• Title/Summary/Keyword: 검량선

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Single Laboratory Validation and Uncertainty Estimation of a HPLC Analysis Method for Deoxynivalenol in Noodles (면류에서 HPLC를 이용한 데옥시니발레놀 분석법의 검증과 불확도 산정)

  • Ee, Ok-Hyun;Chang, Hyun-Joo;Kang, Young-Woon;Kim, Mee-Hye;Chun, Hyang-Sook
    • Journal of Food Hygiene and Safety
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    • v.26 no.2
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    • pp.142-149
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    • 2011
  • An isocratic high performance liquid chromatography (HPLC) method for routine analysis of deoxynivalenol in noodles was validated and estimated the measurement uncertainty. Noodles (dried noodle and ramyeon) were analyzed by HPLC-ultraviolet detection using immunoaffinity column for clean-up. The limits of detection (LOD) and quantification (LOQ) were 7.5 ${\mu}g$/kg and 18.8 ${\mu}g$/kg, respectively. The calibration curve showed a good linearity, with correlation coefficients $r^2$ of 0.9999 in the concentration range from 20 to 500 ${\mu}g$/kg. Recoveries and Repeatabilities expressed as coefficients of variation (CV) spiked with 200 and 500 ${\mu}g$/kg were $82{\pm}2.7%$ and $87{\pm}1.3%$% in dried noodle, and $97{\pm}1.6%$ and $91{\pm}12.0%$ in ramyeon, respectively. The uncertainty sources in measurement process were identified as sample weight, final volume, and sample concentration in extraction volume as well as components such as standard stock solution, working standard solution, 5 standard solutions, calibration curve, matrix, and instrument. Deoxynivalenol concentration and expanded uncertainty in two matrixes spiked with 200 ${\mu}g$/kg and 500 ${\mu}g$/kg were estimated to be $163.8{\pm}52.1$ and $435.2{\pm}91.6\;{\mu}g$/kg for dried noodle, and $194.3{\pm}33.0$ and $453.2{\pm}91.1\;{\mu}g$/kg for ramyeon using a coverage factor of two which gives a level of statistical confidence with approximately 95%. The most influential component among uncertainty sources was the recovery of matrix, followed by calibration curve.

Consideration of the analytical bias involved in the detection of total volatile organic compounds (TVOC) (총휘발성유기화합물 (TVOC) 검량의 오차인자에 대한 연구)

  • Kim, K.H.
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.489-495
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    • 2004
  • In this article, various aspects of errors involved in the measurement of TVOC were examined as part of study to develop the indoor pollution indices. For this purpose, TVOC term was computed by two different calibration approaches, i.e., by assuming all VOC are detected in the same manner as toluene and by summing up as many individual VOC as possible. The results of our study indicate that the common, toluene-based method suffers from errors inherent in the development of such theory. Consequently, it is concluded that more research efforts have to be directed to the improvement of such concept as TVOC.

Determination of trace arsenic in seawater by flow injection-hydride generation inductively coupled plasma mass spectrometry (연속흐름주입-수소화물생성-유도결합플라스마 질량분석장치를 이용한 바닷물표준시료중의 극미량 비소분석방법의 확립)

  • Suh, Jung-Ki
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.316-325
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    • 2008
  • An inductively coupled plasma mass spectrometry (ICP-MS) instrument equipped with flow injection-hydride generation system was used for the determination of trace arsenic in seawater sample. The accuracy in this method was verified by the analysis of certified reference materials (CRM) of seawater (CASS-4, NASS-5). The analytical results agreed with certified value within the range of uncertainty. The expanded uncertainties for CASS-4 and NASS-5 in this experiment were ranged from 6.2% to 6.8% obtained from repeated analyses of the CRMs (n=5). The detection limit of $As^+$ (m/z=74.9216) in this method was confirmed about 0.01 ug/kg. Linearity obtained from calibration curve of arsenic was excellent ($R^2=1$). The detection at $As^+$ (m/z=74.9216) and $AsO^+$ (m/z=90.9165) by using oxygen reaction gas in DRC mode was compared. Sensitivity at $AsO^+$ (m/z=90.9165) was decreased about 25-fold, but the analytical results are the same that at $As^+$ (m/z=74.9216).

Properties and biological studies on Cinnamic acid derivative of Minoxidil

  • Joon su Shin;Kim, Jong ho;Sang sup Jue;Kim, Kyung ho;Kim, Bak-kwang
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1996.04a
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    • pp.269-269
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    • 1996
  • 발모제에 관한 연구의 일환으로 현재 발모제로 쓰여지고 있는 미녹시딜에 구충제 또는 모근 혈관확장제 둥의 효능을 갖고 있는 씬나믹산을 반응시켜 새로운 화합물 (이하 CINMI라 칭함)을 만들었다. 이 화합물에 대하여 액성영향 및 반응시간 등 제반물성을 검토하고, 최적조건에서 흡광도를 측정하여 검량선을 작성하였으며, 그리고 결합구조 및 육모효과 등에 대하여 검토하였다.

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Determination of Seed Protein and Oil Concentration in Kiddny Bean by Near Infrared Spectroscopic Analysis (근적외 분광분석법을 이용한 강낭콩 종실단백질 및 지방의 비파괴 분석)

  • 이한범;최병렬;강창성;김영호;최영진
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.46 no.3
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    • pp.248-252
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    • 2001
  • Near infrared spectroscopy (NIRS) is a rapid and accurate analytical method for determining the composition of agricultural products and feeds. An important merit of the NIRS analytical system is consistent predictions across instruments. However, proper calibration is the most important factor for a NIRS analytical system. Forty samples were obtained from Kyonggi-do Agricultural Research and Extension Services, and used to develop calibrations for crude protein content and crude oil content. Calibrations equations were developed using multiple linear regression (MLR). Accuracy and precision of NIRS predictions were adequate for quality measurement for the two constituents in kidney bean seed. In calibration sample sets (N=30), multiple correlation coefficient between NIR and lab measurements is 0.90 for seed, 0.97 for powder in seed protein concentration and 0.40 for seed and 0.92 for powder in seed oil concentration, respectively. It is concluded that NIRS method is suitable for the determination of seed composition in whole kidney bean.

