• Title/Summary/Keyword: Limit of Detection

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Comparison of isoButoxycarbonyl derivatives, tert.-butyldimethylsilyl derivatives, with US EPA Method in the sensitivity of Alkylphenols, Chlorophenols, and Bisphenol A Potential field-screening applications of GC/MS-SIM (기체 크로마토그래피/질량분석기를 이용한 field-screening 적용을 위한 알킬페놀류, 클로로페놀류 및 비스페놀 A의 isoBOC 유도체, TBDMS 유도체와 US EPA 방법의 비교)

  • Kim, Hyub;Hong, Jong-Ki;Kim, Yong-Hwa;Kim, Kyoung-Rae
    • Analytical Science and Technology
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    • v.15 no.3
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    • pp.196-213
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    • 2002
  • The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode followed by three work-up methods for comparison; EPA method, isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in water samples were extracted with dichloromethane. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1~109.9% (EPA method) and 90.3~126.6% (isoBOC derivatization and TBDMS derivatization), respectively. The method detection limit of bisphenol A for SIM were 0.732 ${\mu}g/{\ell}$ (EPA method), 0.002 ${\mu}g/{\ell}$ (isoBOC derivatization) and 0.021 ${\mu}g/{\ell}$ (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755~0.9981 (isoBOC derivatization), and 0.9908~0.9996 (TBDMS derivatization). When these methods were applied to treated wastewater sample from a polyethylene plant, the concentrations of 11 phenols were below the method detection limit.

A Study on the Analysis of Polycyclic Aromatic Hydrocarbons by RPLC/DAD (I) (RPLC/DAD를 이용한 Polycyclic Aromatic Hydrocarbon류의 분석에 관한 연구(I))

  • Lee, Won;Hong, Jee-Eun;Park, Song-Ja;Pyo, Hee Soo
    • Analytical Science and Technology
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    • v.10 no.5
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    • pp.315-324
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    • 1997
  • The retention behaviors of 16 PAHs and 4 nitro-PAHs were studied with several parameters involved numbers of carbon atoms, F factor, aqueous solubility, L/B ratio, and numbers of interfering hydrogen atom pairs on the chemical structures of PAHs by using reversed-phase liquid chromatography/diode array detection method (RPLC/DAD) and gradient elution method. It was obtain that the log k' for most of PAHs with increasing the number of carbon and the F factor in their molecules. Chromatographic retention of PAH isomers and nitro-PAHs were examined with aqueous solubility, L/B ratio and number of interfering hydrogen atom pairs. As a result of comparison with these factors and retention times, it was found that those solutes having larger aqueous solubilities and greater L/B ratios were retained longer on stationary phase. This tendency was also occured in the molecules having the more number of interfering hydrogen atom pairs. Detection limits of PAHs which were obtained with three times measurements by RPLC/DAD were in the range of 100~500ng/mL and method detection limit(MDL) for water sample were in the range of 0.1~0.5ng/mL.

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Determination of Haloperidol Serum Levels in Psychiatric Patients with Gas Chromatography-Nitrogen Phosphorus Detection (GC/NPD를 이용한 정신분열증 환자의 혈중 Haloperidol 정량분석)

  • Paik, Man-Jeong;Kang, Bo-Kyoung;Lee, Kyoung-Ok;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.11 no.3
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    • pp.161-166
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    • 1998
  • Analytical method of haloperidol (HAL) in serum which has been widely used in therapy of schizophrenic disorders is developed. Gas chromatography/nitrogen-phosphorus detection (GC/NPD) was used for this study. Bromoperidol was used as an internal standard and diethylether as a solvent of three-step extraction. The extraction yield in this procedure was $67.5{\pm}1.9%$ at 15 ng/mL. A good linear response in the range of 1~40 ng/mL was obtained with correlation coefficient of $r^2=0.999$. Detection limit was 0.5 ng/mL when 2 mL of serum was used. This method was applied for the analysis of HAL in serum of schizophrenic patients. After HAL decanoate (HD) was intaken as intramuscular route, HAL levels were determined at second week and forth week. From the result, the concentration of HAL at forth week appeared to 29.6% lower than those at second week. The present method showed low detection limit and high selectivity. Therefore it can be applied for the trace analysis of HAL in serum and the monitoring.

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Analysis of Butyltin Compounds(mono-, di-, and tributyltin) in Human Blood (혈액 중의 주석화합물(MBT, DBT, TBT)의 분석과 농도에 관한 연구)

