• Title/Summary/Keyword: Primary standard gas

Search Result 40, Processing Time 0.027 seconds

Development and validation of a qualitative GC-MS method for methamphetamine and amphetamine in human urine using aqueous-phase ethyl chloroformate derivatization

  • Kim, Jiwoo;Sim, Yeong Eun;Kim, Jin Young
    • Analytical Science and Technology
    • /
    • v.33 no.1
    • /
    • pp.23-32
    • /
    • 2020
  • Methamphetamine (MA) is the most common and available drug of abuse in Korea and its primary metabolite is amphetamine (AP). Detection of AP derivatives, such as MA, AP, phentermine (PT), MDA, MDMA, and MDEA by the use of immunoassay screening is not reliable and accurate due to cross-reactivity and insufficient specificity/sensitivity. Therefore, the analytical process accepted by most urine drug-testing programs employs the two-step method with an initial screening test followed by a more specific confirmatory test if the specimen screens positive. In this study, a gas chromatography-mass spectrometric (GC-MS) method was developed and validated for confirmation of MA and AP in human urine. Urine sample (500 µL) was added with N-isopropylbenzylamine as internal standard and ethyl chloroformate as a derivatization reagent, and then extracted with 200 µL of ethyl acetate. Extracted samples were analysed with GC-MS in the SIM/ Scan mode, which were screened by Cobas c311 analyzer (Roche/Hitachi) to evaluate the efficiency as well as the compatibility of the GC-MS method. Qualitative method validation requirements for selectivity, limit of detection (LOD), precision, accuracy, and specificity/sensitivity were examined. These parameters were estimated on the basis of the most intense and characteristic ions in mass spectra of target compounds. Precision and accuracy were less than 5.2 % (RSD) and ±14.0 % (bias), respectively. The LODs were 3 ng/mL for MA and 1.5 ng/mL for AP. At the screening immunoassay had a sensitivity of 100% and a specificity of 95.1 % versus GC-MS for confirmatory testing. The applicability of the method was tested by the analysis of spiked urine and abusers' urine samples.

Development of Korean Condition Based Maintenance Systems to Monitor Naval Weapon Systems (해군 무기체계 한국형 상태진단시스템 발전방향 연구)

  • Oh, Kyungwon
    • Journal of Aerospace System Engineering
    • /
    • v.10 no.4
    • /
    • pp.67-74
    • /
    • 2016
  • The primary aim for using a Korean Condition Based Maintenance (CBM) system is to maintain military operational readiness using Interactive Collection Analysis Systems (ICAS) installed on naval vessels. Other aims are to preemptively provision maintenance and supply functions, to guarantee economical management of logistical assets, and to implement data driven equipment life cycle management. In order to accomplish these aims, it is necessary to establish standard system conditions. However, because manufacturers do not provide the technology necessary for maintenance management, it is required to retain component performance maps for each piece of equipment, and to accumulate data about frequently occurring fault patterns. This study confirms the validity of component performance maps using micro gas turbines and provides accumulated data on machine break downs. This would allow real time equipment performance checks and present performance trends. Then analysis would provide solutions for maintaining the best machine operating conditions with detailed maintenance manuals for operators. This study is a basis for further research to investigate additional ways to develop CBM using data obtained from naval vessels used in actual military operations.

Chemical Derivatization of Catecholamines for Gas Chromatography-Mass Spectrometry

  • Park, Sun-Young;Kang, Bo-Xin;Li, Quing;Kim, Hoon-Sik;Lee, Jun-Gae;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
    • /
    • v.30 no.7
    • /
    • pp.1497-1504
    • /
    • 2009
  • GC/MS analysis of catecholamines (CAs) in biological sample may produce poor reproducible quantitaion when chemical derivatization is used as the technique to form a volatile derivative. Significant quantities of the side products can be formed from CAs with primary amine during the derivatization reaction under un-optimized conditions. We have tested various chemical derivatization techniques in an attempt to find an optimum derivatization method that will reduce side product formation, enable to separate several catecholamine derivatives in GC chromatogram, and obtain significant improvement of detection sensitivity in GC/MS analysis. Whereas several derivatization techniques such as trimethylsilylation (TMS), trifluoroacylation (TFA), and two step derivatization methods were active, selective derivatization to form O-TMS, N-heptafluorobutylacyl (HFBA) derivative using N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) and N-methyl-bis(heptafluorobutyramide) (MBHFBA) reagents was found to be the most effective method. Moreover, this derivative formed by selective derivatization could provide sufficient sensitivity and peak separation as well as produce higher mass ion as base peak to use selected ion in SIM mode. Calibration curves based on the use of an isotopically labeled internal standard show good linearity over the range assayed, 1 ~ 5000 ng/mL, with correlation coefficients of > 0.996. The detection limits of the method ranged from 0.2 to 5.0 ppb for the different CAs studied. The developed method will be applied to the analysis of various CAs in biological sample, combined with appropriate sample pretreatment.

