• Title/Summary/Keyword: 정량검출한계

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The Effect of Proficiency in Environmental Sample Measurement on Analysis Results (환경시료 측정에서 분석자의 숙련도가 분석결과에 미치는 영향)

  • Yoon, Seok-Pyo;Kang, Seong Min;Son, Yeonmi;Jeon, Gang Weon
    • Journal of the Korea Organic Resources Recycling Association
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    • v.29 no.2
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    • pp.25-30
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    • 2021
  • This study investigated how the indicators of quality control are improved by proficiency in the measurement of phosphate concentration. In addition, analysis equipments were to be compared to see if there were any differences in measurements depending on the type of analysis device. In order to find out the effect of the proficiency of the analyst on the analysis results, three analysts measured phosphate concentration seven times in accordance with the Korean water pollution test standards, and met the quality control indices if repeated more than five times. The limit of quantification for phosphate was calculated at 0.02 mg/L. If the analysis devices are different, the absorbance and concentration of the samples near the limit of quantification are statistically significant difference.

Determination of Minimum Detectable Activity in Environmental Samples (환경방사능 측정에서의 검출한계치의 정량적 고찰 및 최소검출방사능 농도 계산)

  • Lee, Myung-Ho;Shin, Hyun-Sang;Hong, Kwang-Hee;Cho, Young-Hyun;Lee, Chang-Woo
    • Journal of Radiation Protection and Research
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    • v.24 no.3
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    • pp.171-184
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    • 1999
  • In this paper, using statistical theory the basic concepts and the formulars of lower limit of detection were deasribed. Assuming that risks of 5% are acceptable (95% confidence level), lower limits of detection were calculated on the measuring apparatus for alpha, beta and gamma nuclides. Also, on the basis concepts of lower limit of detection, the MDA values were calculated for the radionuclides detected easily in the environment. These results make it possible to evaluate confidence limits on the radioanalytical results in the environmental sample.

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Analysis of gibberellic acid from fruits using HPLC/UV-vis (HPLC/UV-vis을 이용한 과일류 중의 지베렐린 산 분석)

  • Ma, Kyung Na;Cho, Hyun-Woo;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.26 no.1
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    • pp.19-26
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    • 2013
  • Gibberllic acid ($GA_3$) is one of gibberellins (GAs) that are a class of plant growth hormones that exert profound and diverse effects on plant growth and development. $GA_3$ is essentially non-UV absorbing and is difficult to assay by UV-detector. For effective extraction of gibberellic acid from fruits by using liquid-liquid extraction, optimized pH and extraction solvent were established. The selective and sensitive derivative of $GA_3$ for HPLC/UV-vis was derivatized using phenacyl bromide, and the experimental factors, including reaction time, reaction temperature and amount of derivatizing reagent and base were investigated for the effective synthesis. The derivatized $GA_3$ with phenacyl bromide was effectively analyzed by HPLC/UV-vis. The structure of derivatized $GA_3$ was confirmed by HPLC/ESI-MS. For apple, LOD and LOQ were 0.008 mg/kg and 0.027 mg/kg, respectively. For pear, LOD and LOQ were 0.003 mg/kg, 0.012 mg/kg, respectively. The established method can be applied to more effective analysis of $GA_3$ from plant and food.

Establishment for analytical method of methanol in wet wipes by headspace gas chromatography (가스크로마토그래프-헤드스페이스를 이용한 물휴지 중 메탄올 정량법 확립 연구)

  • Choi, Yongkyu;Baek, Eunji;Min, Chungsik;Lee, Rheeda;Park, Soonyoung;Ahn, Jaehyung;Kim, Sangseop;Hong, Seonghwa;Kim, Younglim
    • Analytical Science and Technology
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    • v.29 no.5
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    • pp.242-247
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    • 2016
  • This research aims to set up and validate methods of analyzing the methanol in wet wipes and verifies the analysis methods that applied to the wet wipes. We used Headspace (HS) Gas Chromatography (GC) - Flame Ionization Detector (FID) to the establish analysis method of methanol in wet wipes and optimized heating temperature, heating time, GC conditions with column. The result indicated that 3 mL of sample in 20 mL headspace vial can be equilibrated efficiently in headspace sampler at 70 ℃ for 10 min and sample was measured by GC with spli injection mode(10:1). The results show that linearity from 1 to 100 ppm was over R2 0.9995, precision was RSD 1.83 % and accuracy(recovery rate) was 105.44 (±1.05 %) on water matrix and wet wipes matrix removed non-woven fabric. Also, monitoring results of total 20 cosmetics on the market, from 0.00017 to 0.00156 % of methanol was detected from wet wipes.

HPLC-based Analysis of Biogenic Amines in Aging-Cheese (HPLC를 이용한 숙성치즈로부터 바이오제닉 아민 분석법 개발)

  • Park, Jong-Hyuk;Lee, Sang-Cheon;Moon, Hye-Jung;Oh, Jeon-Hui;Song, Gi-Bong
    • Journal of Dairy Science and Biotechnology
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    • v.34 no.3
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    • pp.187-191
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    • 2016
  • Biogenic amines have been used as chemical indicators of fermented foods. So far, several chromatography methods have been developed to detect biogenic amines in foods. However, few methods have identified these compound in domestic cheese. We analyzed the biogenic amines (histamine dihydrochloride, tyramine hydrochloride, ${\beta}$-phenylethylamine hydrochloride, putrescine dihydrochloride, cadaverine, spermidine, tryptamine hydrochloride, ethanolamine hydrochloride and butylamine) in cheese by using HPLC. The calibration curves of the biogenic amines were found to be linear over the concentration range of 10-50 ppm with a correlation coefficient of above 0.99. The limit of detection (LOD) and limit of quantitation (LOQ) of the biogenic amines in the given order were 3.7 and 11.3 ppm, 3.4 and 10.4ppm, 3.4 and 10.3 ppm, 4.0 and 12.2 ppm, 3.4 and 10.4 ppm, 3.4 and 10.5 ppm, 3.5 and 10.7 ppm, 4.1 and 12.5 ppm, and 3.4 and 10.4 ppm, respectively. Recovery rates of the biogenic amines in the given order were 112, 104, 93, 108, 91, 102, 101, and 92%, respectively. The findings of this study suggest that HPLC is a suitable method for the determination of biogenic amines, thereby indicating its potential application in the quality control of aging cheese.

