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Analytical Method for the Validation of Hispidulin as a Marker Compound for the Standardization of Salvia plebeia R. Br. Extracts as a Functional Ingredient (배암차즈기 추출물의 기능성원료 표준화를 위한 지표성분으로서 Hispidulin의 분석법 평가)

  • Jeon, Yoon Jung;Kwak, Hoyoung;Choi, Jong Gil;Lee, Je Hyuk;Choi, Soo Im
    • Korean Journal of Medicinal Crop Science
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    • v.24 no.4
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    • pp.271-276
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    • 2016
  • Background: In the present study, we established an HPLC (high performance liquid chromatography)-analysis method for the determination of marker compounds as a part of the material standardization for the development of health-functional foods from Salvia plebeia R. Br. extract. Methods and Results: The quantitative determination method of hispidulin as a marker compound was optimized by HPLC analysis using a YMC hydrosphere C18 column with a gradient elution system. This method was validated using specificity, linearity, accuracy, and precision tests. It showed a high linearity in the calibration curve with a coefficient of correlation ($r^2$) of 0.999995. The method was fully validated, and was sensitive, with the limit of detection (LOD) at $0.09{\mu}g{\cdot}m{\ell}^{-1}$ and limit of quantification (LOQ) at $0.27{\mu}g{\cdot}m{\ell}^{-1}$. The relative standard deviation (RSD) values of the data from intra- and inter-day precision were 0.05 - 0.22% and 0.32 - 0.42%, respectively, and the intra- and inter-day accuracy of hispidulin were 99.5 - 102.3% and 98.8 - 101.5%, respectively. The average content of hispidulin in Salvia plebeia R. Br. extract was $3.945mg{\cdot}g^{-1}$ (0.39%). Conclusions: These results suggest that the developed HPLC method is very efficient, and that it could contribute to the quality control of Salvia plebeia R. Br. extracts as a functional ingredient in health functional foods.

Analysis of Organic Acids in Urine by Gas Chromatography/Mass Spectrometry (기체 크로마토그래피/질량분석법을 이용한 요 중에서의 유기산 분석)

  • Yoo, Eun Ah;Ko, Sun Young;Kim, Jong Won;Kim, Jeong Uk;Myung, Seung Woon
    • Journal of the Korean Chemical Society
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    • v.41 no.9
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    • pp.471-482
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    • 1997
  • GC/MS was used to find an optimum experimental condition for the screening of organic acids in urine. Urinary organic acids were isolated through the liquid-liquid extraction method (LLE) to examine the influence of pH and the effect of including the back extraction and oximation processes respectively on the extraction. When pH was adjusted to 0.5 during the extraction without oximation process, relatively higher recovery rate and the smallest relative standard deviations (0.3-12.4%) were obtained. By removing the interference, the addition of back extraction made possible surer identification of organic acids with retention time of 15-16 minutes. Under this condition, we obtained the content distribution of urinary organic acids in healthy Korean children (n=16) by establishing the calibration curves for 51 standard organic acids.

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Analysis of formaldehyde using DNPH cartridge/LC-MS in the Ban-Woll.Shi-Hwa Industrial Complex (DNPH cartridge/LC-MS 방법에 의한 반월.시화산업단지의 폼알데하이드 분석에 관한 연구)

  • Cho Deok-Hee;Song Il-Seok;Kim In-Gu;Kim Woong-Soo;Kim Jong-Bo;Kim Tae-Hyun;Hwang Sun-Min;Nam Woo-Kyong
    • Journal of environmental and Sanitary engineering
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    • v.21 no.1 s.59
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    • pp.35-43
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    • 2006
  • Formaldehyde is important because of their irritant and toxic properties, mutagenicity and carcinogenicity. In this study, liquid chromatography-mass spectrometry (LC-MS) is used for the analysis of formaldehyde after derivatization with 2,4-dinitrophenylhydrazine (DNPH) cartridge. Analytical parameters such as linearity, repeatability and minimum detection limit were evaluated. The linearity ($r^2$) was 0.9997 when analyte concentration ranges from 25 to $200{\mu}g/l$. The relative standard deviation (%RSD) was 1.25 % for concentration of $200{\mu}g/l$. The minimum detection limit (MDL) was 0.73 ppbv. It was shown that LC-MS method has a great potential for formaldehyde analysis. The results of formaldehyde from the survey of Ban-Woll and Shi-Hwa Industrial Complex samples, the highest level was 6.20, 3.93 ppb, respectively. The highest emission level of formaldehyde at chemical plants in the Ban-Woll' Shi-Hwa Industrial Complex was 5421.25 ppb.

