• Title/Summary/Keyword: 체화방법

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Analysis of anatoxin-a in aqueous and cyanobacterial samples from korean lakes by liquid chromatography with fluorescence detection (액체크로마토그래피-형광검출법에 의한 호소시료의 아나톡신-a 분석)

  • Lee, In-Jung;Lee, Chul-Gu;Heo, Seong-Nam;Lee, Jae-Gwan
    • Analytical Science and Technology
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    • v.24 no.3
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    • pp.225-230
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    • 2011
  • Anatoxin-a is a cyanobacterial neurotoxin with a high toxicity produced by Anabaena, Aphanizomenon and Oscillatoria. Water bloom, formed by Anabaena has been occurring frequently in Lake Yeongchun. It is need to develop a sensitive method for determination of anatoxin-a to control potential hazard in raw water resources. In this study, we developed a highly sensitive analytical method of anatoxin-a using solid phase extraction (SPE) and high performance liquid chromatography (HPLC) with fluorescence detection. Anatoxin-a was converted into a highly fluorescent derivative using 4-fuoro-7-nitro-2,1,3-benzoxadiazole (NBF-F). The method was evaluated in terms of linearity of calibration curve, recovery and repeatability, and the adequate values were obtained. The method detection limit was $0.034\;{\mu}g/g$ and $0.022\;{\mu}g/L$ for algal and water samples, respectively. The concentrations of anatoxin-a were measured in algal and water samples from Lake Andong, Yeongchun and Daechung and ranged from $0.135\;{\mu}g/g$ to $10.979\;{\mu}g/g$ in algal samples and not detected in water samples.

Quantification of urea in serum by isotope dilution HPLC/MS (동위원소 희석 HPLC/MS에 의한 혈청 내 urea의 정량)

  • Lee, Hwashim;Park, Sangryoul
    • Analytical Science and Technology
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    • v.18 no.4
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    • pp.271-277
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    • 2005
  • Urea in blood has been measured as an effective marker for diagnosis of renal function. Urea which is e end-product of nitrogen containing metabolites such as proteins is filtered through glomeruli of kidneys and then excreted as urine. If the renal function is deteriorated, the urea concentration in blood will be increased, from which the healthiness of renal function is judged. In order to improve the confidence of diagnosis results, the results must keep traceability chain to certified reference materials, which was certified by primary reference method. In this study, we proposed isotope dilution-liquid chromatography/mass spectrometry (ID-LC/MS) as a candidate primary method, in which $15^N_2$-urea is used as an internal reference material. The developed method is highly accurate in principle and is convenient as it does not require cumbersome derivatization. 0.1 mmol/L ammonium chloride was selected as a mobile phase for HPLC because it provided low interference in MS analysis of relatively low molecular weighted urea. HPLC and MS were connected with an electrospray ionization (ESI) interface of positive mode, which provided high sensitivity and reproducibility. The developed method was validated with internationally recognized reference materials, and we have obtained satisfactory results in an international ring trial. The expanded uncertainty calculated according to ISO guide was 1.8% at 95% confidence interval. The developed method is being used as a primary reference measurement method such as for certification of serum certified reference materials (CRMs).

Determination of Amitrole in Water Samples by Evaporation and GC/MS (증발법과 GC/MS를 이용한 수질 시료 중의 Amitrole의 분석법 연구)

  • Yoon, So Hee;Hong, Ji Eun;Pyo, Hee Soo;Park, Song Ja
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.483-487
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    • 2003
  • Amitrole is well-known as a non-selective herbicide and it is able to cause contamination of driking water as well as pollution of ground water and surface water. However, it is difficult to extract from water because it has a high solubility for water whereas a low solubility for general organic solvents. This method is described for the determination of amitrole in water samples by GC/MS. After evaporation of 10 mL water sample by a vacuum evaporator, amitrole was derivatized with isobutyl chloroformate (iso-BCF) on room temperature for 15~20 min. As a result, the sensitivity for GCfMS was improved as N-isobutoxycarbonyl amitrole derivative was formed. The linearity of the calibration curve showed good as 0.997. The recoveries were obtained more than 94.9% and relative standard deviations were less than 2.8% at $1.0{\mu}g/L$, $10.0{\mu}g/L$ and $100.0{\mu}g/L$. The limit of detection showed $0.1{\mu}g/L$ with a signal-to-noise ratio (S/N) of 3.

