• Title/Summary/Keyword: Absorption spectrometry

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Simultaneous Preconcentration and Determination of Trace Elements in Water Samples by Coprecipitation-Flotation with Lanthanum Hydroxide $[La(OH)_3]$

  • 김영상;김기찬
    • Bulletin of the Korean Chemical Society
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    • v.16 no.7
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    • pp.582-588
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    • 1995
  • The preconcentration and determination of trace Cd(Ⅱ), Cu(Ⅱ), Pb(Ⅱ), Mn(Ⅱ) and Zn(Ⅱ) in water samples were studied by the precipitate flotation using La(OH)3 as a coprecipitant. The analytes were quantitatively coprecipitated by adding 3.0 mL of 0.1 M La(Ⅲ) solution in a 1,000 mL water sample and adjusting the pH to 9.5 with NaOH solution. After the addition of the 1:8 mixed surfactant solution of each 0.1% sodium oleate and sodium lauryl sulfate, the solution was stirred with a magnetic stirrer for 10 minutes. The precipitates were floated to the surface by bubbling with nitrogen gas and collected in a small sampling bottle. The precipitates were dissolved in nitric acid and then the solutions were diluted to 25.00 mL with a deionized water. The analytes were determined by flame atomic absorption spectrometry. This procedure was applied to the waste water analysis. This technique was simple, convenient and especially rapid for the analysis of a large volume of sample. And also, from the recoveries of better than 92% which were obtained from real samples, this method could be judged to be applicable to the preconcentration and quantitative determination of trace elements in water samples.

FTIR study of gamma and electron irradiated high-density polyethylene for high dose measurements

  • Al-Ghamdi, Hanan;Farah, Khaled;Almuqrin, Aljawharah;Hosni, Faouzi
    • Nuclear Engineering and Technology
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    • v.54 no.1
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    • pp.255-261
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    • 2022
  • A reliable and well-characterized dosimetry system which is traceable to the international measurement system, is the key element to quality assurance in radiation processing with cobalt-60 gamma rays, X-rays, and electron beam. This is specifically the case for health-regulated processes, such as the radiation sterilization of single use medical devices and food irradiation for preservation and disinfestation. Polyethylene is considered to possess a lot of interesting dosimetric characteristics. In this work, a detailed study has been performed to determine the dosimetric characteristics of a commercialized high-density polyethylene (HDPE) film using Fourier transformed infrared spectrometry (FTIR). Correlations have been established between the absorbed dose and radiation induced infrared absorption in polyethylene having a maximum at 965 cm-1 (transvinylene band) and 1716 cm-1 (ketone-carbonyl band). We have found that polyethylene dose-response is linear with dose for both bands up to1000 kGy. For transvinylene band, the dose-response is more sensitive if irradiations are made in helium. While, for ketone-carbonyl band, the dose-response is more sensitive when irradiations are carried out in air. The dose-rate effect has been found to be negligible when polyethylene samples are irradiated with electron beam high dose rates. The irradiated polyethylene is relatively stable for several weeks after irradiation.

Development and validation of an analytical method to quantify baphicacanthin A by LC-MS/MS and its application to pharmacokinetic studies in mice

  • Jeon, So Yeon;Kim, San;Park, Jin-Hyang;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Analytical Science and Technology
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    • v.35 no.2
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    • pp.60-68
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    • 2022
  • In this study, we developed and validated a sensitive analytical method to quantify baphicacanthin A in mouse plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The standard calibration curves for baphicacanthin A ranged from 0.5 to 200 ng/mL and were linear, with an r2 of 0.985. The inter- and intra-day accuracy and precision and the stability fell within the acceptance criteria. Besides, we investigated the pharmacokinetics of baphicacanthin A following its intravenous (5 mg/kg) and oral administration (30 mg/kg). Intravenously injected baphicacanthin A showed biphasic elimination kinetics with high clearance and volume of distribution values. Furthermore, baphicacanthin A showed a rapid absorption but low aqueous solubility (182.51±0.20 mg/mL), resulting in low plasma concentrations and low oral bioavailability (2.49 %). Thus, we successfully documented the pharmacokinetic properties of baphicacanthin A using this newly developed sensitive LC-MS/MS quantification method, which could be used in future lead optimization and biopharmaceutic studies.

