• Title/Summary/Keyword: Analytical-synthetic

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Changes of Endogenous Steroids Profile After Oral Administration of Danazol (Danazol의 경구투여에 따른 내인성 스테로이드들의 변화)

  • Choi, Man Ho;Chung, Bong Chul
    • Analytical Science and Technology
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    • v.11 no.5
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    • pp.353-359
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    • 1998
  • Danazol, one of the IOC banned substances, is a synthetic steroid which stimulates the synthesis of cellular protein with multiple and diverse biologic effects. To confirm the androgenic effects of danazol, levels of eight endogenous steroids and its major metabolite in human urine were simultaneously analyzed by selected ion monitoring (SIM) of GC/MS after oral administration. The recovery range of this method was 71.59%~93.56% and the RSD values of precision and accuracy test were 1.87%~10.48% and 1.32%~11.25%, respectively. The limits of detection of most of the drugs were $0.01{\sim}0.05{\mu}g/mL$ and calibration was carried out using urine spiked with each endogenous steroid and ethisterone standard at a concentration of 0.1, 0.5, 1.0, 10, 20 and $50{\mu}g/mL$ and with $10{\mu}g/mL$ of internal standard. Correlation coefficients varied between 0.963 and 0.991. The endogenous steroid profiling is one of valuatle tool for decteation of anabolic steroids.

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Gas Chromatographic Analysis on Residual Concentration and Half-life Time of Cyfluthrin in Potato and Soil (감자와 토양 중에서 Cyfluthrin의 잔류농도와 반감기에 대한 기체 크로마토그래피 분석)

  • Han, Seong Soo;Jeong, Seung Il;Chun, Hyun Ja;Hoang, Geun Chang;Kim, Il Kwang
    • Analytical Science and Technology
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    • v.13 no.6
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    • pp.722-730
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    • 2000
  • The residual concentration and half-life time of synthetic pyrethroid insecticide cyfluthrin in potato and soil were investigated by gas chromatography (GC). The pesticide in potato was extracted with n-hexane, filtered and concentrated. The concentrated phase was transferred to the Sep-Pak silica gel column and purified with acetonitrile and acetone for the analysis by gas chromatography equipped with electron capture detector (GC-ECD). From the standard additional experiments with 0.01 and $0.1{\mu}g$, the recoveries were 85-87% and the detection limit was 0.005 ng. The soil sample was extracted with acetone and dichloromethane. The organic phase was concentrated and redissolved with n-hexane and analyzed with GC-ECD after cleaned with Sep-Pak column. From the standard additional experiments with 0.01 and 0.1 ng, the recoveries were 84-88% and the detection limit was 0.005ng. The half-life time of cyfluthrin in the silty clay was 25 days in the room laboratory and 0.6 days in the fieJd test whereas it was 38 days and 0.5 days for each in case of silty loam.

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Simultaneous Spectrophotometric Determination of Copper, Nickel, and Zinc Using 1-(2-Thiazolylazo)-2-Naphthol in the Presence of Triton X-100 Using Chemometric Methods (화학계량학적 방법을 사용한 Triton X-100이 함유된 1-(2-Thiazolylazo)-2-Naphthol을 사용한 구리, 니켈과 아연의 동시 분광광도법적 정량)

  • Low, Kah Hin;Zain, Sharifuddin Md.;Abas, Mhd. Radzi;Misran, Misni;Mohd, Mustafa Ali
    • Journal of the Korean Chemical Society
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    • v.53 no.6
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    • pp.717-726
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    • 2009
  • Multivariate models were developed for the simultaneous spectrophotometric determination of copper (II), nickel (II) and zinc (II) in water with 1-(2-thiazolylazo)-2-naphthol as chromogenic reagent in the presence of Triton X-100. To overcome the drawback of spectral interferences, principal component regression (PCR) and partial least square (PLS) multivariate calibration approaches were applied. Performances were validated with several test sets, and their results were then compared. In general, no significant difference in analytical performance between PLS and PCR models. The root mean square error of prediction (RMSEP) using three components for $Cu^{2+}$, $Ni^{2+}$ and $Zn^{2+}$ were 0.018, 0.010, 0.011 ppm, respectively. Figures of merit such as sensitivity, analytical sensitivity, limit of detection (LOD) were also estimated. High reliability was achieved when the proposed procedure was applied to simultaneous determination of $Cu^{2+}$, $Ni^{2+}$ and $Zn^{2+}$ in synthetic mixture and tap water.

