• Title/Summary/Keyword: analytical testing

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Analysis of Methamphetamine and Amphetamine in Oral Fluid of Eleven Drug Abusers (마약남용자 11명의 타액 중 메스암페타민의 분석)

  • Kim, Eun-Mi;Lee, Ju-Seon;Choi, Hye-Young;Choi, Hwa-Kyung;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.52 no.6
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    • pp.419-425
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    • 2008
  • A qualitative and quantitative analytical method was developed for detection of methamphetamine (MA) and its main metabolite amphetamine (AM) in oral fluid. Oral fluids of eleven drug abusers were provided by Police, specimens were collected by stimulation with a cotton swab treated with 20 mg of citric acid ($Salivette^{(R)}$; Sarstedt, USA). As the preliminary test, oral fluid samples were screened for amphetamines by Fluorescence Polarization Immunoassay (TDxFLx, Abbott Co.). Extraction for MA was performed using solid-phase extraction (SPE) by $RapidTrace^{TM}$ (Zymark, USA) with mixed mode cation exchange cartridge, CLEAN $SCREEN^{(R)}$ (130 mg/3 ml, UCT) after dilution with phosphate buffer. Samples were evaporated and derivatized by pentafluoropropionic acid anhydride (PFPA). Quantitation of MA and AM was performed by gas chromatography-mass spectrometry (GC-MS) using selective ion monitoring (SIM), the quantitation ions were m/z 204 (MA), 208 (MA-$D_5$), 190 (AM) and 194 (AM-$D_5$). The selectivity, linearity of calibration, limit of detection (LOD) and quantification (LOQ) within- and between day precision, accuracy and recoveries were examined as parts of the method validation. All oral fluid samples gave positive results to immunoassay for MA (cut-off level, 50 ng/ml as d-amphetamine). Concentrations of MA and AM by GC-MS in eleven samples were ranged 104.2${\sim}$4603.3 ng/ml and 32.4${\sim}$268.6 ng/ml, respectively. Extracted calibration curves of MA and AM were linear over the two concentration range of 1${\sim}$100 and 50${\sim}$1000 ng/ml with correlation coefficient of above 0.999. LOQ of MA and AM was 1 and 3 ng/ml, respectively. The intraand inter-day run precisions (CV) for MA and AM were less than 10%, and the accuracies (bias) for MA and AM were also less than 10% at the two different concentrations 5 and 100 ng/ml at low calibration range, 50 and 1000 ng/ml at high calibration range. The absolute recoveries of MA and AM at low and high calibration ranges were more than 82% and 75%, respectively. In this study the qualitative and quantitative analytical method of MA in oral fluid was established. Oral fluid testing may detect drug use in past hours because of its shorter detection window than urine, and be useful in post-accident situations. So oral fluids will be most useful for testing drug abuse in the driving under the influence of drug (DUID) as the alternative specimens of urine.

Study of sweat content analysis and latent fingerprint developing (땀의 성분 분석과 잠재지문 현출에 관한 연구)

  • Choi, Mi-Jung;Sun, Yale-Shik;Kim, Chang-Seong;Choi, Man-Sik;Sung, Nack-Do;Park, Sung-Woo
    • Analytical Science and Technology
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    • v.20 no.2
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    • pp.147-154
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    • 2007
  • Sweat contents were investigated for using those data to forensic purpose. The experiments of identifying sweat contents were as follow: 1) measurement of amino acids (aspartic acid, serine, glycine etc) by HPLC, 2) anions ($Cl^-$, $F^-$, and $SO{_4}^{2-}$) by IC and 3) trace elements (Cu, Zn, Li, B, etc.) by ICP-MS. Amino acid contents in sweat are varied with individual samples and glycine, threonine, alanine, valine and histidine are detected as the prime one. The detected anions are $Cl^-$(2167~4073 ppm) and $F^-$(454~582 ppm) mostly. Trace elements of Rb, Zn and Cu are detected and those concentrations are relatively very high. The compositions of sweat can be influenced by various factors (diet, anthropometric, characteristics, physical fitness, age, gender and the state of the health).

Introduction of a New Method for Total Organic Carbon and Total Nitrogen Stable Isotope Analysis of Dissolved Organic Matter in Aquatic Environments (수환경 내 용존성 유기물질의 총 유기탄소 및 총 질소 안정동위원소 신규 분석법 소개)