A Quantitative Study for Hydrothermal Alteration Zones using Short Wavelength Infrared Spectrometry (단파장적외선 분광분석법을 이용한 열수변질대 정량화 연구)

  • Kim, Yong-Hwi;Choi, Seon-Gyu;Ko, Kwang-Beom;Han, Kyeong-Soo;Koo, Min-Ho
    • Economic and Environmental Geology
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    • v.50 no.1
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    • pp.15-26
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    • 2017
  • Advanced argillic, argillic, and phyllic zones are the most important alteration patterns to predict the hidden ore body during exploration of hydrothermal deposits. We examined the quantitative relationship between the spectral absorption characteristics and the mineral content of the synthetic mixtures such as alunite-kaolinite and illite-kaolinite using short wavelength infrared (SWIR) spectroscopy. In the alunite-kaolinite mixtures, the spectral absorption characteristics of the alunite was highly correlated with the Hull quotient reflectance(0.99) and the kaolinite had the highest correlation with the Gaussian peak(0.92). Illite-kaolinite mixtures are essential for Gaussian deconvolution because of the overlap of absorption region. Illite and kaolinite mixtures indicate the high correlation of 0.93 and 0.98, respectively. The error ranges in the alunite-kaolinite(8%) and illite-kaolinite mixtures(5%) derived from SWIR were smaller than the ones(29% and 26%) obtained from X-ray diffraction(Rietveld) analysis. These results show that SWIR spectroscopic analysis is more reliable than XRD Rietveld analysis in terms of quantification of allowed minerals.

Bioequivalence of LesacinTM Tablet to Jeil CravitTM Tablet (Levofloxacin 100 mg) by Liquid Chromatography- Electrospray Tandem Mass Spectrometry (LC-MS/MS를 이용한 제일크라비트정(레보플록사신 100 mg)에 대한 레사신정 100 mg의 생물학적 동등성)

  • Lee, Jin-Sung;Choi, Sang-Jun;Ryu, Ju-Hee;Seo, Ji-Hyung;Lee, Myung-Jae;Kang, Jong-Min;Tak, Sung-Kwon;Kang, Jin-Yang;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.38 no.4
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    • pp.269-275
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    • 2008
  • The purpose of the present study was to evaluate the bioequivalence of two levofloxacin tablets, Jeil $Cravit^{TM}$ tablet (Jeil Pharm. Co., Ltd., Korea, reference drug) and $Lesacin^{TM}$ tablet (Ilhwa. Co., Ltd., Korea, test drug), according to the guidelines of Korea Food and Drug Administration (KFDA). Twenty-four healthy male Korean volunteers received two tablets containing levofloxacin 200 mg in a $2{\times}2$ crossover study. There was a one-week washout period between the doses. Plasma concentrations of levofloxacin were monitored for over a period of 24 hr after administration by using a high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The area under the plasma concentration-time curve from time zero to 24 hr ($AUC_t$), maximum plasma drug concentration ($C_{max}$) and time to reach $C_{max}\;(T_{max})$ were complied from the plasma concentration-time data. Analysis of variance (ANOVA) test was utilized for the statistical analysis of the parameters using logarithmically transformed $AUC_t$ and $C_{max}$. The 90% confidence intervals of the $AUC_t$ ratio and the $C_{max}$ ratio for $Lesacin^{TM}$/Jeil $Cravit^{TM}$ were $\log\;0.9527{\sim}\log\;0.9981$ and $\log\;0.8712{\sim}\log\;1.0556$, respectively. These values were within the acceptable bioequivalence intervals of $\log\;0.80{\sim}\log\;1.25$, recommended by KFDA. In all of these results, we concluded that $Lesacin^{TM}$ tablet was bioequivalent to Jeil $Cravit^{TM}$ tablet, in terms of rate and extent of absorption.

