• Title/Summary/Keyword: Detection Rate/Time

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High Performance Liquid Chromatographic Analysis of a New Proton Pump Inhibitor KR60436 and Its Active Metabolite O-Demethyl-KR60436 in Rat Plasma Samples Using Column-Switching

  • Lee, Hyun-Mee;Lee, Hee-Yong;Choi, Joong-Kwon;Lee, Hye-Suk
    • Archives of Pharmacal Research
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    • v.24 no.3
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    • pp.207-210
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    • 2001
  • A fully automated high performance liquid chromatography with column-switching was developed for the simultaneous determination of KR60436, a new reversible proton pump inhibitor, and its active metabolite O-Demethyl-KR60436 from rat plasma samples. Plasma sample (50$\mu$l) was directly introduced onto a Capcell Pak MF Ph-1 column ($10{\times}4$ mm I.D.) where primary separation was occurred to remove proteins and concentrate target Substances Using acetonitrile-Potassium Phosphate (PH 7, 0.1 M) (2 : 8, v/v). The drug molecules eluted from MF Ph-1 column were focused in an intermediate column ($10{\times}2$ I.D.) by the valve switching step. The substances enriched in intermediate column were eluted and separated on a Vydac 218MR53 column ($250{\times}3.2$ I.D.) using acetonitrilepotassium phosphate (pH 7, 0.02 M) (47:53, v/v) at a flow rate of 0.5 ml/min when the valve status was switched back to A position. The method showed excellent sensitivity (detection limit of 2 ng/ml) with small volume of samples ($50{\mu}$l), good precision and accuracy, and speed (total analysis time 24 min) without any loss in chromatographic efficiency. The response was linear ($r^2{\geq}0.797$) over the concentration range of 5-500 ng/ml.

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High Performance Liquid Chromatographic Assay of a New Fluoroquinolone, LB20304, in the Plasma of Rats and Dogs

  • Seo, Mi-Kyeong;Jeong, Yi-Na;Kim, Hoon-Joo;Kim, In-Chull;Lee, Yong-Hee
    • Archives of Pharmacal Research
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    • v.19 no.6
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    • pp.554-558
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    • 1996
  • High-performance liquid chromatographic method was developed for the determination or LB 20304 (compound 1) in the plasma of rats and dogs. The analyte was deproteinized with 1 volume of methanol and 1/2 volume of 10% zinc sulfate, and the supernatant was injected onto a reversed-phase HPLC column. The mobile phase was a mixture of 24 parts of acetonitrile and 76 parts of 0.1% trifluoroacetic acid. The flow rate was 1 ml/min, and the effluent was monitored by fluorescence detector at an excitation wavelength of 337 nm and an emission wavelength of 460 nm. The retention time of compound 1 was 6.3 min. The assay of compound 1 was linear over the concentration range of 0.2-100.mu.g/ml in the plasma of rats and dogs. The lower limit of quantification was 0.2.mu.g/ml using 100.mu.l of plasma with a 97-99% accuracy and a 12-14% precision. In the 0.5, 5, and 50.mu.g/ml quality control samples, the intra- and inter-day accuracy were 88-95% and 88-97%, whereas intra- and interday precision were 0.5-6.6% and 0.2-9.3%, respectively, in the plasma of rats and dogs. The recoveries were 68-71% independent of concentration and species in the plasma. No interferences from endogenous substances were observed. Taken together, the above HPLC assay method by deproteinization and fluorescence detection was suitable for the determination of compound 1 in the preclinical pharmacokinetics.

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Analysis of Related Compounds from Commercial Atenolol Raw Materials and Preparations by High-Performance Liquid Chromatography (HPLC를 이용한 시판 아테놀롤 원료 및 제품 중 유연물질의 분석)