Solvent Extraction of Trace Amount of Ni(II) in Sea Water by using Salen[N,N'-bis(salicylidene)ethylenediamine] (Salen[N,N'-bis(salicylidene)ethylenediamine]을 이용한 해수 중 극미량 니켈의 용매추출)

  • In, Gyo;Choi, Jong-Moon;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.481-488
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    • 2004
  • Solvent extraction of Ni(II) into a chloroform by using salen[N,N'-Bis (salicylidene)-ethylenediamine] as a ligand has been studied. Salen was synthesized from ethylenediamine and salicylaldehyde by simple condensation reaction in an ethanol. Salen formed a 1 : 1 complex with Ni(II) and its extraction constant was $10^{5.12}$. For the determination of Ni(II) in sea water samples, some experimental conditions such as pH of solution, amount of salen, acid type and concentration for back extraction, extraction time, and influence of foreign ions were optimized by using a synthetic sea water. The sea water of which the composition was similar to a natural sea water was synthesized in this laboratory. Trace Ni(II) was extracted into the chloroform in the weak basic solution above pH 8. And the nickel could be quantitatively extracted with the concentration of salen higher than $1.2{\times}10^{-4}mol/L$. This concentration was more than 180 times of Ni(II) in the solution with a mole ratio. Real samples of Korean coastal sea water were analyzed under optimized conditions. Even though Ni(II) was not detected in these samples. Recoveries more than 98% were obtained in the samples which 40 ng/mL of Ni(II) was spiked. And detection limit of proposed method was 1.3 ng/mL. From these results, it could be known that salen of this type would be applied for the determination of trace metals as an organic chelating reagent.

Seismic Response of Multiple Span Prestressed Concrete Girder Bridges in the New Madrid Seismic Zone (New Madrid 지진대의 다경간 PSC 교량의 지진거동)

  • Choi, Eun-Soo;Kim, Hak-Soo;Kim, Kwang-Il;Cho, Byung-Wan
    • Journal of the Earthquake Engineering Society of Korea
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    • v.10 no.5 s.51
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    • pp.11-23
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    • 2006
  • This paper evaluates the seismic response of multi-span prestressed concrete girder bridges typically found in the New Madrid Seismic Zone region of the central United States. Using detailed nonlinear analytical models and synthetic ground motion records for Memphis, TN, nonlinear response history analyses are performed for two levels of ground motion: 10% probability of exceedance (PE) in 50 years, and 2% probability of exceedance (PE) in 50 years. The results show that the bridge performance is very good fur the 10% PE in 50 years ground motion level. However, the performance for the 2% PE in 50 years ground motion is not so good because it results in highly inelastic behavior of the bridge. Impact between decks results in large ductility demands on the columns, and failure of the bearings that support the girders. It is found that making the superstructure continuous, which is commonly performed for reducing dead load moments and maintenance requirements, results in significant improvement in the seismic response of prestressed concrete girder bridges.

N-oleoyl-D-erythro-sphingosine-based Analysis of Ceramide by High Performance Liquid Chromatography and Its Application to Determination in Diverse Biological Samples

  • Lee, Youn-Sun;Choi, Heon-Kyo;Yoo, Jae-Myung;Choi, Kyong-Mi;Lee, Yong-Moon;Oh, Sei-Kwan;Kim, Tack-Joong;Yun, Yeo-Pyo;Hong, Jin-Tae;Okino, Nozomu;Ito, Makoto;Yoo, Hwan-Soo
    • Molecular & Cellular Toxicology
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    • v.3 no.4
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    • pp.273-281
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    • 2007
  • Ceramide is involved in cell death as a lipid mediator of stress responses. In this study, we developed an improved method of ceramide quantification based on added synthetic ceramide and thin layer chromatography (TLC) separation, and applied to biological samples. Lipids were extracted from samples spiked with N-oleoyl-D-erythro-sphingosine ($C_{17}$ ceramide) as an internal standard. Ceramide was resolved by TLC, complexed with fatty-acidfree bovine serum albumin (BSA), and deacylated by ceramidase (CDase). The released sphingosine was derivatized with o-phthalaldehyde (OPA) and measured by high performance liquid chromatography (HPLC). The limit of detection for ceramide was about 1-2 pmol and the lower limit of quantification was 5 pmol. Ceramide recovery was approximately 86-93%. Ceramide concentrations were determined in biological samples including cultured cells, mouse tissues, and mouse and human plasma. TLC separation of ceramide provides HPLC chromatogram with a clean background without any interfering peaks and the enhanced solubility of ceramide by BSAceramide complex leads to the increased deacylation of ceramide. The use of an internal standard for the determination of ceramide concentration in these samples provides an accurate and reproducible analytical method, and this method can be applicable to diverse biological samples.

Fuzzy Analytic Hierarchy Process for the Evaluation of Old Dwelling Façade Design Factor

  • Park, Jin-A
    • Science of Emotion and Sensibility
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    • v.16 no.3
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    • pp.333-340
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    • 2013
  • The purpose of this paper is to evaluate facade design factors of old dwellings using a Fuzzy Analytical Hierarchy Process (AHP) based on a pairwise comparison analysis using "Façade Design Factors" as evaluation criteria. Traditional old dwellings were presented and evaluated. A Fuzzy AHP based model was used for pairwise comparison of traditional old dwellings, whereby seven criteria and nine alternatives were described through a questionnaire and constructional data. The Fuzzy AHP was used to determine the impact of the facade design factors, because "Traditional" old dwellings are identified by the combination of their facade design factors. Furthermore, the fuzzy AHP is used to verify the feasibility and efficiency of this approach as well as for extent analysis to comprehend the priority of the traditional old dwellings using a sensibility measuring scale.