Gemological Characterization of B. C. Jade (비씨 제이드의 보석학적 연구)

  • Kim, Won-Sa;Wight, Willow
    • Journal of the Mineralogical Society of Korea
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    • v.21 no.2
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    • pp.177-182
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    • 2008
  • The Gemological characteristics of B.C. jade from Cassiar Mine, British Colombia, Canada, have been investigated, using polarizing microscopy, Mohs' hardness, refractive index and density measurements, X-ray powder diffraction, X-ray fluorescence spectrometry, ICP-MS, Infrared absorption spectrometry, and DTA/TGA. The B.C. jade is deeply green (spinach peen or olive green) in color and is translucent. It shows a resinous or waxy luster. The principal mineral of the material is tremolite-actinolite solid solution and minor amount of Cr-garnet and unidentified opaque minerals are accompanied. Mohs' hardness value ($5.5{\sim}6$). refractive index (1.62), and specific gravity (3.01) are measured. It is very highly tough and shows hackly fracture. The high Fe content ($Fe_2O_3\;4.14{\sim}4.66\;wt%$) in B.C. jade is attributable to a deepening of green color of the material. The B.C. jade starts to dehydrate at v and dehydration is completed at $1000.8^{\circ}C$, transforming tremolite-actinolite solid solution to enstatite, diopside, quartz, and water in its place. This possible reaction is supported by the weight loss of B.C. jade (1.93 wt%) at $1000.8^{\circ}C$ indicated by TGA curve.

Evaluation of a Sample-Pooling Technique in Estimating Bioavailability of a Compound for High-Throughput Lead Optimazation (혈장 시료 풀링을 통한 신약 후보물질의 흡수율 고효율 검색기법의 평가)

  • Yi, In-Kyong;Kuh, Hyo-Jeong;Chung, Suk-Jae;Lee, Min-Haw;Shim, Chang-Koo
    • Journal of Pharmaceutical Investigation
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    • v.30 no.3
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    • pp.191-199
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    • 2000
  • Genomics is providing targets faster than we can validate them and combinatorial chemistry is providing new chemical entities faster than we can screen them. Historically, the drug discovery cascade has been established as a sequential process initiated with a potency screening against a selected biological target. In this sequential process, pharmacokinetics was often regarded as a low-throughput activity. Typically, limited pharmacokinetics studies would be conducted prior to acceptance of a compound for safety evaluation and, as a result, compounds often failed to reach a clinical testing due to unfavorable pharmacokinetic characteristics. A new paradigm in drug discovery has emerged in which the entire sample collection is rapidly screened using robotized high-throughput assays at the outset of the program. Higher-throughput pharmacokinetics (HTPK) is being achieved through introduction of new techniques, including automation for sample preparation and new experimental approaches. A number of in vitro and in vivo methods are being developed for the HTPK. In vitro studies, in which many cell lines are used to screen absorption and metabolism, are generally faster than in vivo screening, and, in this sense, in vitro screening is often considered as a real HTPK. Despite the elegance of the in vitro models, however, in vivo screenings are always essential for the final confirmation. Among these in vivo methods, cassette dosing technique, is believed the methods that is applicable in the screening of pharmacokinetics of many compounds at a time. The widespread use of liquid chromatography (LC) interfaced to mass spectrometry (MS) or tandem mass spectrometry (MS/MS) allowed the feasibility of the cassette dosing technique. Another approach to increase the throughput of in vivo screening of pharmacokinetics is to reduce the number of sample analysis. Two common approaches are used for this purpose. First, samples from identical study designs but that contain different drug candidate can be pooled to produce single set of samples, thus, reducing sample to be analyzed. Second, for a single test compound, serial plasma samples can be pooled to produce a single composite sample for analysis. In this review, we validated the issue whether the second method can be applied to practical screening of in vivo pharmacokinetics using data from seven of our previous bioequivalence studies. For a given drug, equally spaced serial plasma samples were pooled to achieve a 'Pooled Concentration' for the drug. An area under the plasma drug concentration-time curve (AUC) was then calculated theoretically using the pooled concentration and the predicted AUC value was statistically compared with the traditionally calculated AUC value. The comparison revealed that the sample pooling method generated reasonably accurate AUC values when compared with those obtained by the traditional approach. It is especially noteworthy that the accuracy was obtained by the analysis of only one sample instead of analyses of a number of samples that necessitates a significant man-power and time. Thus, we propose the sample pooling method as an alternative to in vivo pharmacokinetic approach in the selection potential lead(s) from combinatorial libraries.

