• Title/Summary/Keyword: Mass standards

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Measurement of Cortisol in Human Serum by Isotope Dilution Liquid Chromatography/Mass Spectrometry and a Comparison through a Proficiency Testing

  • Lee, Hwa-Shim;Shin, Hye-Sun;Park, Sang-Ryoul;Park, Chang-Joon
    • Bulletin of the Korean Chemical Society
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    • v.31 no.5
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    • pp.1149-1154
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    • 2010
  • Liquid chromatography/mass spectrometry using isotope dilution method has been established as a primary method for the measurement of cortisol in human serum. Verification of this method was accomplished by the participation in Consultative Committee for Amount of Substance-Metrology in Chemistry (CCQM) pilot study. Two levels of cortisol certified reference materials were prepared and certified by the established method. They were used as sample materials for the proficiency testing. The expanded uncertainty in the measurement of cortisol in human serum was approximately 1.2% at 95% confidence level. The results of the proficiency testing showed a good precision among the participants, but some bias to the certified values. This means that commercial field laboratories should keep traceability chain to SI unit through available reference measurement procedures and/or available reference materials.

Development of an Isotope-Dilution Liquid Chromatography/Mass Spectrometric Method for the Accurate Determination of Acetaminophen in Tablets

  • Shin, Hyun-Ju;Kim, Byung-Joo;Lee, Joon-Hee;Hwang, Eui-Jin
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3663-3667
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    • 2010
  • Acetaminophen (N-acetyl-p-aminophenol) is one of the most popular analgesic and antipyretic drugs. An isotope dilution mass spectrometric method based on LC/MS was developed as a candidate reference method for the accurate determination of acetaminophen in pharmaceutical product. After spiking an isotope labeled acetaminophen (acetyl-$^{13}C_2$, $^{15}N$-acetaminophen) as an internal standard, tablet extracts were analyzed by LC/MS in a selected reaction monitoring (SRM) mode to detect ions at m/z $152{\rightarrow}110$ and m/z $155{\rightarrow}111$ for acetaminophen and acetyl-$^{13}C_2$, $^{15}N$-acetaminophen, respectively. The repeatability and reproducibility of the developed ID/LC-MS method were tested for the validation and assessment of metrological quality of the method.

Study on the Measurement of TMP Pumping Speed (터보분자펌프(TMP) 배기속도 측정에 관한 고찰)

  • Kang, S.B.;Shin, J.H.;Cha, D.J.;Koh, D.Y.;Cheung, W.S.;Lim, J.Y.
    • Journal of the Korean Vacuum Society
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    • v.19 no.4
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    • pp.249-255
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    • 2010
  • Methods of the characteristics evaluation of turbo-molecular pumps (TMP) are well-defined in the international measurement standards such as ISO, PNEUROP, DIN, JIS, and AVS. The Vacuum Center in the Korea Research Institute of Standards and Science (KRISS) has recently designed, constructed, and established the integrated characteristics evaluation system of TMPs based on the international documents by continuously pursuing and acquiring the reliable international credibility through measurement perfection. The measurement of TMP pumping speed is normally performed with the throughput and orifice methods dependent on the mass flow regions. However, in the UHV range of the molecular flow region, the high uncertainties of the gauges, mass flow rates, and conductance are too critical to precisely accumulate reliable data. In order to solve the uncertainty problems of pumping speeds in the UHV range, we introduced a SRG with 1% accuracy and a constant volume flow meter (CVFM) to measure the finite mass flow rates down to $10^{-1}$ Pa-L/s with 3% uncertainty for the throughput method. In this way we have performed the measurement of pumping speed down to $10^{-4}$ Pa with an uncertainty of less than 6% for a 1000 L/s TMP. In this article we suggest that the CVFM has an ability to measure the conductance of the orifice experimentally with flowing the known mass through the orifice chambers, so that we may overcome the discontinuity problem encountering during introducing two measurement methods in one pumping speed evaluation sequence.