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Quantitative Analysis of Eupatilin and Jaceosidin in Artemisia herba (약쑥 함유 Eupatilin과 Jaceosidin 성분의 분석)

  • Ryu Su-Noh;Kang Sam Sik;Kim Ju Sun;Ku Bon Il
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.49 no.6
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    • pp.452-456
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    • 2004
  • Artemisia Herb is the dry aboveground part of Artemisia asiatica (Compositae). This is listed officially in the Korean Herbal Pharmacopoeia and used mainly in stopping all kinds of bleeding, regulating menses and curing menstrual disorders as well as in alleviating pain. Eupatilin and jaceosidin were isolated from Sazabalsuk and Sajuarisuk. and identified by means of spectral methods $(UV,\;^1H\;and\;^{13}C-NMR,\;MS) $ and quantitative analysis using HPLC. Regression equations for two flavonoid component standards obtained from Artemisia asiatica were $y=76069_x\;+\;107329\;(r=0.9999^{**})$ for eupatilin, $y=76651_x\;+\;77399\;(r=0.9996^{**})$ for jaceosidin. The eupatilin content of Sazabalsuk was 240mg, jaceosidin was 10mg in 100 g dry leaves. The Sajuarisuk were 330mg, 123mg in 100g dry leaves, respectively.

Comparative analysis of glycerin in cosmetics by LC/MS and 1H NMR (LC/MS와 1H NMR을 이용한 화장품속의 글리세린 비교분석)

  • Park, Gyo-Beom;Park, Chan Jo;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.400-405
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    • 2007
  • The comparative analysis of glycerin in cosmetic samples was carried out by LC/MS and $^1H$ NMR spectrometry. For the LC/MS analysis, aqueous solution was controlled in strong basic condition with sodium hydroxide, and benzoyl chloride was added to the solution for the derivatization of glycerin. The derivative was extracted using pentane and analyzed by the LC/MS. For the $^1H$ NMR analysis, sample was directly dissolved in $D_2O$ solvent without pretreatment. The quantitative analysis of glycerin was done by $^1H$ NMR ERETIC method. The analysis results of LC/MS and $^1H$ NMR showed that the calibration curves were a good linearity with $r^2=0.9991$ in the range of 0.1 to $10{\mu}g/mL$ and $r^2=1$ in the range of 25 to $500{\mu}g/mL$, respectively.

Studies of gas chromatographic analysis of malodorous S compounds in air (대기 중 악취황 성분들에 대한 GC 분석의 특성)

  • Kim, Ki-Hyun;Oh, Sang In;Choi, Y.J.
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.145-152
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    • 2004
  • In this study, analytical characteristics of S gas detection technique were investigated against four major reduced S compounds (including hydrogen sulfide; methyl mercaptan; dimethyl sulfide (DMS); and dimethyl disulfide (DMDS)). To analyze such properties, an analytical system was constructed by combining the GC/PFPD system with the loop injection method. The results of our analysis indicated that response behavior of S gases differs greatly between compounds; H2S exhibited the weakest sensitivity of all compounds, while DMDS with two S-atom compounds the strongest sensitivity. To learn more about their response behavior on GC/PFPD method, their calibration patterns were compared using the three arbitrarily set concentration ranges of low, intermediate, and high. The results showed that calibration patterns of each compound are distinguished because of different factors. There was a line of evidence that calibration of $H_2S$ was affected noticeably by adsorptive loss within the system, whereas those of DMS and DMDS were influenced most sensitively by such factor as the linearity response at a given PMT voltage setting. The overall results of our study suggest that quantification of malordorous S compounds require a better knowledge of compound-specific response behavior against GC detection.

Effect of SPR Chip with Nano-structured Surface on Sensitivity in SPR Sensor (나노형상을 가진 표면플라즈몬공명 센서칩의 감도 개선 효과)

  • Cho, Yong-Jin;Kim, Chul-Jin;Kim, Namsoo;Kim, Chong-Tai;Kim, Tae-Eun;Kim, Hyo-Sop;Kim, Jae-Ho
    • Food Engineering Progress
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    • v.14 no.1
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    • pp.49-53
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    • 2010
  • Surface plasmon resonance (SPR) which is utilized in thin film refractometry-based sensors has been concerned on measurement of physical, chemical and biological quantities because of its high sensitivity and label-free feature. In this paper, an application of SPR to detection of alcohol content in wine and liquor was investigated. The result showed that SPR sensor had high potential to evaluate alcohol content. Nevertheless, food industry may need SPR sensor with higher sensitivity. Herein, we introduced a nano-technique into fabrication of SPR chip to enhance SPR sensitivity. Using Langmuir-Blodgett (LB) method, gold film with nano-structured surface was devised. In order to make a new SPR chip, firstly, a single layer of nano-scaled silica particles adhered to plain surface of gold film. Thereafter, gold was deposited on the template by an e-beam evaporator. Finally, the nano-structured surface with basin-like shape was obtained after removing the silica particles by sonication. In this study, two types of silica particles, or 130 nm and 300 nm, were used as template beads and sensitivity of the new SPR chip was tested with ethanol solution, respectively. Applying the new developed SPR sensor to a model food of alcoholic beverage, the sensitivity showed improvement of 95% over the conventional one.