Modeling of Parasitic Source/Drain Resistance in FinFET Considering 3D Current Flow (3차원적 전류 흐름을 고려한 FinFET의 기생 Source/Drain 저항 모델링)

  • An, TaeYoon;Kwon, Kee-Won;Kim, SoYoung
    • Journal of the Institute of Electronics and Information Engineers
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    • v.50 no.10
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    • pp.67-75
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    • 2013
  • In this paper, an analytical model is presented for the source/drain parasitic resistance of FinFET. The parasitic resistance is a important part of a total resistance in FinFET because of current flow through the narrow fin. The model incorporates the contribution of contact and spreading resistances considering three-dimensional current flow. The contact resistance is modeled taking into account the current flow and parallel connection of dividing parts. The spreading resistance is modeled by difference between wide and narrow and using integral. We show excellent agreement between our model and simulation which is conducted by Raphael, 3D numerical field solver. It is possible to improve the accuracy of compact model such as BSIM-CMG using the proposed model.

Monitoring of Benzene, Toluene, Ethylbenzene and Xylene (BTEX) Residues in Arable Lands around Oil Reservoir (유류저장시설 인근 농경지 중 Benzene, Toluene, Ethylbenzene 및 Xylene (BTEX) 잔류량 모니터링)

  • Lim, Sung-Jin;Kim, Jin-Hyo;Choi, Geun-Hyoung;Cho, Nam-Jun;Hong, Jin-Hwan;Park, Byung-Jun
    • Korean Journal of Environmental Agriculture
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    • v.33 no.4
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    • pp.414-418
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    • 2014
  • BACKGROUND: Benzene, toluene, ethylbenzene and xylene (BTEX), which are volatile aromatic hydrocarbons and main constituents of gasoline, are neuro-carcinogenic organic pollutants in soil and groundwater. Korea Ministry of Environment has established the maximum permissible level of BTEX in arable soil to 1, 20, 50 and 15 mg/kg, respectively. METHODS AND RESULTS: To understand an arable soil contamination by BTEX, we collected 92 samples from the arable lands around oil reservoir, and analyzed the BTEX residue using a GC-MS with head-space sampler. A linear correlation between BTEX concentration and peak areas was detected with coefficient correlations in the range of 0.9807-0.9995. The method LOQ of BTEX was 0.002, 0.014, 0.084, and 0.038 mg/kg, respectively. Recoveries of 0.5 mg/kg BTEX were found to be 73.7-96.9%. The precision was reliable since RSD percentage (0.7-7.5%) was below 30, which was the normal percent value. Also, BTEX in all samples were detected under the LOQ. CONCLUSION: These results showed that the investigated arable soils around airport and oil reservoir in Korea were not contaminated by oils.

Analysis of Agrochemical Residues in Tobacco Using Solid Phase Microextraction-Gas Chromatography with Different Mass Spectrometric Techniques

  • Lee, Jeong-Min;Jang, Gi-Chul;Kim, Hyo-Keun;Hwang, Geon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.30 no.2
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    • pp.117-124
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    • 2008
  • A solid phase microextraction (SPME) method in combination with gas chromatography/mass spectrometric techniques was used for the extraction and quantification of 12 selected agrochemical residues in tobacco. The parameters such as the type of SPME fiber, adsorption/desorption time and the extraction temperature affecting the precision and accuracy of the SPME method were investigated and optimized. Among three types of fibers investigated, polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB), PDMS fiber was selected for the extractions of the agrochemicals. The SPME device was automated and on-line coupled to a gas chromatograph with a mass spectrometer. Mass spectrometry (MS) was used and two different instruments, a quadrupole MS and triple quadrupole MS-MS mode, were compared. The performances of the two GC-MS instruments were comparable in terms of linearity (in the range of 0.01$\sim$0.5 $\mu$g/mL) and sensitivity (limits of detection were in the low ng/mL range). The triple quadrupole MS-MS instrument gave better precision than that of quadrupole MS system, but generally the relative standard deviations for replicates were acceptable for both instruments (< 15%). The LODs was fully satisfied the requirements of the CORESTA GRL. Recoveries of 12 selected agrochemicals in tobacco yielded more than 80% and reproducibility was found to be better than 10% RSD so that SPME procedure could be applied to the quantitative analysis of agrochemical residues in tobacco.

Competitive Extraction and Trace Analysis of BTEX and MTBE by Solid-Phase Microextraction (SPME) (고체상미량추출법을 이용한 BTEX와 MTBE의 경쟁적 추출효과 및 미량분석에 관한 연구)

  • An, Sang-Woo;Chun, Suk-Young;Lee, Si-Jin;Park, Jae-Woo;Chang, Soon-Woong
    • Journal of Korean Society on Water Environment
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    • v.26 no.4
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    • pp.622-628
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    • 2010
  • In this study, Solid-phase microextraction (SPME) with GC/FID was studied as a possible alternative to liquid-liquid extraction for the analysis of BTEX and MTBE. Experimental parameters affecting the SPME process (such as kind of fibers, adsorption time, desorption time, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. Experimental parameters such as CAR/PDMS, adsorption time of 20 min, desorption time of 5 min at $250^{\circ}C$, headspace volume of 50 mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of BTEX and MTBE. The general affinity of analytes to CAR/PDMS fiber was high in the order p-Xylene>Toluene>Ethylbenzene>MTBE>Benzene. The linearity of $R^2$ for BTEX and MTBE was from 0.970 to 0.999 when analyte concentration ranges from $30{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.5% to 3.2% for concentration of $100{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for BTEX and MTBE were from $7.5{\mu}g/L$ to $15{\mu}g/L$, respectively.