  • Dong, Nguyen Thanh;Kang, Ji-Youn;Jung, Young-Hee;Lim, Eun-Hee;Hwang, Gwi-Seo;Kang, Chan-Soon;Kim, Eun-Jung;Kang, Jong-Seong
    • Journal of Pharmaceutical Investigation
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    • v.34 no.6
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    • pp.453-457
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    • 2004
  • Atenolol and related compounds found in raw materials and commercial products were analyzed by reversed-phase high-performance liquid chromatography. A mixed solution of phosphate buffer (3.4 g/l, pH 3.0), tetrahydrofurane and methanol (800:20:180, v/v/v) including sodium octanesulfonate (1 g/l) and tetrabutylammonium-hydrogensulfate (0.4 g/l) was used as mobile phase at the flow rate of 0.25 ml/min. Detection was carried out at UV 226 nm. Atenolol related compounds, such as bis ether, tertiary amine and blocker acid were identified by comparing the retention time of the standard. The within-day and between-day precisions of the separated compounds were less than 1.2% and 3.4%, respectively. The contents of related compounds of the tested samples were under the limit prescribed in the European Pharmacopoeia. The pattern of the related compounds showed that atenolol raw materials and products could be classified in three different groups, indicating that the materials originated from different source or treated in different way.

Development of Luciferase Reporter Gene-based Cell Bioassay for the Aromatic Hydrocarbon Receptor Agonists

  • Kim, Sun-Young;Choi, Eun-Jung;Yang, Jae-Ho
    • The Korean Journal of Physiology and Pharmacology
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    • v.10 no.6
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    • pp.349-354
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    • 2006
  • The aromatic hydrocarbon receptor (AhR) is a ligand-activated transcription factor that mediates many of the biological and toxicological effects of 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD, dioxin) and related chemicals. The application of recombinant reporter plasmid such as the firefly luciferase gene has proven to be a very effective method to detect these chemicals. The bioassay system, CALUX, is sensitive in directly detecting AhR-agonists from a variety of environmental and biologic materials. However, responses of the AhR-dependent bioassays are dependent on the cell types used. Thus, we developed a sensitive bioassay using the recombinant mouse hepatoma cell (Hepa1c1c7) for the determination of dioxins. The recombinant cell line was stably transfected with firefly luciferase reporter gene (pGudLuc1.1). The transfected cells showed the highest induction of luciferase activity at 4.5 hr and a decrease beyond this time point. The system showed the highest sensitivity of detection ever reported. Upon TCDD exposure cells showed 2 fold increase at 10 pM and 7 fold increase at 100 pM, respectively. The passage number after the transfection played an important role in the sensitivity. The increase of passage number tended to increase the sensitivity of the cells up to 15. The media without phenol red showed a higher induction rate than with phenol red, suggesting the preferable use of phenol red-free media for the bioassay. Since each of the assays has unique characteristics that make them suitable for some screening applications and not others, development of sensitive bioanalytical methods based on a variety of cellular systems in a key to the successful determination of dioxins. The bioassay system developed in this study will contribute to further development of successful screening the AhR agonists among the environmental mixture. In addition, the rapid and sensitive nature of this cellular system can be applied as a valuable tool to screen the dioxin-like moieties among the prodrugs at the initial stage, thereby expediting the new drug discovery.

A Study on the Detection Technique of DDoS Attacks on the Software-Defined Networks (소프트웨어-정의 네트워크에서 분산형 서비스 거부(DDoS) 공격에 대한 탐지 기술 연구)

  • Kim, SoonGohn
    • The Journal of Korea Institute of Information, Electronics, and Communication Technology
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    • v.13 no.1
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    • pp.81-87
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    • 2020
  • Recently, the network configuration is being rapidly changed to enable easy and free network service configuration based on SDN/NFV. Despite the many advantages and applications of SDN, many security issues such as Distributed Denial of Service (DDoS) attacks are being constantly raised as research issues. In particular, the effectiveness of DDoS attacks is much faster, SDN is causing more and more fatal damage. In this paper, we propose an entropy-based technique to detect and mitigate DDoS attacks in SDN, and prove it through experiments. The proposed scheme is designed to mitigate these attacks by detecting DDoS attacks on single and multiple victim systems and using time - specific techniques. We confirmed the effectiveness of the proposed scheme to reduce packet loss rate by 20(19.86)% while generating 3.21% network congestion.

