, organic acids, and inorganic salts tested, the fastest hyphal growth was observed in the presence of leucine, acetic acid or gluconic acid, and KCl or KH2PO4, respectively. The column test showed that the best mycelial growth occurred in a mixed medium of 80% pine sawdust, 10% rice bran, and 10% corncob sawdust.

Metabolites profiling and hypolipidemic/hypocholesterolemic effects of persimmon (Diosyros kaki Thumb.) by different processing procedures: in vitro and in vivo studies (제조방법에 따른 떫은감 (Diosyros kaki Thumb.)의 대사체 프로파일링과 중성지질/콜레스테롤 대사 관련 유전자발현 연구 : in vitro 및 in vivo 연구)

  • Park, Soo-Yeon;Oh, Eun-Kyung;Lim, Yeni;Shin, Ji-Yoon;Jung, Hee-Ah;Park, Song-Yi;Lee, Jin Hee;Choe, Jeong-Sook;Kwon, Oran
    • Journal of Nutrition and Health
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    • v.51 no.4
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    • pp.275-286
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    • 2018
  • Purpose: Our previous study demonstrated that persimmon (Diospyros kaki Thumb.) at different stages of ripening provided different protective effects against high-fat/cholesterol diet (HFD)-induced dyslipidemia in rats. In this study, we compared the metabolites profile and gene expressions related to triglyceride (TG)/cholesterol metabolism in vitro and in vivo after treating with persimmon water extracts (PWE) or tannin-enriched persimmon concentrate (TEP). Methods: Primary and secondary metabolites in test materials were determined by GC-TOF/MS, UHPLC-LTQ-ESI-IT-MS/MS, and UPLC-Q-TOF-MS. The expression of genes related to TG and cholesterol metabolism were determined by RT-PCR both in HepG2 cells stimulated by oleic acid/palmitic acid and in liver tissues obtained from Wistar rats fed with HFD and PWE at 0, 150, 300, and 600 mg/d (experiment I) or TEP at 0, 7, 14, and 28 mg/d (experiment II) by oral gavage for 9 weeks. Results: PLS-DA analysis and heatmap analysis demonstrated significantly differential profiling of metabolites of PWE and TEP according to processing of persimmon powder. In vitro, TEP showed similar hypolipidemic effects as PWE, but significantly enhanced hypocholesterolemic effects compared to PWE in sterol regulatory element-binding protein 2 (SREBP2), HMG-CoA reductase (HMGCR), proprotein convertase subtilisin/kexin type 9 (PCSK9), cholesterol $7{\alpha}-hydroxylase$ (CYP7A1), and low density lipoprotein receptor (LDLR) gene expression. Consistently, TEP and PWE showed similar hypolipidemic capacity in vivo, but significantly enhanced hypocholesterolemic capacity in terms of SREBP2, HMGCR, and bile salt export pump (BSEP) gene expression. Conclusion: These results suggest that column extraction after hot water extraction may be a good strategy to enhance tannins and long-chain fatty acid amides, which might cause stimulation of hypocholesterolemic actions through downregulation of cholesterol biosynthesis gene expression and upregulation of LDL receptor gene expression.