• 제목/요약/키워드: SRM analysis

검색결과 389건 처리시간 0.024초

Simultaneous Liquid Chromatography Tandem Mass Spectrometric Determination of 35 Prohibited Substances in Equine Plasma for Doping Control

  • Kwak, Young Beom;Yu, Jundong;Yoo, Hye Hyun
    • Mass Spectrometry Letters
    • /
    • 제13권4호
    • /
    • pp.158-165
    • /
    • 2022
  • Many therapeutic class drugs such as beta-blocker, corticosteroids, NSAIDs, etc are prohibited substances in the horse racing industry. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology makes it possible to isolate drugs from interference, enables various drug analyses in complex biological samples due to its sensitive sensitivity, and has been successfully applied to doping control. In this paper, we describe a rapid and sensitive method based on solid-phase extraction (SPE) using solid phase cartridge and LC-MS/MS to screen for different class's 35 drug targets in equine plasma. Plasma samples were pretreated by SPE with the NEXUS cartridge consisted non-polar carbon resin and minimum buffer solvent. Chromatographic separation of the analytes was performed on ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 ㎛). The elution gradient was conducted with 5 mM ammonium formate (pH 3.0) in distilled water and 0.1% formic acid in acetonitrile at a flow rate of 0.25 mL/min. The selected reaction monitoring (SRM) mode was used for drug screening with multiple transitions in the positive ionization mode. The specificity, limit of detection, recovery, and stability was evaluated for validation. The method was found to be sensitive and reproducible for drug screening. The method was applied to plasma sample analysis for the proficiency test from the Association of Racing Chemist.

Securing the Information using Improved Modular Encryption Standard in Cloud Computing Environment

  • A. Syed Ismail;D. Pradeep;J. Ashok
    • KSII Transactions on Internet and Information Systems (TIIS)
    • /
    • 제17권10호
    • /
    • pp.2822-2843
    • /
    • 2023
  • All aspects of human life have become increasingly dependent on data in the last few decades. The development of several applications causes an enormous issue on data volume in current years. This information must be safeguarded and kept in safe locations. Massive volumes of data have been safely stored with cloud computing. This technology is developing rapidly because of its immense potentials. As a result, protecting data and the procedures to be handled from attackers has become a top priority in order to maintain its integrity, confidentiality, protection, and privacy. Therefore, it is important to implement the appropriate security measures in order to prevent security breaches and vulnerabilities. An improved version of Modular Encryption Standard (IMES) based on layered modelling of safety mechanisms is the major focus of this paper's research work. Key generation in IMES is done using a logistic map, which estimates the values of the input data. The performance analysis demonstrates that proposed work performs better than commonly used algorithms against cloud security in terms of higher performance and additional qualitative security features. The results prove that the proposed IMES has 0.015s of processing time, where existing models have 0.017s to 0.022s of processing time for a file size of 256KB.

중성자 방사화분석법과 Gent SFU 샘플러를 이용한 도시의 농촌지역의 대기분지($PM_{10}$)관측 연구 (Study on Airborne Particulate Matter ($PM_{10}$) Monitoring in Urban and Rural Area by Using Gent SFU Sampler and Instrumental Neutron Activation Analysis)

  • 정용삼;문종화;김선하;박광원;강상훈
    • 한국대기환경학회지
    • /
    • 제16권5호
    • /
    • pp.453-467
    • /
    • 2000
  • The aim of this research is to collect and characterize fine particles (FPM:$\leq$2.5${\mu}{\textrm}{m}$) and coarse particles (CPM: 2.5~10${\mu}{\textrm}{m}$) using a low volume air sampler provided by the IAEA, at urban (Taejon) and rural area(Wonju) for a period of about two years(April 1996 to May 1998) and to promote a use of nuclear analytical techniques for air pollution studies. For the collection of airborne particulate matter (PM(sub)10), the Gent stacked filter unit sampler and polycarbonate membrane filters were employed. The concentration of trace elements in collected APM samples were determined byu instrumental Neutron Activation Analysis. For validation of the analytical data, internal quality control were implemented by using both the comparison of the analytical results of standard reference materials(NIST SRM 1648) and interlaboratory comparison for proficiency test (NAT-3). The standard uncertainty was less than 15% and Z-score of two samples were within $\pm$1. The monitoring of (PM(sub)10) mass concentration and elemental concentrations were carried out weekly. The average mass concentration of (PM(sub)10) in urban and rural areas were 59.2$\pm$36.5$\mu\textrm{g}$/㎥ and 41.4$\pm$23.7$\mu\textrm{g}$/㎥, respectively. To investigate the emission source, the enrichment factors were calculated for the fine and coarse particle fractions at two sites, respectively and these values were classified for anthropogenic and soil origin elements.