  • Si-yeong Park;Heeju Choi;Seoyeon Hong;Bo Ra Lim;Seoyeong Choi;Eun-Mi Kim;Yujeong Huh;Soohyung Lee;Min-Seob Kim
    • Korean Journal of Ecology and Environment
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    • v.56 no.4
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    • pp.339-347
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    • 2023
  • Dissolved organic matter (DOM) is a key component in the biogeochemical cycling in freshwater ecosystem. However, it has been rarely explored, particularly complex river watershed dominated by natural and anthropogenic sources, such as various effluent facility and livestock. The current research developed a new analytical method for TOC/TN (Total Organic Carbon/Total Nitrogen) stable isotope ratio, and distinguish DOM source using stable isotope value (δ13C-DOC) and spectroscopic indices (fluorescence index [FI] and biological index [BIX]). The TOC/TN-IR/MS analytical system was optimized and precision and accuracy were secured using two international standards (IAEA-600 Caffein, IAEA-CH-6 Sucrose). As a result of controlling the instrumental conditions to enable TOC stable isotope analysis even in low-concentration environmental samples (<1 mgC L-1), the minimum detection limit was improved. The 12 potential DOM source were collected from watershed, which includes top-soils, groundwater, plant group (fallen leaves, riparian plants, suspended algae) and effluent group (pig and cow livestock, agricultural land, urban, industry facility, swine facility and wastewater treatment facilities). As a result of comparing characteristics between 12 sources using spectroscopic indices and δ13C-DOC values, it were divided into four groups according to their characteristics as a respective DOM sources. The current study established the TOC/TN stable isotope analyses system for the first time in Korea, and found that spectroscopic indices and δ13C-DOC are very useful tool to trace the origin of organic matter in the aquatic environments through library database.

Analysis of the polychlorinated biphenyls in transformer oils using peak matching method (피크패턴법을 이용한 절연유 중 PCBs 분석)

  • Shin, Sun Kyoung;Kim, Hye-Jin;Chung, David;Jeon, Tae Wan;Kim, Jin Kyoung;Park, Seok Un;Chung, Young Hee;Chung, Il Rok
    • Analytical Science and Technology
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    • v.18 no.5
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    • pp.410-418
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    • 2005
  • PCBs had numerous uses such as hydraulic fluid, heat exchange fluid, sealant, lubricant, and carbonless copy paper. They are most likely found in electric utilities, power stations, industrial facilities, electronic manufacturing plants, petrochemical plants, railroad systems, electric equipment repair facilities, mining sites (active or abandoned), and military camps. Due to its outstanding chemical and thermal stabilities and electrical insulation properties, the commercial and industrial products of PCBs, such as Aroclors, Kaneclors, Clophens, Phenaclors etc., had been widely used as thermal oil and transformer oil from 1930s until the 1970s. The transformer oils were analyzed as a main source of polychlorinated biphenyls (PCBs) emission into the environment. Qualitative estimation of oil extracts as carried out with Aroclor 1242, 1248, 1254, 1260. The transformer oils contained the pure and mixed of Aroclor 1242, Aroclor 1254, and Aroclor 1260. Also, commercial screening kit of 20 ppm and 50 ppm were applied to the transformer oil samples.

Conventional Analytical and New Raman Spectroscopy-Based Methods for Detecting Benzo[a]pyrene in Food: Review and Perspective (식품 내 벤조피렌 분석법의 기존 연구동향 및 라만분광법 기반기술 전망)

  • Lee, Mi-Hyun;Yee, So-Yoon;Jin, Xuanyan;Choi, Dae Sik;Rhee, Hanju;Rhee, Jin-Kyu
    • Microbiology and Biotechnology Letters
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    • v.43 no.3
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    • pp.177-186
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    • 2015
  • With a view to supporting the provisions of the current Korean food code for the detection of Benzo[a]pyrene, various analytical methods of detection in foods were evaluated and established in terms of linearity, limits of detection/quantitation, efficiency, and accuracy, amongst others. It was observed that to improve the technologies involved in the application of these methods, complicated and combined preparation processes of foods, including extraction, separation and purification, have been the main focus of efforts at optimization. Recently, on-site quick reaction for the detection of hazardous substances in the environment and food materials aims at developing simplified examination processes, such as lable-free and non-invasive technological analysis, to reduce the costs and time involved in the examination. Herein, current benzo[a]pyrene detection methods are reviewed in addition to new Raman spectroscopy-based trials established to pursue improve the speed, simplicity and suitability of testing.

Evaluation of proficiency and improvement of accuracy on the analysis of brominated flame retardants (PBDEs) in ABS polymer (ABS수지 중 polybrominated diphenyl ether(PBDE)류 분석 숙련도 평가 및 정확도 향상)

  • Ryu, Jehoon;Kim, Dalho
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.446-452
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    • 2015
  • In order to evaluate and improve the ability of Korean testing laboratories to measure Polybrominated diphenyl ethers in acrylonitrile-butadiene-styrene (ABS), a proficiency test was organised by Korea Research Institute of Standards and Science (KRISS) based on ISO/IEC 17043. The proficiency test material used was 10 g of a granular ABS fortified with a mixture of congeners of PBDE (BDE-154, 183, 206, 209). Homogeneity and stability were investigated to assess the adequacy of the test material. The certified value established by KRISS based on the national reference was used for assigned value of each PBDE. The test materials were distributed to the 16 participating laboratories. The participating laboratories were requested to analyse the samples employing the methods used in their routine analysis. Each laboratory was given it’s own code to secure the anonymity. Participants results were evaluated with z-scores according to ISO/IEC 17043. The standard deviation for proficiency assessment was set by standard deviation of the participants results except for outlier. The results, the laboratory's performance and improvement of accuracy were discussed.