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Analysis of Lacquer and CNSL Using Infrared Spectrometer and Pyrolysis-GC/MS (적외선분광분석과 Py-GC/MS를 이용한 옻칠 및 캐슈칠도막 분석)

  • Choi, Jaewan;Kim, Soo-Chul
    • Journal of the Korean Wood Science and Technology
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    • v.46 no.1
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    • pp.1-9
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    • 2018
  • Nowadays, synthetic resin varnish such as cashew nut shell liquid (CNSL) is being used as well as traditional lacquer. The code of ethics states that material must be identical to the original when preserving cultural heritage. Therefore, lacquer should be used. However, problem is that even experts have difficulties differentiating lacquer and CNSL as they have similar components. Therefore, this study was carried out to identify the difference between lacquer and CNSL using IR and Py-GC/MS. As a result of IR, in lacquer, $720cm^{-1}$ peak was detected and in CNSL, $750cm^{-1}$, $720cm^{-1}$ and $700cm^{-1}$ peaks were detected. The results of Py-GC/MS detect benzene compounds and alkyl chains for both varnishes. However, hexanoic acid was detected from CNSL but not lacquer. Using these analytical methods, the differences between lacquer and CNSL can be identified on the scene. This is expected to be applied to the authentic conservation and restoration of lacquerware.

Development of HPTLC Fingerprinting and Phytochemical Study of a Polyherbal Unani Formulation

  • Alam, Abrar;Siddiqui, Javed Inam;Naikodi, Mohammed Abdul Rasheed;Kazmi, Munawwar Husain
    • CELLMED
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    • v.10 no.1
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    • pp.7.1-7.6
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    • 2020
  • Plants produce a wide range of active principles, making them a rich source of different types of medicines. Without any knowledge of the phytoconstituents or active principles the medicinal plants itself or in the form of polyherbal formulations, were used by all society of human being from ancient times for prevention and cure of disease, but most of the traditional formulations including the formulation of Ayurveda and Unani have not been scientifically validated in order to establish the pharmacopoeial standards to improve the efficacy. Globally, the people become conscious that uses of synthetic drugs for a long period is not safe; the trend of medical society at large is looking at alternatives from natural, safe sources to combat diseases. Due to this comprehension, it has been increased the demand for plant-derived medicine, and on the other side, it is extremely important to standardize the polyherbal formulations and validate them scientifically to improve their safety and efficacy. The polyherbal Unani formulation Safuf-e-Muallif is widely used and recommended in Unani system of medicine (USM) as a spermatogenic agent, semen thickening agent, etc. to treat sexual disorders viz. premature ejaculation, nocturnal emission, etc. The study mainly deals with phytochemical screening for the detection of nature of phytoconstituents and analytical technique like High-performance thin-layer chromatography (HPTLC) for developing fingerprint of Safuf-e-Muallif revealing specific identities of the drug. The phytochemical screening and HPTLC fingerprint profile for SM reported here may be used as a reference standard for quality control purpose in future.

Quantitative Analysis of Cinnamaldehyde, Cinnamylalcohol and Salicylaldehyde in Commercial Biopesticides Containing Cinnamon Extract Using Gas Chromatography - Flame Ionization Detector

  • Lim, Sung-Jin;Lee, Ji-Hye;Kim, Jin-Hyo;Choi, Geun-Hyoung;Cho, Nam-Jun;Park, Byung-Jun
    • Korean Journal of Environmental Agriculture
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    • v.33 no.3
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    • pp.213-219
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    • 2014
  • BACKGROUND: In an environment-friendly agriculture, plant extracts have been perceived as alternatives of synthetic pesticides. The Environment-friendly Agriculture Promotion Act of Korea has approved cinnamon extract as a matter for the production of commercial biopesticides. Thirteen commercial biopesticides containing cinnamon extract have been marketed locally. However, the analytical method for the quality control of these biopesticides containing cinnamon extract has not been studied. METHODS AND RESULTS: Cartridge clean-up method for the determination of cinnamaldehyde, cinnamylalcohol and salicylaldehyde in biopesticides containing cinnamon extract was developed and validated by gas chromatography (GC). The clean-up method was optimized with HLB SPE cartridges for the bioactive substance in biopesticides containing cinnamon extract, and the eluate was analyzed by GC. The developed method was validated, and the LOQ and recovery rates of cinnamaldehyde, cinnamylalcohol and salicylaldehyde were 0.139, 0.067 and $0.062mgL^{-1}$ and 84.2, 86.5 and 82.1%, respectively. The contents of cinnamaldehyde, cinnamylalcohol and salicylaldehyde were analyzed using the developed method in the 13 commercial biopesticides. Results showed 0.06-17.37%,