  • PDF

유도결합 플라스마-질량분석법에 의한 혈청, 생우유 및 사료첨가제중 요오드의 분석에 관한 연구 (A Study on Determination of Iodine in Serum, Fresh Milk, and Feed Additive by Inductively Coupled Plasma-Mass Spectrometry)

  • 이원;박경수;김선태;김영만
    • 분석과학
    • /
    • 제12권6호
    • /
    • pp.528-533
    • /
    • 1999
  • 유도결합 플라스마-질랑분석법을 이용하여 혈청, 생우유 및 사료첨가제 중 요오드를 정량하였다. 시료를 매트릭스 변형제인 $NH_4OH$(0.5% v/v)+$CH_3OH$(5% v/v) 혼합용액으로 25배 묽힌 다음, m/z=127에서 이온세기를 측정하였다. 이 방법에 대한 요오드의 검정곡선은 $0-100{\mu}g/L$ 범위에서 상관계수($R^2$)가 0.99인 직선관계를 나타내었으며, 검출한계는 $0.084{\mu}g/L$이었다. 최적 분석 및 기기 조건에서 분유 표준시료를 분석한 결과 상대오차는 2.30-4.73% 범위이었다. 또한 혈청, 생우유, 동물의 사료 첨가제 등과 같은 실제시료를 분석한 결과 요오드의 함유량은 각각 $12.4-40.2{\mu}g/L$, < 0.01-3.11 mg/L,< $10^{-7}-2.60g/kg$ 범위이었다.

  • PDF

Ultra-fast Generic LC-MS/MS Method for High-Throughput Quantification in Drug Discovery

  • Kim, So-Hee;Yoo, Hye Hyun;Cha, Eun-Ju;Jeong, Eun Sook;Kim, Ho Jun;Kim, Dong Hyun;Lee, Jaeick
    • Mass Spectrometry Letters
    • /
    • 제4권3호
    • /
    • pp.47-50
    • /
    • 2013
  • An ultra-fast generic LC-MS/MS method was developed for high-throughput quantification of discovery pharmacokinetic (PK) samples and its reliability was verified. The method involves a simple protein precipitation for sample preparation and the analysis by ultra-fast generic LC-MS/MS with the ballistic gradient program and selected reaction monitoring (SRM) mode. Approximately 290 new chemical entities (NCEs) (over 10,000 samples) from 5 therapeutic programs were analyzed. The calibration curves showed good linearity in the concentration range of 1, 2 or 5 to 2000 ng/mL. No significant ion suppression was observed in the elution region of all the NCEs. When approximately 300 plasma samples were continuously analyzed, the peak area of internal standard was constant and reproducible. In the repeated analysis of samples, the plasma concentrations and the area under the curve (AUC) were consistent with the results from the first analysis. These results showed that the present ultra-fast generic LC-MS/MS method is reliable in terms of selectivity, sensitivity, and reproducibility and could be useful for high-throughput quantification and other bioanalysis in drug discovery.

중성자방사화분석법에 의한 국내 식품원재료의 무기질 분포 연구 (A Study on Mineral Distribution in Korean Foodstuffs by Neutron Activation Analysis)

  • 조승연;홍우정;이정연;강상훈;정용삼
    • 한국식품과학회지
    • /
    • 제34권3호
    • /
    • pp.390-395
    • /
    • 2002
  • 핵분석기술의 하나인 중성자방사화분석법을 이용하여 국내 주요식품 및 원재료 50종에 대한 주요 무기질 성분 중 Ca, K, Mg, Na 등의 다량원소들과 Se, Zn, Fe, Mn 등의 필수원소들의 분포를 확인하고자 하였다. 원소손실을 최소화하기 위해 동결건조의 과정을 거쳤으며, 균일한 매질분포를 위해 분쇄 후 체걸림을 통해 시료를 준비하였다. 분석법의 검증을 위해 미국 NIST사의 표준시료를 이용하였는데, 실제시료와 가장 유사한 시료를 선택하여 조사시간, 냉각시간, 계측시간 등의 분석조건을 일치시킴으로서 분석법에 대한 검증 및 정밀도와 정확도 측정에 이용하였다. 표준시료의 보증값에 대한 상대오차와 합성불확도는 대부분 10% 이내였으며, Z값도 2 이내로 측정값의 수용한계로 인정할 수 있었다. 분석결과 근육 수축 및 뼈 생성 등에 작용하는 Ca은 일반적으로 알려진 멸치나 치즈 외에 참깨와 김 등에 높은 농도를 나타냈으며 라면 등에는 검출되지 않았다. K와 Na는 해조류 및 동물성 식품에 주로 분포하였으며, 세포 내 주요 영양물질로 작용하는 Mg은 곡류 및 김 등에 높은 농도를 나타냈다. 또한 성장촉진 및 효소의 구성성분으로 알려진 Se은 어패류에, Fe, Zn 등 기타 원소들은 멸치 등 특정 식품에 다량 함유되어 있음을 확인할 수 있었다.