Soft Error Detection for VLIW Architectures with a Variable Length Execution Set (Variable Length Execution Set을 지원하는 VLIW 아키텍처를 위한 소프트 에러 검출 기법)

  • Lee, Jongwon;Cho, Doosan;Paek, Yunheung
    • KIPS Transactions on Computer and Communication Systems
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    • v.2 no.3
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    • pp.111-116
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    • 2013
  • With technology scaling, soft error rate has greatly increased in embedded systems. Due to high performance and low power consumption, VLIW (Very Long Instruction Word) architectures have been widely used in embedded systems and thus many researches have been studied to improve the reliability of a system by duplicating instructions in VLIW architectures. However, existing studies have ignored the feature, called VLES (Variable Length Execution Set), which is adopted in most modern VLIW architectures to reduce code size. In this paper, we propose how to support instruction duplication in VLIW architecture with VLES. Our experimental results demonstrate that a VLIW architecture with VLES shows 64% code size decrement on average at the cost of about 4% additional cell area as compared to the case of a VLIW architecture without VLES when instruction duplication is applied to both architectures. Also, it is shown that the case with VLES does not cause extra execution time compared to the case without VLES.

유도 결합 플라즈마를 이용한 스퍼터-승화 증착 시스템의 공정 분석

  • Yu, Yeong-Gun;Choe, Ji-Seong;Ju, Jeong-Hun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.08a
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    • pp.186-186
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    • 2013
  • 종래의 흑연 위주 연료전지 분리판 개발되어 최근 고분자 전해질 막 연료전지가 높은 전력, 낮은 배기 가스 배출, 낮은 작동 온도로 자동차 산업에서 상당한 주목을 받고 있다. 요구사항은 높은 전기 전도도, 높은 내식성, 낮은 가스 투과성, 낮은 무게, 쉬운 가공, 낮은 제조비용이다. Thin film Cr 장비로 저항가열 furnace, sputter 등이 사용된다. 연료전지 분리판의 고전도도, 내부식성 보호막의 고속 증착을 위한 새로운 증착원으로 스퍼터 - 승화형 소스의 가능성을 유도 결합 플라즈마에 금속 봉을 직류 바이어스 함으로써 시도하였다. 유도 결합 플라즈마를 이용하여 승화증착 시스템을 사용하여 OES (SQ-2000)와 QMS (CPM-300)를 사용하여 $N_2$ flow에 따른 유도 결합 플라즈마를 이용한 스퍼터-승화증착 시스템을 사용 하여도 균일한 공정을 하는 것을 확인 하였다. 5 mTorr의 Ar 유도 결합 플라즈마를 2.4 MHz, 500 W로 유지하면서 직류 바이어스 전력을 30 W (900 V, 0.02 A) 인가하고, $N_2$의 유량을 0.5, 1.0, 1.5 SCCM로 변화를 주어 특성을 분석하였다. MID (Multiple Ion Detection) mode에서 유도결합 플라즈마를 이용한 스퍼터-승화 증착 장비를 사용하여 CrN thin flim 성장시켰고, deposition rate은 44.8 nm/min으로 얻을 수 있었다. 또한 $N_2$의 유량이 증가할 수록 bias voltage가 증가하는 것을 확인 할 수 있었다. OES time acquisition을 이용한 공정 분석에서는 $N_2$ 유량을 off 하였을 때 Ar, Cr의 중성 intensity peak이 상승하였고, 시간 경과에 따라 sublimation에 의한 영향이 없는 것을 확인 할 수가 있었다. XRD data에서는 질소 유량이 증가함에 따라 $Cr_2N$이 감소하고, CrN이 증가하는 것을 확인할 수가 있었다. 결정배향성과 Morphology는 다결정 재료의 경도에 영향을 주는 인자이다. CrN 결정 구조의 경우는 (200)면이 경도가 제일 높은데 (200)면에서 성장한 것을 확인 할 수 있었다. 잔류가스 분석 결과로는 일정한 Ar의 유량을 흘렸을 때 $N_2$의 변화량이 비례적인 경향이 보이는 것을 확인 할수 있었다. 또한 $N_2$가 흐르면서도 유도 결합 플라즈마를 이용한 스퍼터-승화 증착 시스템을 사용하면 일정한 공정을 하는 것을 확인 할 수 있었다. 질소의 분압이 유량에 따라서 $3.0{\times}10^{-10}$ Torr에서 $1.65{\times}10^{-9} $Torr까지 일정한 비율로 증가한다. 즉, 이 시스템으로 양산장비 설계를 하여도 가능 하다는 것을 말해준다.