Uncertainty evaluation of the analysis of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol in hair by GC-NCI-MS/MS (GC-NCI-MS/MS를 이용한 모발 중 대마 대사체 분석의 측정불확도 평가)

  • Kim, Jin-Young;Lee, Jae-Il;Cheong, Jae-Chul;Suh, Yong-Jun;In, Moon-Kyo
    • Analytical Science and Technology
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    • v.24 no.1
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    • pp.1-9
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    • 2011
  • We described an estimation of measurement uncertainty in quantitative analysis of 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THC-COOH), the metabolite of ${\Delta}^9$-tetrahydrocannabinol, in hair samples by using the bead-assisted liquid-liquid extraction and gas chromatography-tandem mass spectrometric (GC-NCI-MS/MS) detection. Traceability of measurement was established through the use of reference materials, calibrated volumetric tubes, volume measuring devices, and measuring instruments. The analytical results were compared and the different contributions to the uncertainty were evaluated. Inter-day variation was performed by using statistical analysis of several indicative factors. Measurement uncertainty associated with the analyte in real forensic hair samples were estimated using QC data. The major factor of contribution to combined standard uncertainty was inter-day repeatability, while those associated with preparation of analytical standard and also sample of weight were insignificant considering the degree of contribution. Relative uncertainty of relative extended standard uncertainty divided into the measured concentration of the analyte was 17% in a hair sample. The uncertainty of result evaluation will be invaluable to improve quality of the analysis.

Simultaneous quantitative determination of urinary cholesterol, desmosterol and lanosterol in pravastatin treated rats by gas chromatography/mass spectrometry (Gas Chromatography/Mass Spectrometry를 이용한 Pravastatin 투여 쥐의 뇨 중 Cholesterol, Desmosterol, Lanosterol의 동시분석법)

  • Kumar, Bhowmik Salil;Chung, Bong Chul;Lee, Young-Joo;Yi, Hong Jae;Jung, Byung Hwa
    • Analytical Science and Technology
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    • v.22 no.5
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    • pp.407-414
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    • 2009
  • A simultaneous determination method for cholesterol, lanosterol and desmosterol was developed using gas chromatography/mass spectrometry. Urine was enzymatically hydrolyzed with ${\beta}$-glucuronidase/arylsulfatase. Samples were prepared using extractions with a mixture of ethyl acetate-hexane (2:3, v/v), followed by derivatization with a mixture of MSTFA/TMSI/TMCS (100:2:5 v/v/v). All analyses were performed using GC/MS in selective ion monitoring mode. Good linearities ($r^2=0.998{\sim}0.999$) in calibration curve and a satisfactory recovery (80.0%~113%) were achieved. Accuracy and precision values within ${\pm}15%$ in the concentration range of 5 to 200 ng/mL were also observed for all compounds. The developed method was applied to pravastatin-treated (70 and 250 mg/kg/day for 7 days, oral) hyperlipidemia rats. Those sterols were significantly lower in drug-treated rats compared to the controls, which justifies the drug efficacy. Therefore, these results indicate that the developed method was successfully applied to examine statin drug efficacy with urine sample.

Determination of the Homocysteine, Cysteine and Methionine in Human Plasma by Gas Chromatography with Electron Capture Detector (기체크로마토그래피-전자포획검출기를 이용한 혈장 중의 Homocysteine, Cysteine 및 Methionine의 동시 분석법)

  • Myung, Seung-Woon;Chang, Yoon-Jung;Yoo, Eun-Ah;Park, Joon-Ho;Min, Hye-Ki;Kim, Myung-Soo
    • Analytical Science and Technology
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    • v.12 no.5
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    • pp.408-414
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    • 1999
  • A selective and sensitive method for the derivatization of total homocysteine (Hcy) and the related compounds in plasma by gas chromatograph (GC)-electron capture detector (ECD) has been developed. To determine total homocysteine, cysteine (Cys), and methionine (Met) in human plasma using GC-ECD, analytes were reduced and converted into their N(O,S)-ethylearbonyl pentafluoropropyl (PFP) ester by derivatization with ethyl chloroformate and pentafluoropropyl alcohol (PFP-OH) in plasma. The best derivatizing agent N(O,S)-ethyl carbonyl PFP ester, was chosen by comparing the sensitivity of derivatized analysis in GC-ECD. The derivatized analytes in plasma were extracted by chloroform, and subsequently back-extracted with hexane and analyzed by GC-ECD. The calibration carves ($R^2$ > 0.990) were linear over the range $5-50{\mu}mol/L$ of Hcy and Met, $40-400{\mu}mol/L$ of Cys spiked in plasma. The detection limit observed by the established method was below $0.5{\mu}mol/L$. This method is highly sensitive and specific in the analysis of Hcy, Cys, and Met. Therefore, we suggest that this method is appropriate in the analysis of trace concentration of Hcy, Cys, and Met in biological fluids.