LC-MS/MS를 이용한 조제유류 중 비오틴 함량 분석법 연구 (Establishment of Biotin Analysis by LC-MS/MS Method in Infant Milk Formulas)

  • 신용운;이화정;함현숙;신성철;강윤정;황경미;권용관;서일원;오재명;구용의
    • 한국식품위생안전성학회지
    • /
    • 제31권5호
    • /
    • pp.327-334
    • /
    • 2016
  • 본 연구는 "축산물의 가공기준 및 성분규격"에 기준규격은 설정되어 있지 않으나, 국제 기준과의 조화를 위해 규격 신설 검토 대상 성분인 비오틴의 분석법을 마련하고자 수행하였다. 조제유류에 미량으로 함유된 비오틴함량 분석을 위해 선택성과 정밀성이 뛰어난 LC-MS/MS를 이용한 분석법을 확립하고 시중에 유통중인 제품을 대상으로 적용성을 검토하였다. 비오틴 표준품을 이용하여 LC-MS/MS를 이용한 기기분석조건을 확립하고, 식품의 기준 및 규격 분석법을 참고로 0.01 M 인산이수소칼륨(pH 4.8) 용액을 이용하여 시료중의 비오틴을 추출하여 분석하였다. 분석법 검증은 특이성, 직선성, 검출한계 및 정량한계, 정확성, 정밀성에 대해 수행되었다. 5~60 ng/mL의 농도범위에서 $R^2=0.999$ 이상의 우수한 직선성을 확인할 수 있었으며, LOD와 LOQ는 각각 0.10, 0.31 ng/mL 이었다. CRM (NIST SRM 1849a) 및 표준물질 첨가법을 이용하여 정확성을 검토하였으며, CRM에서 103%, 조제분유에서 101~104%, 조제우유에서 99~101%의 회수율을 확인할 수 있었다. 정밀성을 검토한 결과 시료 채취량에 따른 상대표준편차가 조제분유 0.4~0.9%, 조제우유1.4~1.6%로 확인하였으며, 실험일자에 따른 재현성은 조제분유에서 1.3%, 조제우유에서 1.2%로 확인하였다. 본 연구에서 확립된 분석법을 적용하여 조제분유 39건, 조제우유 3건, 성장기용조제분유 23건 등 국내 유통중인 조제유류 65건에 대해 적용성 검토를 실시한 결과 전체시료에서 분석이 용이하였으며, 모두 표시기준에 적합함을 확인하였다.

임상 간호사의 도덕성 발달과 윤리적 가치관에 대한 연구 (A Study of Moral Development and Ethical Values of the Nurse)

  • 김미정;김명희
    • 간호행정학회지
    • /
    • 제5권2호
    • /
    • pp.337-353
    • /
    • 1999
  • This study is to provide the basic sources to develop educational data that can establish ethical values with research on the interrelation between moral development and ethical values of nurses. The subjects of this study are the convenience sample from 111 nurses working in clinical settings from 5 general hospitals located in Pusan area. The questionnairs for this study are comprised two parts: Part 1 is SRM-SF(1995) guestionnaire, and translated by Kil, 1m Ju(1997): Part 2 is the guestion papers about the ethical values, and disigned by Jung, Hee Ja. The data were collected from June lth to 31th, 1997 and analyzed by S.A.S(Statistical Analysis System) Package for frequency, percent, and Pearson's correlation coefficient. The results of the study is as the followings: 1) According to the moral development. the nurses are in the levels of Stage3 or Transition3/4, which are generally focused on the personal relations or personality. Thus, nurses are considered to need to get the stage4 of education that helps them recognize a person as a member of society. a family as an unit of society, and human life as the values of human dignity. 2) According to the ethical values, nurses have the positive ethical values of respecting the right of the patients, providing information, keeping the secret, truth. and credit of patients. But they also experience some troubles by the patients to care and the clinical situation. Thus, to overcome the problems, nurses are considered to need to get the education that establishs the right ethical values. 3) The analysis result on the interrelation between moral development level and ethical values shows as r=0.28 and p=0.003. This indicates that the interrelation between them is low. In conclusion, it is considered that the moral development level is viewed broadly from a person and family to a society, and then it can affect to the ethical values positively.