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A study on the development of Gas-Vent Automatic Exchange Machine with Vision System (영상정보를 이용한 가스벤트자동교환 장치)

  • Kwon, Jang-Woo;Hong, Jun-Eui;Yoon, Dong-Eop;Kil, Gyung-Suk;Lee, Dong-Hoon;Lee, Dong-Hoon
    • Journal of the Korea Institute of Information and Communication Engineering
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    • v.11 no.6
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    • pp.1141-1149
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    • 2007
  • This paper describes two major techniques; image processing and gas vent insert and rejection control, for efficient gas vent exchange and holes detecting on the shoes mold. The key idea is to detect holes on the mold to select which holes to insert and to reject automatically guide center of hole's position. This allows us to save labor time while minimizing defective rate of PU shoes mold forming and production costs for gas vent exchange such as insertion and rejection.. Our experimental results have demonstrated that the hole's detection and gasvent exchange mechanism are more efficient and provide accurate mechanism to mitigate risks of vent injection/rejection failures.

Reasonability of Logistic Curve on S/W (로지스틱 곡선을 이용한 타당성)

  • Kim, Sun-Il;Che, Gyu-Shik;Jo, In-June
    • Journal of the Korea Institute of Information and Communication Engineering
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    • v.12 no.1
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    • pp.1-9
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    • 2008
  • The Logistic cone is studied as a most desirable for the software testing effort. Assuming that the error detection rate to the amount of testing effort spent during the testing phase is proportional to the current error content, a software-reliability growth model is formulated by a nonhomogeneous Poisson process. Using this model the method of data analysis for software reliability measurement is developed. After defining a software reliability, This paper discusses the relations between testing time and reliability and between duration following failure fixing and reliability are studied SRGM in several literatures has used the exponential curve, Railleigh curve or Weibull cure as an amount of testing effort during software testing phase. However, it might not be appropriate to represent the consumption curve for testing effort by one of already proposed curves in some software development environments. Therefore, this paper shows that a logistic testing- effort function can be adequately expressed as a software development/testing effort curve and that it gives a good predictive capability based on real failure data.

Method development and validation of spectrophotometric and RP-HPLC methods for simultaneous estimation of spironolactone and furosemide in bulk and combined tablet dosage forms

  • Chavan, Rohankumar R.;Bhinge, Somnath D.;Bhutkar, Mangesh A.;Randive, Dheeraj S.;Salunkhe, Vijay R.
    • Analytical Science and Technology
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    • v.34 no.5
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    • pp.212-224
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    • 2021
  • The intent of the present work was to develop a simple, sensitive, accurate, precise, rapid and economical UV- spectrophotometric and reverse phase high pressure liquid chromatographic method for the simultaneous estimation of Spironolactone and Furosemide in bulk and combined tablet dosage forms. UV-Spectrophotometry was carried out by simultaneous equation method using 0.02 M potassium dihydrogen phosphate buffer pH 3.5: Acetonitrile (50:50) v/v as a solvent. The linearity range was 2-14 ㎍ mL-1 for Spironolactone and Furosemide with a correlation coefficient > 0.99. The chromatographic separation was achieved on 250 mm × 4.6 mm, hypersil BDS C18 column with particle size 5 ㎛, by using an isocratic mixture of 0.02 M potassium dihydrogen phosphate buffer pH 3.5: Acetonitrile: tert butyl methyl ether (49:50:1) v/v/v as a solvent at a flow rate of 1 mL min-1 and UV detection was carried out at 254 nm. The retention time were observed to be 3.666 and 6.661 minutes for Furosemide and Spironolactone respectively. The two developed methods were validated according to the ICH guidelines for accuracy, precision, linearity, LOD, LOQ and were found to be within the limits. It can be concluded that these two methods could be successfully used for the simultaneous estimation of Spironolactone and Furosemide in bulk and combined tablet dosage forms.