  • Kim, Nam Sook;Park, Dong Uk;Oh, Jae Ryoung;Shim, Woon Joon
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.115-122
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    • 2001
  • Butyltin compounds, including mono-(MBT), di-(DBT) and tributyltin(TBT) were analyzed in 44 human blood samples randomly collected from a hospital in "K" a city. Gas chromatograph equipped with flame photometric detector(FPD) was used to quantify the amounts of butylin compounds. Method detection limits(MDL) of this analytical method were 3.69ng Sn/g for MBT, 0.91ng Sn/g for DBT and 1.09ng Sn/g wet wt for TBT respectively. Standard reference material(SRM) containing of $1.3{\mu}g/g$ TBT as chloride was analyzed to check if this analytical results would be reliable. Recovery of about 90% was obtained through this analysis, indicating that the analytical method from butyltin compounds blood was reliable. The concentrations of butyltin compounds ranged MDL(<3.69) to 7.93ng Sn/g for MBT and 1.15 to 5.41ng Sn/g wet wt for DBT. Tributyltin was below detection limit in all samples. Detection limits of our results are lower than those reported by Kannan et al. who reported butyltin compounds in 33 human blood samples in the United States. Detection of MBT and DBT on blood sample implies that butyltin compounds could be absorbed through consumption of seafoods or exposure to food stuffs made of plastics and household items. Further study is needed to examine if butyltin compounds in blood can be reliably analyzed and used as intake index.

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Analysis of Biurea Decomposed from Azodicarbonamide in Food Products by High Performance Liquid Chromatography Mass/Mass Spectrometry (LC/MS/MS를 이용한 식품 중 아조디카르본아미드 분해산물인 Biurea 함량 분석)

  • Lim, Ho-Soo;Pahn, Kyeong-Nyeo;Kim, Jun-Hyun;Jang, Gui-Hyeon;Moon, Gui-Im;Yang, Hyo-Jin;Park, Sung-Kwan;Park, Hae-Kyong;Kim, So-Hee
    • Korean Journal of Food Science and Technology
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    • v.42 no.4
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    • pp.377-382
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    • 2010
  • This study was conducted to establish a method to analyze biurea decomposed from azodicarbonamide in processed foods such as wheat flour and bread. New method was developed using high performance liquid chromatography mass/mass spectrometry to determine biurea in wheat flour and bakery products. The recovery rate was 94.3-112.5%. The limit of detection for biurea was 0.003 mg/kg, and the limit of quantification was 0.01 mg/kg. The monitoring results for biurea content using established methods showed that biurea was detected at 2.76 mg/kg in the azodicarbonamide-detected flour (detection rate, 2%). The detection rate in processed foods such as baked goods was 27% (16/59). The detection range was 0.19-18.01 mg/kg (average, 3.79 mg/kg). However, it was thought that the detection level was safe due to much lower values than the standard (45 mg/kg). As a result, the newly established biurea analytical method will contribute to the management of azodicarbonamide in processed foods such as wheat flour and bakery products.

The Rapid Detection of Pathogens in Organically Grown Vegetables Using PCR-DGGE (PCR-DGGE를 이용한 유기농 채소의 유해 미생물 신속 검지)

  • Kwon, Oh Yeoun;Son, Seok Min
    • Food Engineering Progress
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    • v.15 no.4
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    • pp.370-375
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    • 2011
  • In this study the polymerase chain reaction (PCR) combined with denaturing gradient gel electrophoresis (DGGE) was evaluated as a method permitting the rapid detection of pathogens in fresh originally grown vegetables. A universal primer (341GCf/534r) was selected for its ability to amplify the V3 region of 16S-rRNA genes in their target pathogens (Salmonella typhimurium, Pseudomonas fluorescens, Bacillus cereus, Listeria monoytogenes, Staphyloocus aureus, E. coli). The 194 bp fragments in PCR were successfully duplicated as expected. The amplified fragments of the same size from six different pathogens also showed good separation upon DGGE. The detection limit of PCR-DGGE for six pathogens in fresh-cut lettuces were over $10^{5}$ CFU/g when sampled by stomaching. However, when the sampling method was changed from stomaching to shaking, the detection limit of six pathogens in organic vegetables was shown to increase by over $10^{1}$ CFU/g, but only those of B. cereus were over $10^{3}$ CFU/g. Therefore, PCR-DGGE was shown to be a reliable method for the detection of pathogens in fresh-cut vegetables.

Development of a deep-learning based automatic tracking of moving vehicles and incident detection processes on tunnels (딥러닝 기반 터널 내 이동체 자동 추적 및 유고상황 자동 감지 프로세스 개발)

  • Lee, Kyu Beom;Shin, Hyu Soung;Kim, Dong Gyu
    • Journal of Korean Tunnelling and Underground Space Association
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    • v.20 no.6
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    • pp.1161-1175
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    • 2018
  • An unexpected event could be easily followed by a large secondary accident due to the limitation in sight of drivers in road tunnels. Therefore, a series of automated incident detection systems have been under operation, which, however, appear in very low detection rates due to very low image qualities on CCTVs in tunnels. In order to overcome that limit, deep learning based tunnel incident detection system was developed, which already showed high detection rates in November of 2017. However, since the object detection process could deal with only still images, moving direction and speed of moving vehicles could not be identified. Furthermore it was hard to detect stopping and reverse the status of moving vehicles. Therefore, apart from the object detection, an object tracking method has been introduced and combined with the detection algorithm to track the moving vehicles. Also, stopping-reverse discrimination algorithm was proposed, thereby implementing into the combined incident detection processes. Each performance on detection of stopping, reverse driving and fire incident state were evaluated with showing 100% detection rate. But the detection for 'person' object appears relatively low success rate to 78.5%. Nevertheless, it is believed that the enlarged richness of image big-data could dramatically enhance the detection capacity of the automatic incident detection system.