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Preparation Conditions of Hydrolyzed Vegetable Protein Soy Sauce for the Reduction of 3-Monochloropropane-1,2-Diol (3-MCPD) (3-Monochloropropane-1,2-diol(3-MCPD) 저감화를 위한 아미노산 간장의 제조조건)

  • Chung, Yong-Il;Lee, Ji-Soo;Lee, Hyeon-Gyu
    • Korean Journal of Food Science and Technology
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    • v.41 no.5
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    • pp.522-527
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    • 2009
  • The principal objective of this study was to assess the effects of various manufacturing conditions of soy sauce containing hydrolyzed vegetable protein (HVP) (HVP-soy sauce) on 3-monochloropropane-1,2-diol (3-MCPD) contents. Various HVP soy sauces were prepared under different conditions of alkaline treatment and retention process. Derivatives of heptafluorobutylimidazole (HFBI) 3-MCPD were determined via GC/MS below $0.010{\mu}g/g$, which was sensitive with a good recovery rate. The quantity of 3-MCPD decreased with the pH and temperature of alkaline treatment, and the time and temperature of the retention process increased. Alkaline treatment at pH 10.0-10.5 and a 72 hr retention process were shown to reduce effectively the 3-MCPD contents of HVP-soy sauces. This result indicates that the manufacturing process, particularly alkaline treatment, and retention process would be critical steps in managing 3-MCPD contents in HVP-soy sauce.

Review on the Articles of the Effect of Image Training Program with 3D Virtual Reality and Use for Physical Activity of Older Adults: Based on the Embodied Cognition (3D 가상현실 심상운동 프로그램 효과 및 노인체육 적용가능성에 대한 문헌고찰연구: 체화된 인지접근)

  • Moon, Kyung-Ji;Han, Kyung-Hun
    • Journal of the Korean Applied Science and Technology
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    • v.35 no.3
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    • pp.886-904
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    • 2018
  • The 3D(dimension) vritual reality(VR) has already been used in various sports fields, especially in the training of elite athletes. It is mainly used to maximize the effectiveness of image training, and the use of VR-based image training has received special attention as evidence-based pratices for its feasibility, practicality, and appropriateness. However, in recent years, the use of VR is no longer used only for the training of elite athletes, but is widely used in social sports. This is because, the advantage of exercise in VR is that it is highly stable and has fewer restrictions from the external environment. Considering these advantages, it can be used for the elderly physical activity. This study identifies and reviews studies applying VR-based image training. Several recommendations for the future study on VR-based image training for the older such as interdisciplinary approach to VR-based image training, support needs regarding characteristics of the older, and generalization and maintenance of acquired technology were discussed.

Observation Training Research of Stanislavski School for Creating the Role (역할 창조를 위한 스타니슬랍스키 학파의 관찰훈련 연구)

  • Ha, Byoung-Hun
    • The Journal of the Korea Contents Association
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    • v.17 no.1
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    • pp.585-593
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    • 2017
  • This study is about an observation, namely, the starting point of a role creation with playing a bridge role regarding the work of the role at the work with oneself in the actor training program of the stanislavsky school called the bible about the reenactment acting which is the most basic study of the performance, and in the circumstance of theatrical circles of Korea, which relatively have a lack of the research as mentioned earlier, it described the necessity, usefulness and types of the observation as well as methods of a stepwise observation. First of all, actors should capture observing targets suitable for a role in the play, and if the targets were captured, he needs to imitate and then learn it by using his own body In addition, it must go through the process of an extended application by an adjustment, an amplification, and the application depending on the circumstances of the role after understanding the principle of physical behavior. Also, in order to overcome the simple duplication of outward appearance, making it his own should be conducted through the process of learning it by body and identification by attempting empathy, and for become not the process of the observations which can be partially and fragmentarily finished but the whole acts handling the whole play, it requires the actors to continuously make efforts to create the role, designed to be appropriate for the role while comprehensively arranging each behavior of fragmented figures.

Determination of p-Anisic Acid and Methylparaben by Using High Performance Liquid Chromatography (HPLC를 이용한 p-아니식애씨드와 메칠파라벤의 분리 분석법 개발)

  • Kim, Il Hyun;Ryu, De Hun;Kim, Young Soo;Jung, Eun Sun;Park, Deok Hoon
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.40 no.4
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    • pp.359-364
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    • 2014
  • In this study, we developed a HPLC method for the separation and analysis of methylparaben and p-anisic acid, which are commonly used as a synthetic preservative and natural preservative, respectively. Methylparaben and p-anisic acid have same molecular weight (152.15 g/mol), similar structure and same maximum absorption wavelength (250 nm), thus they showed same retention time (RT) value (13.3 min) in HPLC experiment. We observed that two substances are separated on C18 column after methylparaben was derivatized selectively through the acetylation reaction. Instead, RT of the acetylated methylparaben was moved to 23.9 min from 13.3 min. The average retention time was $23.9{\pm}0.1min$ and peak area values was $5042882{\pm}4778$. In addition it showed a high linearity in the calibration curve with a correlation coefficient (R2) of 0.9999658. Detection and quantitation limits were $1.47{\mu}g/mL$ and $4.44{\mu}g/mL$, respectively. In conclusion, the developed method can be useful for separation and analysis of preservatives with similar structure in cosmetic fields.