Analysis of coenzyme Q 1O in dietary supplement by HPLC (HPLC를 이용한 건강기능식품 중 코엔자임 Q10 성분 분석)

  • No, Ki-Mi;Leem, Dong-Gil;Kim, Mi-Gyeong;Park, Kyoung-Sik;Yoon, Tae-Hyung;Hong, Jin;Park, Sun-Young;Jeong, Ja-Young
    • Journal of Food Hygiene and Safety
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    • v.26 no.1
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    • pp.12-15
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    • 2011
  • A method based on high-performance liquid chromatography (HPLC) with ultraviolet detection has been developed to quantify coenzyme Q10 (CoQ10) in raw materials and dietary supplements. Single-laboratory validation has been performed on the method to determine linearity, selectivity, accuracy, limits of quantification (LOQ) and repeatability for CoQ10. An excellent linearity (r=0.999) was observed for CoQ10 in the concentration range $15.625{\sim}500\;{\mu}g/ml$ in dietary supplement. Observed recovery of CoQ10 was found to be between 98.33 and 99.38%. LOQ was found to be $250\;{\mu}g/ml$ Repeatability precision for CoQ10 was between 0.15 and 0.21% relative standard deviation (RSD). Further, limited studies showed that some adulterants and degraded material could be satisfactorily separated from CoQ10 and identified.

Simultaneous Quantification of Three Marker Compounds in Samultang by HPLC/DAD (HPLC-DAD를 이용한 사물탕 중 3종 성분의 동시분석법 확립)

  • Won, Jin-Bae;Ma, Jin-Yeul;Lee, Jae-Hoon;Ma, Choong-Je
    • Korean Journal of Pharmacognosy
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    • v.40 no.4
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    • pp.298-302
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    • 2009
  • Samultang is one of traditional medicine composed of Paeonia lactiflora, Angelica gigas, Rehmannia glutinosa and Cnidium officinale. To develop simultaneous determination of paeoniflorin, decursin and 5-HMF in Samultang, a high performance liquid chromatography with diode array detector was used. To separate three marker components, Dionex $C_{18}$ column (5 ${\mu}m$, 120 ${\AA}$, 4.6 mm${\times}$150 mm) was used with a gradient elution system of water and methanol. UV wavelength of detector set at 230 nm and 280 nm. This method was validated by linearity, precision test and recovery test. Calibration curves of three standard components were showed good linear regression ($R^2$>0.9973). LOD and LOQ ranged from 0.08 ${\mu}g$/ml to 0.38 ${\mu}g$/ml and 0.25 ${\mu}g$/ml to 1.16 ${\mu}g$/ml, respectively. The relative standard deviations (RSDs) of data of the inter-day and intra-day experiments were less than 0.54% and 0.89%, respectively. The measured results of recovery test were varied from 93.36 to 107.79 with RSD values 0.01~1.45%. The established method was applied for separation of bio-conversion Samultang sample and compared with control sample.

A Study on the Mercury Emission Characteristic and Comparison Tests for Applicability of Latest Mercury Measuring Methods - Focus on the Cement Kiln - (시멘트 소성시설에서의 수은 배출특성 및 최신 측정방법 적용성 평가 연구)

  • Kim, Hyung-Chun;Kim, Hee-Jin;Kim, Jong-Hyeon;Kang, Dea-Il;Park, Jung-Min;Kim, Jeong-Hun
    • Journal of Korean Society for Atmospheric Environment
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    • v.33 no.3
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    • pp.241-250
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    • 2017
  • Recently, there has been growing interest in the emission characteristics and behavior of anthropogenic mercury compounds from emission sources. It is required to establish a standard for reliable mercury measurement method. Therefore, this study has evaluated the applicability of the new measurement method; Continuous Emission Monitoring (US EPA 30A, CEM). In addition, the reliability evaluation was conducted through Ontario Hydro Method (ASTM D6784, OHM) and Sorbent trap method (US EPA Method 30B). As a monitoring result for three months via CEM from cement kiln, the maximum mercury compounds concentration was about $600{\mu}g/Sm^3$. This is because of the various of raw materials and fuel, and the absence of mercury-control device. The mercury compounds concentrations of OHM, Sorbent trap and CEM were 13.64 $(3.33{\sim}32.41){\mu}g/Sm^3$, $13.94(5.97{\sim}23.44){\mu}g/Sm^3$ and $14.68(6.19{\sim}26.75){\mu}g/Sm^3$, respectively. The relative standard deviations (% RSD) of the three methods were 5.1~40.9%. The result of this study suggest that it is possible to apply the CEM in the cement kiln when, QA/QC such as calibration is verified.