Emission Characteristics of Fine Particles from Thermal Power Plants (화력발전소의 미세먼지 배출특성)

  • Park, Sooman;Lee, Gayoung
    • KEPCO Journal on Electric Power and Energy
    • /
    • v.6 no.4
    • /
    • pp.455-460
    • /
    • 2020
  • In order to identify the characteristics of fine particle emissions from thermal power plants, this study conducted measurement of the primary emission concentration of TPM, PM10 and PM2.5 according to Korea standard test method (ES 01301.1) and ISO 23210 method (KS I ISO 23210). Particulate matters were sampled in total 74 units of power plants such as 59 units of coal-fired power plants, 7 units of heavy oil power plants, 2 units of biomass power plant, and 6 units of liquid natural gas power plants. The average concentration of TPM, PM10, PM2.5 by fuel are 3.33 mg/m3, 3.01 mg/m3, 2.70 mg/m3 in coal-fired plant, 3.02 mg/m3, 2.99 mg/m3, 2.93 mg/m3 in heavy oil plant, 0.114 mg/m3, 0.046 mg/m3, 0.036 mg/m3 in LNG plant, respectively. These results of TPM, PM10 and PM2.5 were satisfied with the standards of fine dust emission allowance in all units of power plants, respectively. Also, this study evaluated the characteristics of fine particle emissions by conditions of power plants including generation sources, boiler types and operation years and calculated emission factors and then evaluated fine particle emissions by sources of electricity generation.

An Ozone-based Advanced Oxidation Process for an Integrated Air Pollution Control System (복합대기오염 저감 시스템을 위한 오존 고속산화 기반 고도산화공정)

  • Uhm, Sunghyun;Hong, Gi Hoon;Hwang, Sangyeon
    • Applied Chemistry for Engineering
    • /
    • v.32 no.3
    • /
    • pp.237-242
    • /
    • 2021
  • Simultaneous removal technologies of multi-pollutants such as particulate matters (PMs), NOx, SOx, VOCs and ammonia have received consistent attention due to the enhancement of pollutant abatement efficiency in addition to the stringent environmental regulation and emission standard. Pretreatment of insoluble NO by an ozone oxidation can be considered to be more effective route for saving space occupation as well as operation cost in comparison with that of traditional selective catalytic reduction (SCR) process. Moreover the primary advantage of ozone oxidation process is that the simultaneous removal with acidic gas including SOx is also available. Herein, we highlight recent studies of multi-pollutant abatement via ozone oxidation process and the promising research topics for better application in industrial sectors.

A Study on the Collection and Analysis of Tire and Road Wear Particles(TRWPs) as Fine Dust Generated on the Roadside (도로변에서 발생되는 미세먼지로써 타이어와 도로 마모입자 채집과 분석 연구)

  • Kang, Tae-Woo;Kim, Hyeok-Jung
    • Journal of the Korean Recycled Construction Resources Institute
    • /
    • v.10 no.3
    • /
    • pp.293-299
    • /
    • 2022
  • Recently, various stakeholder are interested in microplastic to cause pollution of the marine's ecosystem and effort to conduct study of product's life cycle to reduce pollution of marine's ecosystem. The micorplastic refer to materials of the nano- to micro- sized units and it can be classified into primary and secondary. The primary microplastic mean the manufactured for use in the specific field such as the microbead of the cosmetic or cleanser. also, secondary mean the unintentionally generated during use of the product such as the textile crumb by the doing the laundry. Tire and Road Wear Particles(TRWPs) are also defined as secondary microplastic. Typically, TRWPs are created by friction between the tread compound's rubber of the tire and the surface of the road du ring the driving cars. Most of the generated TRWPs exist on the roadside and some of them were carried to marine by the rainwater. In this study, we perform the quantitative analysis of the TRWPs existed in fine dust at the roadside. So, we collected the dust from the roadside in Chungcheongnam-do's C site with a movement of 1,300 cars per the hour. The collected samples were separated according to size and density. And shape analysis was performed using the Scanning Electron Microscope(SEM). We were possible to discover a lot of TRWPs at the fine dust of the 100 ± 20 ㎛. And we analysis it u sing the Thermo Gravimetric Analysis(TGA) and Gas Chromatography/Mass Spectrometer(GC/MS) for the quantitative components from the tire. As a result, it was confirmed that TRWPs generated from the roadside fine dust were included the 0.21 %, and the tire and road components in the generated TRWPs consisted of the 3:7 ratio.

