• 제목/요약/키워드: Mass standards

검색결과 465건 처리시간 0.033초

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
    • /
    • 제31권5호
    • /
    • pp.1149-1154
    • /
    • 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
    • /
    • 제31권12호
    • /
    • pp.3663-3667
    • /
    • 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.

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

  • 강상백;신진현;차덕준;고득용;정완섭;임종연
    • 한국진공학회지
    • /
    • 제19권4호
    • /
    • pp.249-255
    • /
    • 2010
  • 터보분자펌프(TMP)의 특성평가는 ISO, PNEUROP, DIN, JIS, AVS 등 세계 여러 나라의 표준제정기구에서 제정한 국제규격에 그 근거를 두고 있다. 한국표준과학연구원에서는 이러한 국제규격에 기반을 둔 터보분자펌프의 특성평가시스템을 자체 설계/제작하여 그 신뢰성을 확인하기 위해 개발품 및 상용품의 평가에 주력하고 있다. 터보분자펌프의 배기속도 측정방법으로서 기체흐름 영역에 따른 throughput method와 orifice method를 적용하고 있으나 측정게이지, 유량계 및 orifice conductance의 불확도 등 실질적으로 정확한 배기속도를 제시하기 위한 조건들의 제약 때문에 많은 측정오차를 포함하고 있다고 볼 수 있다. 이러한 배기속도의 측정오차를 줄이기 위한 하나의 고찰로서 본 논문에서는 $10^{-1}$ Pa-L/s 영역까지의 유량 주입범위를 가지는 기 구축된 정적법을 이용한 유량주입에 기반을 둔 throughput method를 이용하여 1000 L/s TMP의 측정 능력을 검증하고자 한다. 또한 분자류 영역인 orifice method를 사용할 경우 고진공영역, 미세유량 주입영역으로 진입할수록 커질 수밖에 없는 배기속도 측정 불확도를 최소화시키기 위해 검증된 유량을 이용한 conductance 값을 제시하여, 기 언급한 두 가지 배기 속도 측정 방법의 연속성을 유지하기 위한 실험적인 방법론을 제기하고자 한다.

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

  • Lee, Hyoung Jun;Yim, Yong-Hyeon
    • Mass Spectrometry Letters
    • /
    • 제10권4호
    • /
    • pp.103-107
    • /
    • 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
    • /
    • 제44권1호
    • /
    • pp.105-114
    • /
    • 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
    • /
    • 제9권3호
    • /
    • pp.77-80
    • /
    • 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.

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

  • 서승희;이신영
    • 복식
    • /
    • 제65권1호
    • /
    • pp.46-60
    • /
    • 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.

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

  • 우진춘;임흥빈;문대원;이광우;김효진
    • 분석과학
    • /
    • 제5권2호
    • /
    • pp.169-176
    • /
    • 1992
  • 금속시료의 미량원소를 분석하기 위하여 jet형과 글로우방전 이온원을 제작하여 질량 분석기와 연결시킨 후 상대이온세기와 검출한계를 측정하였다. Jet형 이온원으로 구리시료의 시료 손실속도를 측정하였을 때 가스흐름속도가 0.01L/min이었을 때 0.23 mg/min이고 가스흐름이 없을 때는 0.11 mg/min이었다. 그러나 구리의 이온세기를 측정하였을 때는 두 이온원에서 큰 차이가 없었다. 여섯 개의 동합금시료의 검정곡선으로부터 구한 각 원소의 상대이온세기는 철의 0.57부터 크롬의 3.5 범위였다. Jet형 이온원으로 4mA, 1000V 방전시 순수 구리시료의 각 원소에 대한 검출한계는 0.9 ppm에서 2 ppm 수준으로 나타났다.

  • PDF

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
    • 한국진공학회:학술대회논문집
    • /
    • 한국진공학회 2012년도 제42회 동계 정기 학술대회 초록집
    • /
    • pp.275-275
    • /
    • 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.

  • PDF