Determination of Polycyclic Aromatic Hydrocarbons in Smoked Food Products (훈연식품 중 polycyclic aromatic hydrocarbons 함량 분석)

  • Seo, Ilwon;Nam, Hejung;Lee, Songyoung;Lee, Kyueun;Shin, Han-Seung
    • Food Engineering Progress
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    • v.13 no.3
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    • pp.195-202
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    • 2009
  • This study was accomplished that analysis of seven polycyclic aromatic hydrocarbons (PAHs) in smoked or nonsmoked processing foods by high performance liquid chromatography (HPLC) with fluorescence detection. The calibration line was constructed with injected different levels of standard concentration. Limit of detection (LOD) and limit of quantification(LOQ) showed higher linearity ($r^{2}$=0.998) reasonably, and recovery exhibited 0.033-0.666 $\mu$g/kg, 0.108-2.217 $\mu$g/kg and 69.31-90.14%, respectively. As a result, the samples using smoked tuna as smoked materials contained seven PAHs with different range from 0.256 to 0.486 $\mu$g/kg. The benzo[a]pyrene, indicator of PAHs, was detected to below the LOQ in two samples. Concentrations of benzo[a]pyrene in three samples were below the 2 $\mu$g/kg which is the limit of regulation. Smoked tuna sauces were detected from 0.321 to 0.552 $\mu$g/kg and not detected in drying powders. PAHs of smoked meat products were ranged from 0.720 to 2.027 $\mu$g/kg and are higher than concentration of tuna smoked samples. PAHs were very low in non-smoked foods including mustard, herb, and roasted meats.

Determination of Oxycarboxin Residues in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 Oxycarboxin의 분석)

  • Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.2
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    • pp.117-124
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    • 2018
  • BACKGROUND: Oxycarboxin(5,6-dihydro-2-methyl-N-phenyl-1,4-oxathiin-3-carboxamide-4,4-dioxide) as oxanthiin is a systemic fungicide commonly used for control of various pathogens in agronomic and horticultural crops. In an effort to develop an analytical method to trace the fungicide, a method using HPLC equipped with UVD/MS was studied. METHODS AND RESULTS: Oxycarboxin was extracted with acetone from hulled rice, soybean, Kimchi cabbage, green pepper, and apple samples. The extract was diluted with saline water, followed by liquid-liquid extraction with methylene chloride. Florisil column chromatography was employed for the purification of the extracts. Oxycarboxin was determined on a Zorbax SB-AQ $C_{18}$ column by HPLC with UVD. Accuracy of the proposed method was validated by the recovery tests from crop samples fortified with oxycarboxin at 3 levels per crop. CONCLUSION: Mean recoveries ranged from 78.3% to 96.1% in five representative agricultural commodities. The coefficients of variation were less than 10%, and limit of quantitation of oxycarboxin was 0.04 mg/kg. A confirmatory technique using LC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. The method was reproducible and sensitive to determine the residue of oxycarboxin in agricultural commodities.

A Study on the Determination of Caffeine in Coffee, Black tea and Green Tea by high performance Liquid Chromatography (고속액체 크로마토크래피에 의한 커피, 홍차, 녹차중의 카페인 정량에 관한 연구)

  • 권익부;이윤수;우상규;이충영;서준걸
    • Journal of Food Hygiene and Safety
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    • v.5 no.4
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    • pp.213-217
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    • 1990
  • A simple and practical method for the determination of caffeine in coffee, black tea and green tea was studied. The analysis of caffeine was performed by reverse phase high perfomance liquid chromatography using a ${\mu}-Bondapak$ C18 column at isocratic condition with methanol-acetic acid-water (20: 1: 79) on UV detector at 280 nm. The extraction and clean-up of caffeine in sample is based on combing a simple pretreatment with the use of a Sep-Pak Alumina A cartridge. The average recoveries of caffeine from several samples were 95.2 -101.3%, the relative standard deviation for the whole procedure was 0.10 ~ 0.62%, and the detection limit of caffeine in sample solution was about $0.1\;\mu\textrm{g}\;per\;ml$.

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Determination of Total Chlorine Residuals by Flow Injection Analysis (흐름 주입 분석법에 의한 총 잔류염소의 정량)

  • Choi, Yong Wook
    • Journal of the Korean Chemical Society
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    • v.43 no.4
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    • pp.430-437
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    • 1999
  • The determination of total chlorine residuals in drinking water by flow injection analysis(FIA) with iodometric UV detection was investigated. The pH of the acid stream, the concentration of the iodide ion,the length of the mixing and reaction coils, the injection sample size, and flowrate were optimized as parameters for determining total chlorine residuals by FIA method. lodide was selectively oxidized to iodine by hypochlorite at pH 8.3 Ethylenediamine as masking agent for masking interference ions from the sample was given the best efficency. Calibration curve presented linear range of 0.03-3 mg/L for hypochlorite ion with a correlation coefficient of 0.999 or better. The detection limit was found to be 0.007 mg/L for hypochlorite ion. Under these analytical conditions, total chlorine residuals in several tap water sampled in the city of Jeonju were analyzed.

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