Characteristics and Sampling of Dioxins/Furans from Emission Gas and Fly Ash Produced in Municipal Waste Incinerator (도시 소각로 쓰레기 소각후 생성된 폐가스 및 비산재중에 포함된 다이옥신류의 측정 및 특성고찰)

  • Lim, Chae-Hyun;Kim, Hee-Taik;Sohn, Jung-Hyun;Chang, Yoon-Seok
    • Applied Chemistry for Engineering
    • /
    • v.8 no.5
    • /
    • pp.790-795
    • /
    • 1997
  • Polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofuransfurans are the archetype of toxic chemicals. So it has absorbed public attention. The majors primary sources of PCDDS and PCDFs are chemical, thermal and photochemical reactions. Municipal solid waste incinerator facilities has been reported as the major contributors of dioxins to the environment. In this paper, Dioxins and furans were examined emission gas and fly ash produced during combustion in municipal solid waste incinerator. More effective method for sampling, extraction was described. The sample was extracted using a soxhlet method and purified using silicagel, alumina and carbon fibre HPLC to remove interfering compound. The extract was then analyzed by HRGC/HRMS. The result of this study showed recovery standard was good and the data resembled those of thermal processes. Total dioxins and furans were $1076.20pg/Nm^3$ and $1452.34pg/Nm^3$ respectively. The amount of highly chlorinated compound was more than that of lowly chlorinated compound. The 2,3,7,8-substituted TCDD was Just 0.34% of the total dioxins/furans amount.

  • PDF

Optimization of Analytical Methods for Octacosanol in Related Health-functional Foods with GC-MS (GC-MS를 이용한 건강기능식품 중 옥타코사놀 분석법 개발 연구)

  • Lee, Jin Hee;Oh, Mi Hyune;Lee, Kyung Jin;Kim, Yang Sun;Keum, Eun Hee;Park, Ji Eun;Cho, Mee Hyun;Seong, Min Hye;Kim, Sang A;Kim, Mee hye
    • Journal of Food Hygiene and Safety
    • /
    • v.33 no.4
    • /
    • pp.266-271
    • /
    • 2018
  • The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health-functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we continue our research on developing analytical methods for the items. Octacosanol is the major component of polycosanol and is a high-molecular-mass primary fatty alcohol, obtained from sugar cane wax. Previous researchers have shown that octacosanol can lower cholesterol and has antiaggregatory properties, cytoprotective uses, and ergogenic properties for human health. Recently, octacosanol products have been actively introduced into the domestic market because of their functional biological activity. We have developed a sensitive and selective test method for octacosanol that the TMS derivatives by means of gas-chromatographic-tandem mass spectrometry (GC-MS). The trimethylsilyl ether derivative of the target analyte showed excellent chromatographic properties. The procedure was validated in the range of $12.5{\sim}200{\mu}g/L$. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.999, and the limits of detection (LOD) and limits of quantitation (LOQ) were $4.5{\mu}g/L$ and $13.8{\mu}g/L$, respectively. The high recoveries (92.5 to 108.8%) and precision (1.8 to 2.4%) obtained are in accordance with the established validation criteria. Our research can provide scientific evidence to amend the octacosanol test method for the Health-Functional Food Code.

Development and Validation of a Simultaneous Analytical Method for 5 Residual Pesticides in Agricultural Products using GC-MS/MS (GC-MS/MS를 이용한 농산물 중 잔류농약 5종 동시시험법 개발 및 검증)

  • Park, Eun-Ji;Kim, Nam Young;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
    • /
    • v.36 no.3
    • /
    • pp.228-238
    • /
    • 2021
  • The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. The extracts were cleaned up using MgSO4, primary secondary amine (PSA) and octadecyl (C18). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R2) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

Improvement of an Analytical Method for Methoprene in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 살충제 메토프렌의 잔류분석법 개선)

  • Park, Eun-Ji;Kim, Nam Young;Park, So-Ra;Lee, Jung Mi;Jung, Yong Hyun;Yoon, Hae Jung
    • Journal of Food Hygiene and Safety
    • /
    • v.37 no.3
    • /
    • pp.136-142
    • /
    • 2022
  • The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO4, primary secondary amine (PSA), and octadecyl (C18), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R2) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.