Fragility functions for eccentrically braced steel frame structures

  • O'Reilly, Gerard J.;Sullivan, Timothy J.
    • Earthquakes and Structures
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    • v.10 no.2
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    • pp.367-388
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    • 2016
  • Eccentrically braced frames (EBFs) represent an attractive lateral load resisting steel system to be used in areas of high seismicity. In order to assess the likely damage for a given intensity of ground shaking, fragility functions can be used to identify the probability of exceeding a certain damage limit-state, given a certain response of a structure. This paper focuses on developing a set of fragility functions for EBF structures, considering that damage can be directly linked to the interstorey drift demand at each storey. This is done by performing a Monte Carlo Simulation of an analytical expression for the drift capacity of an EBF, where each term of the expression relies on either experimental testing results or mechanics-based reasoning. The analysis provides a set of fragility functions that can be used for three damage limit-states: concrete slab repair, damage requiring heat straightening of the link and damage requiring link replacement. Depending on the level of detail known about the EBF structure, in terms of its link section size, link length and storey number within a structure, the resulting fragility function can be refined and its associated dispersion reduced. This is done by using an analytical expression to estimate the median value of interstorey drift, which can be used in conjunction with an informed assumption of dispersion, or alternatively by using a MATLAB based tool that calculates the median and dispersion for each damage limit-state for a given set of user specified inputs about the EBF. However, a set of general fragility functions is also provided to enable quick assessment of the seismic performance of EBF structures at a regional scale.

A study on the Determination of Trace Se and Bi in the Scalp Hair by Hydride Generation- Inductively Coupled Plasma Atomic Emission Spectrometry (수소화물발생 유도결합플라즈마 원자방출분광법에 의한 머리카락 시료 중 미량의 Se와 Bi의 분석에 관한 연구)

  • Choi, Beom Suk;Lee, Dong Kee
    • Analytical Science and Technology
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    • v.9 no.1
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    • pp.26-34
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    • 1996
  • A method to determine the trace amount of Se and Bi in the scalp hair using the hydride generation inductively coupled plasma atomic emmission spectrometry was studied. The optimum operation conditions of ICP for hydride generation are 0.6~0.8L/min for the carrier gas flow rate, and 6mm above the induction coil for the observation height. Hydrochloric acid concentrations for the optimum hydride generation conditions were greater than 1.5M when 2.5% $NaBH_4$ and NaOH were used, and greater than 0.5M when 2.5% $NaBH_4$ and 0.1% NaOH were used. Severe interference effects are observed from transition metals such as Cu and Ni, and they could be circumvented by the coprecipitation with lanthanum hydroxide.

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Determination of terbutaline in human plasma by coupled column chromatography (커플드칼럼크로마토그래피에 의한 사람 혈장 중 테르부탈린의 정량)

  • Ko, Mi Young;Jeon, Sang-Seol;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.28 no.2
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    • pp.125-131
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    • 2015
  • A method was developed and fully validated for the determination of terbutaline, a β2-receptor agonist, in human plasma. Plasma samples were prepared by solid-phase extraction with Sep-Pak silica, followed by high-performance liquid chromatography (HPLC). The terbutaline was pre-separated from the interfering components in plasma on a Luna C18 (2) column, and terbutaline and salbutamol as an internal standard were resolved and determined on a Luna Silica column. The two columns were connected by a switching valve equipped with silica pre-column. The pre-column was used to concentrate the terbutaline in the eluent from the C18 column before back-flushing onto the silica column with fluorescence detection at an excitation/emission wavelength of 276/306 nm. The method was shown to be specific by testing six different human plasma sources. Linearity was established for a concentration range of 0.4-20.0 ng/mL with a correlation coefficient of 0.9999. The lower limit of quantitation was 0.4 ng/mL with a precision of 10.1% as C.V.%.

Fundamental study on the development of the testing method of Triclosan with GC/ECD and GC/MS (GC/ECD 및 GC/MS를 이용한 트리클로산 정량분석에 관한 기초 연구)

  • Jeong, Hui-Jae;Lee, Jae-In;Kweon, Deok-Jun;Eom, Hui-Jeong;Choi, Zel-Ho;Choi, Ki-In
    • Analytical Science and Technology
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    • v.25 no.6
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    • pp.410-415
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    • 2012
  • In this study, a fundamental study was conducted to establish the method for quantitative analysis and pretreatment of triclosan, one of the chemicals to be used as bactericides, detergents, and sterilizers. The extraction efficiency of triclosan was the highest when it was extracted by soxhlet apparatus with n-hexane, and it showed a satisfactory result when the samples were analyzed with both GC/ECD and GC/MS. To evaluate the reproductivity of the results, each 30 reference samples made with paper filter and cotton wool was prepared in this study. From the results with high extraction effectiveness, low analysis deviation, and good statistical analysis data, the method for the extraction and analysis for triclosan were resonable for the paper and textile samples applied in this study.