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Investigation on Reaction Products From Oxidative Coupling Reactions of 1-Naphthol By Manganese Oxide (망간산화물에 의한 1-Naphthol의 산화-결합 반응에 따른 반응산물 연구)

  • Lim, Dong-Min;Lee, Doo-Hee;Kang, Ki-Hoon;Shin, Hyun-Snag
    • Journal of Korean Society of Environmental Engineers
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    • v.29 no.9
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    • pp.989-996
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    • 2007
  • In this study, abiotic transformation of 1-naphthol(1-NP) via oxidative-coupling reaction and its reaction products were investigated in the presence of Mn oxides. The reaction products were characterized for their relative polarity using solvent extraction experiment and reverse-phase HPLC, and for structure using CCMS and LC/MS, and for absorption characteristics using UV-Vis spectrometry. The reaction products present in aqueous phase were more polar than parent naphthol and comprised of 1,4-naphthoquinon(1,4-NPQ) and oligomers such as dimers and trimers. Hydrophilic component present in water phase after solvent$(CH_2Cl_2)$ extractions was identified as naphthol polymerized products having molecular weight(m/z) ranging from 400 to 2,000, and showed similar UV-Vis. absorption characteristics to that of foil fulvic acid. Transformation of 1,4-NPQ, which is non-reactive to Mn oxide, to the polymerized products via cross-coupling reaction in the presence of 1-NP was also verified. In this experimental conditions(20.5 mg/L, 1-NP, 2.5 g/L $MnO_2$, pH 5), the transformation of 1-NP into the oligomers and polymerized products were about 83% of initial 1-NP concentrations, and more than 30% of the reaction products was estimated to be water insoluble fractions, not extracted by $H_2O$ methanol. Results from this study suggest that Mn oxide-mediated treatment of naphthol contaminated soils can achieve risk reduction through the formation of oligomers md polymer precipitation.

Fundamental Studies on the Development of On-line Monitoring of Trace Mercury in Drinking Water (음용수 중 수은 연속자동측정시스템의 개발에 관한 연구)

  • Chang, Soo-Hyun;Kim, Hyo-Jin;Kim, Sun-Tae;Kim, Young-Man
    • Analytical Science and Technology
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    • v.12 no.4
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    • pp.299-305
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    • 1999
  • The electrolyte cathode atomic glow discharge (ELCAD) is a new plasma source for direct determination of trace heavy metals in drinking and waste water. ELCAD has been successfully developed for on-line monitoring of heavy metals, however, shows difficulty to measure mercury. In this study, ELCAD has been modified to apply the atomic absorption spectrometry (AAS) for the direct determination of trace elements of mercury in flowing water.The fundamental characteristics of this new types of plasma source have been investigated and found that the pH of the solution, discharge voltage, and current are most important factors.The absorbance of 1.0 ppm Hg standard solution increases as pH of the solution increases from pH 1.0 to 3.0.However, % RSD of the absorbance also increases as the pH of solution increasesdue to plasma unstability.The detection limits of the standard solution of pH 1.5 and pH 3.0 are about 40 ppb and 10 ppb level, respectively.

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Confirming Animal Glue in Dancheong Sample by Pyrolysis/GC/MS (열분해/GC/MS에 의한 재현 단청 시편에서 아교의 확인)

  • Park, Jong Seo;Kim, Mi Jeong;Kim, Soon Kwan
    • Journal of Conservation Science
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    • v.32 no.1
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    • pp.21-32
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    • 2016
  • Animal glue is a traditional material used extensively as adhesive and binder in mother-of-pearl, wooden structure, traditional painting, etc. Analysis of animal glue is usually performed with IR(infrared spectroscopy) based on the IR absorption of functional group. But, it has a limitation in confirming animal glue when a sample consists of several materials because of overlapping of the absorption band. Py/GC/MS(pyrolysis/gas chromatography/mass spectrometry) is a useful tool in analyzing the constituent of polymeric materials like animal glue by identifying their pyrolysate with very small amount of sample. In this study, confirmation of animal glue in a Dancheong sample was tried with this method. Characteristic pyrolytic compounds of animal glue and tung oil used in Dancheong were identified. Dancheong sample painted with Noerok as a coloring material, animal glue and tung oil was prepared and it was possible to find characteristic peaks of animal glue after thermal degradation and artificial weathering experiment. From this, we found that animal glue can be detected using py/GC/MS in cultural heritage samples consisting of several materials and in different condition. IR was also tried to analyze Dancheong sample and the results were compared with those of py/GC/MS for the detection of animal glue.