Effect of Ultrasonic Microdroplet Generation in the Low-Temperature Plasma Ionization-Mass Spectrometry

  • Lee, Hyoung Jun;Yim, Yong-Hyeon
    • Mass Spectrometry Letters
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    • v.10 no.4
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    • pp.103-107
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    • 2019
  • Low-temperature plasma (LTP) ionization is one of the ambient ionization methods typically used in mass spectrometry (MS) for fast screening of chemicals with minimal or no sample preparation. In spite of various advantages of LTP ionization method, including simple instrumentation and in-situ analysis, more general applications of the method are limited due to poor desorption of analytes with low volatilities and low ionization efficiencies in the negative ion mode. In order to overcome these limitations, an ultrasonic vibrator of a commercial hand-held humidifier was interfaced with an LTP ionization source, which generated microdroplets from sample solutions and assisted with LTP ionization. Ionization behaviors of various chemicals in microdroplet-assisted LTP (MA LTP) were tested and compared with typical LTP ionization from dried samples applied on a surface. MA LTP efficiently ionized small organic, amino, and fatty acids with low volatilities and high polarities, which were hardly ionized using the standard LTP method. Facile interaction of LTP with ultrafine droplets generated by ultrasonic resonator allows efficient ionization of relatively non-volatile and polar analytes both in the positive and negative ion modes.

Putative multiple reaction monitoring strategy for the comparative pharmacokinetics of postoral administration Renshen-Yuanzhi compatibility through liquid chromatography-tandem mass spectrometry

  • Sun, Yufei;Feng, Guifang;Zheng, Yan;Liu, Shu;Zhang, Yan;Pi, Zifeng;Song, Fengrui;Liu, Zhiqiang
    • Journal of Ginseng Research
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    • v.44 no.1
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    • pp.105-114
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    • 2020
  • Background: Exploring the pharmacokinetic (PK) changes of various active components of single herbs and their combinations is necessary to elucidate the compatibility mechanism. However, the lack of chemical standards and low concentrations of multiple active ingredients in the biological matrix restrict PK studies. Methods: A putative multiple reaction monitoring strategy based on liquid chromatography coupled with mass spectrometry (LC-MS) was developed to extend the PK scopes of quantification without resorting to the use of chemical standards. First, the compounds studied, including components with available reference standard (ARS) and components lacking reference standard (LRS), were preclassified to several groups according to their chemical structures. Herb decoctions were then subjected to ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry analysis with appropriate collision energy (CE) in MS2 mode. Finally, multiple reaction monitoring transitions transformed from MS2 of ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry were used for ultrahigh-performance liquid chromatography coupled with triple quadrupole mass spectrometry to obtain the mass responses of LRS components. LRS components quantification was further performed by developing an assistive group-dependent semiquantitative method. Results: The developed method was exemplified by the comparative PK process of single herbs Radix Ginseng (RG), Radix Polygala (RP), and their combinations (RG-RP). Significant changes in PK parameters were observed before and after combination. Conclusion: Results indicated that Traditional Chinese Medicine combinations can produce synergistic effects and diminish possible toxic effects, thereby reflecting the advantages of compatibility. The proposed strategy can solve the quantitative problem of LRS and extend the scopes of PK studies.

Improved Calibration for the Analysis of Emerging Contaminants in Wastewater Using Ultra High Performance Liquid Chromatography and Time-of-Flight Mass Spectrometry

  • Pellinen, Jukka;Lepisto, Riikka-Juulia;Savolainen, Santeri
    • Mass Spectrometry Letters
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    • v.9 no.3
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    • pp.77-80
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    • 2018
  • The focus of this paper is to present techniques to overcome certain difficulties in quantitative analysis with a time-of-flight mass spectrometer (TOF-MS). The method is based on conventional solid-phase extraction, followed by reversed-phase ultra high performance liquid chromatography of the extract, and mass spectrometric analysis. The target compounds included atenolol, atrazine, caffeine, carbamazepine, diclofenac, estrone, ibuprofen, naproxen, simazine, sucralose, sulfamethoxazole, and triclosan. The matrix effects caused by high concentrations of organic compounds in wastewater are especially significant in electrospray ionization mass spectroscopy. Internal-standard calibration with isotopically labeled standards corrects the results for many matrix effects, but some peculiarities were observed. The problems encountered in quantitation of carbamazepine and triclosan, due to nonlinear calibration were solved by changing the internal standard and using a narrower mass window. With simazine, the use of a quadratic calibration curve was the best solution.