Validation and Content Analysis of Putrescine in the Venom of Honeybee (Apis mellifera L.) (서양종꿀벌 일벌독에 함유된 putrescine 밸리데이션 및 함량 분석)

  • Choi, Hong Min;Kim, Hyo Young;Kim, Se Gun;Han, Sang Mi
    • Korean journal of applied entomology
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    • v.60 no.3
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    • pp.263-268
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    • 2021
  • The venom of honeybees (Apis mellifera L.) is used to treat many diseases because of its anti-inflammatory and analgesic effects. Bee venom consists of several biologically active molecules and exhibits remarkable anti-cancer effects. However, biological amines, which exhibit diverse functionality such as anti-inflammatory and antibacterial effects, have not been previously reported in bee venom. In this study, we determined the content of putrescine in bee venom by using ultra-performance liquid chromatography. The specificity, accuracy, and precision of the assay were assessed, and the assay validated. The linearity of the putrescine assay was r ≥ 0.99, indicating a moderate level of putrescine in the bee venom. The limit of detection and limit of quantification were both 0.9 ㎍/mL, while the rate of recovery was 96.4%-99.9%. The relative standard deviation (RSD) of the intra-day precision and inter-day precision of the putrescine assay were 0.16% - 0.23% and 0.09% - 0.36%, respectively, with the RSD ≤ 5% indicating excellent precision. Thus, the linearity, limit of detection, limit of quantification, and recovery rate of the putrescine assay were satisfactory. The analysis of the bee venom showed that the putrescine content was 3.1 ± 0.09 mg/g. This study provides fundamental data on putrescine content in bee venom, which will prove useful in further studies of its bioactivity.

Analysis of Cadaverine and Its Worker Honeybee Venom Content (Apis mellifera L.) (꿀벌(Apis mellifera L.) 일벌독의 생체아민 cadaverine 함량 및 분석법)

  • Choi, Hong Min;Kim, Hyo Young;Kim, Se Gun;Han, Sang Mi
    • Journal of Life Science
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    • v.31 no.2
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    • pp.144-148
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    • 2021
  • This study aimed to analyze the content and composition of a biological amine, cadaverine, isolated from the venom of worker honeybees (Apis mellifera L.). This biological amine―which has diverse functionality, such as anti-inflammatory and antibacterial effects―has not been previously reported in bee venom. An assay completed in 13 minutes was developed for the cadaverine present in the bee venom using an ultra-performance liquid chromatograph and a Halo C18 column with acetonitrile and water as the mobile phase. The specificity, accuracy, and precision of the assay were verified, and the assay was validated. The linearity for cadaverine in the bee venom was R2=0.99 or above, indicating a moderate level. The limit of detection and limit of quantification were both 0.3 ㎍/ml, and the rate of recovery was 97.6%-99.1%. The relative standard deviation (RSD) of the intra-day precision and inter-day precision for cadaverine was 0.25%-0.44% and 0.25%-1.25%, respectively, with an RSD that fell within 5% indicating excellent precision. Through this novel assay, it was found that the mean content of cadaverine was 1.10±0.05 mg/g. Our results indicated that the linearity, limit of detection, limit of quantification, and rate of recovery of the cadaverine assay were of a satisfactory level, and the cadaverine content of the bee venom was ably determined. This study provides basic data on cadaverine in bee venom, which will prove useful in further studies on the bioactivity of this component.

Determination and Validation of Synthetic Antioxidants in Processed Foods Distributed in Korea

  • Park, Hyeon-Ju;Seo, Eunbin;Park, Jin-Wook;Yun, Choong-In;Kim, Young-Jun
    • Journal of Food Hygiene and Safety
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    • v.37 no.5
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    • pp.297-305
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    • 2022
  • Antioxidants are food additives that extend the shelf life of food products by preventing lipid rancidity caused by active oxygen. They can either be naturally-derived or manufactured synthetically via chemical synthesis. In this study, method validation of five synthetic antioxidants, namely butylated hydroxyanisole, butylated hydroxytoluene, tertiary butylhydroquinone, propyl gallate, and disodium ethylenediaminetetraacetic acid, was performed using a high performance liquid chromatography-ultraviolet visible detector, and the method applicability was evaluated by analyzing foods containing antioxidants. The coefficient of determination (R2) average was 0.9997, while the limit of detection and limit of quantification were 0.02-0.53 and 0.07-1.61 mg/kg, respectively. The intra and inter-day accuracies and precisions were 83.2±0.7%-98.7±2.1% and 0.1%-5.7% RSD, respectively. Inter-laboratory validation for accuracy and precision was conducted using the Food Analysis Performance Assessment Scheme quality control material. The results satisfied the guidelines presented by the AOAC International. In addition, the expanded uncertainty was less than 16%, as recommended by CODEX. Consequently, to enhance public health safety, the results of this study can be used as basis data for evaluating the intake of synthetic antioxidants and assessing their risks in Korea.