  • PDF

한글 경추 통증 및 기능장애 측정 도구의 개발과 타당도 및 신뢰도 검사 (Cross-Cultural Adaptation of Korean Language Versions on Neck Pain and Disability Questionnaires and Their Psychometric Testing)

  • 이해정
    • Korean Journal of Acupuncture
    • /
    • 제24권2호
    • /
    • pp.99-112
    • /
    • 2007
  • Objectives : It was to translate three neck and spinal pain disability questionnaires - the Neck Disability Index (NDI), the Neck Pain and Disability Scale (NPDS), and the Functional Rating Index (FRI) - into Korean language, and evaluate the psychometric properties of Korean versions of questionnaires to achieve a good cross-cultural adaptation. Methods : Forty (23 males, 17 females) subjects aged from 15 to 64 years old, participated to examine test-retest reliability. One hundred and eighty (76 males, 104 females) subjects with a primary diagnosis of non-specific neck pain and 81 healthy volunteers were undertaken to examine internal consistemcy, discriminative validity and longitudinal construct validity. Versions of each questionnaire in idiomatic modern Korean were developed using a procedure proposed by Beaton et al. (2000). To assess reliability, the Intraclass Correlation Coefficient (ICC $_{(2,1)}$) was calculated. Internal consistency was evaluated by Cronbach's alpha. Discriminative validity was examined with independent-group t-tests. Responsiveness was tested by calculating the effect size and standardized response mean for each questionnaire and using Pearson' s r and the area under the receiver operating characteristic curve analysis. Results : Test-retest reliability ofthe translated versions of the three disability questionnaires was excellent (ICC $_{(2,1)$ = 0.86-0.90). High internal consistency was found in the three disability questionnaires (Cronbach's alpha ranged from ${\alpha}=0.88$ for the FRI to ${\alpha}=0.96$ for the NPDS and 0.82 for the Short Form McGill Pain Questionnaire(SFMPQ)). the VAS subscale of the SFMPQ was found to be the most responsive of the subscales (ES=1.44, SRM=1.37). The VAS was also the most responsive pain and disability index in internal responsiveness analysis, although disability indices showed marginally better responsiveness when compared with external standards. No floor or ceiling effects were observed. Conclusions : It is concluded that the questionnaires were successfully translated and exhibit acceptable measurement properties, and may suggest that they are suitable for use in clinical and research application.

  • PDF

Stability Index Based Voltage Collapse Prediction and Contingency Analysis

  • Subramani, C.;Dash, Subhransu Sekhar;Jagdeeshkumar, M.;Bhaskar, M. Arun
    • Journal of Electrical Engineering and Technology
    • /
    • 제4권4호
    • /
    • pp.438-442
    • /
    • 2009
  • Voltage instability is a phenomenon that could occur in power systems due to stressed conditions. The result would be an occurrence of voltage collapse leading to total blackout of the system. Therefore, voltage collapse prediction is an important part of power system planning and operation, and can help ensure that voltage collapse due to voltage instability is avoided. Line outages in power systems may also cause voltage collapse, thereby implying the contingency in the system. Contingency problems caused by line outages have been identified as one of the main causes of voltage instability in power systems. This paper presents a new technique for contingency ranking based on voltage stability conditions in power systems. A new line stability index was formulated and used to identify the critical line outages and sensitive lines in the system. Line outage contingency ranking was performed on several loading conditions in order to identify the effect of an increase in loading to critical line outages. Correlation studies on the results obtained from contingency ranking and voltage stability analysis were also conducted, and it was found that line outages in weak lines would cause voltage instability conditions in a system. Subsequently, using the results from the contingency ranking, weak areas in the system can be identified. The proposed contingency ranking technique was tested on the IEEE reliability test system.