A Study on the National Competency Standards of Fashion Accessories Production (패션소품생산 분야의 국가직무능력표준(NCS) 개발에 관한 연구)

  • Suh, Seung-Hee;Lee, Shin-Young
    • Journal of the Korean Society of Costume
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    • v.65 no.1
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    • pp.46-60
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    • 2015
  • This study analyzed the process of development and verification of standards through the competency analysis of fashion accessories products in the development of 'National Competency Standards'(NCS), which was carried out in 2013 for the fashion industry. The NCS for fashion accessories production was developed through three Focus Group Interviews (FGIs) and fashion accessories production was defined as "the process of design, development and manufacture intended to produce items that improve the degree of completion of fashion products that are produced from textile fabric, knitted fabric, leather and other materials such as bags, belts, hats, gloves, scarves, neckties and socks with the exception of clothes". The competency unit for fashion accessories production was analyzed in 11 categories: development of design; development of materials; production of prototype samples; calculation of cost; determination of mass production model and price; planning of main manufacture process; ordering of materials; planning for mass production; preparation for mass production; mass production; and inspection of completed products, and the verification was carried out on development outcomes through a survey carried out of on-site personnel. This study recommends the following direction for future improvements based on an analysis of the development process of the NCS for fashion accessories production. First, future development of standards should first provide a rational category system for each area of fashion good production based on the production process, which should be followed by a detailed competency survey. Second, in order to ensure a more efficient verification survey, an expert for each competency unit should be designated for the develop standard to induce a more sincere response. Also the questionnaire should require supplementation in order to collect the various additional opinions of experts of the field. Finally, this study concludes that it is urgent to procure an education infrastructure and specialized professors in order to apply the competency standard for fashion accessories production to the education sector. This study also concludes that the government will be required to provide systematic and consistent support aimed at supplementing development and forming a firm collaborative working environment for the industry and academia in order to improve the current education environment and build a more field-oriented education environment.

Development of the Ion Source of Glow Discharge/Mass Spectrometry for the determination of trace elements (미량원소 분석을 위한 GD/MS 이온원의 개발에 관한 연구)

  • Woo, Jin Chun;Lim, Heoung Bin;Moon, Dae Won;Lee, Kwang Woo;Kim, Hyo Jin
    • Analytical Science and Technology
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    • v.5 no.2
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    • pp.169-176
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    • 1992
  • Analytical detection limits and Relative Ion Yield (RIY) by a jet type ion source glow discharge mass spectrometer(GD/MS) have been measured. With a jet type ion source, the sample loss rate for a Cu sample is 0.23 mg/min with 0.1 L/min gas flow rate and 0.11 mg/min with no gas flow rate. However, the ion intensity of Cu does not change significantly with thee variation of the gas flow rate. The RIY values obtained from the calibration curves of the six copper based standards were between 0.57 of Fe and 3.5 of Cr. The detection limits of most elements were in the range of 0.9 and 2.0 ppm when the glow discharge was operated at 4 mA, 1000V.

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Quantification of $Cu(In_xGa_{1-x})Se_2$ Solar Cell by SIMS

  • Jang, Jong-Shik;Hwang, Hye-Hyen;Kang, Hee-Jae;Min, Hyung-Sik;Han, Myung-Sub;Suh, Jung-Ki;Cho, Kyung-Haeng;Chung, Yong-Duck;Kim, Je-Ha;Kim, Kyung-Joong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.275-275
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    • 2012
  • The relative composition of $Cu(InGa)Se_2$ solar cells is one of the most important measurement issues. However, quantitative analysis of multi-component alloy films is difficult by surface analysis methods due to severe matrix effect. In this study, quantitative depth profiling analysis of CIGS films was investigated by secondary ion mass spectrometry (SIMS). The compositions were measured by SIMS using the alloy reference relative sensitivity factors derived from the certified compositions and the total counting numbers of each element. The compositions measured by SIMS were linearly proportional to those by inductively coupled plasma-mass spectrometry (ICP-MS) using isotope dilution method. In this study, the quantification measured by ICP-MS method is compared with the composition calculated by SIMS depth profiles with AR-RSFs obtained from the reference. The SIMS depth profile of CIGS thin films according to the manufacturing condition was converted into compositional depth profile.

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