• Title/Summary/Keyword: method detection limit

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Assay of Midazolam in Human Plasma by Gas-Liquid Chromatography with Nitrogen-Phosphorus Detection

  • 신호상;홍춘표;Yun-Suk Oh-Shin;강보경;이경옥;이규범
    • Bulletin of the Korean Chemical Society
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    • v.19 no.5
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    • pp.524-526
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    • 1998
  • A sensitive and specific method is described for the determination of midazolam in human plasma. The drug was extracted from 1 mL of carbonate buffered plasma (pH 9.6) with 8 mL of diethyl ether. Famprofazone was used as internal standard. The organic phase was evaporated to dryness. The residue was dissolved in methanol for the direct analysis by gas chromatograph-nitrogen phosphorus detector system. In the concentration range of 1-5000 ng/mL, the calibration curve was linear. The coefficients of variation from the precision test were <6% at the range of the concentration of 0.10-2.00 μg/mL and the detection limit for midazolam in 1 mL of plasma was o.5 ng. This assay is more sensitive, selective, simple and rapid than earlier methods. Plasma midazolam concentrations were determined by this method after administration of midazolam.

Semi-Automatic Hydride Generation and Atomic Absorption Determination of Bismuth with in situ Concentration in a Graphite Furnace

  • Yong-Keun Lee;Dong Soo Lee;Byung Mok Yoon;Hoon Hwang
    • Bulletin of the Korean Chemical Society
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    • v.12 no.3
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    • pp.290-295
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    • 1991
  • A semi-automatic method for the determination of dissolved bismuth at parts per trillion levels is described. The method involves bismuthine generation, in situ collection of bismuthine in a graphite furnace, and atomic absorption detection. In order to facilitate semi-automation of bismuthine generation and separation from aqueous solution, Gore-tex microporous PTEE membrane is used. The absolute detection limit, taken as three times the standard deviation of the instrument noise is 2 pg. The precisions are 3.1% for 100 pg and 1.9% for 1 ng of bismuth, respectively. As many as 90 measurements can be made in an hour.

Application of Bimodal Histogram Method to Oil Spill Detection from a Satellite Synthetic Aperture Radar Image

  • Kim, Tae-Sung;Park, Kyung-Ae;Lee, Min-Sun;Park, Jae-Jin;Hong, Sungwook;Kim, Kum-Lan;Chang, Eunmi
    • Korean Journal of Remote Sensing
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    • v.29 no.6
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    • pp.645-655
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    • 2013
  • As one of segmentation techniques for Synthetic Aperture Radar (SAR) image with oil spill, we applied a bimodal histogram method to discriminate oil pixels from non-oil pixels. The threshold of each moving window was objectively determined using the two peaks in the histogram distribution of backscattering coefficients from ENVISAT ASAR image. To reduce the effect of wind speed on oil spill detection, we selected ASAR image which satisfied a limit of wind speeds for successful detection. Overall, a commonly used adaptive threshold method has been applied with a subjectively-determined single threshold. In contrast, the bimodal histogram method utilized herein produces a variety of thresholds objectively for each moving window by considering the characteristics of statistical distribution of backscattering coefficients. Comparison between the two methods revealed that the bimodal histogram method exhibited no significant difference in terms of performance when compared to the adaptive threshold method, except for around the edges of dark oil spots. Thus, we anticipate that the objective method based on the bimodality of oil slicks may also be applicable to the detection of oil spills from other SAR imagery.

Validation of ICP-MS method for trace level analysis of Pb in plasma (혈장 중 극미량 납 분석을 위한 ICP-MS 분석법 검증)

  • Lee, Sung-Bae;Kim, Yong-Soon;Lee, Yong-Hoon;Ahn, Byung-Joon;Kim, Nam-Soo;Lee, Byung-Kook;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.28 no.5
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    • pp.309-316
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    • 2015
  • The analytical method of lead in plasma by ICP-MS was validated after securing environment within class 1,000 classification. We tested specificity and accuracy of within-run and between-run. According to measurement of the amount of suspended particulates in a clean room, 0.3~62 particles were detected in 0.3 µm size while 0.0~28.3 particles were observed in 0.5 µm size. Total suspended particulates met required environment with up to 90.3 particles. The MDL (Method detection limit) of the sample which has been fabricated using fetal bovine serum (FBS) blank was 1.77 ng/L, and LOQ (Limit of quantification) was 5.55 ng/L. The slope, intercept and correlation coefficient of the calibration curve were y=1.09×10−3x+4.88×10−2 and r=0.9999, which showed good correlation. The specificity, within-run and between-run accuracy satisfied the standard at more than 50 ng/L. The average lead concentration in plasma of the general people, current workers and retired workers was 55.4 ng/L, 440 ng/L, and 132 ng/L.

Nanometrology and its perspectives in environmental research

  • Kim, Hyun-A;Seo, Jung-Kwan;Kim, Taksoo;Lee, Byung-Tae
    • Environmental Analysis Health and Toxicology
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    • v.29
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    • pp.16.1-16.9
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    • 2014
  • Objectives Rapid increase in engineered nanoparticles (ENPs) in many goods has raised significant concern about their environmental safety. Proper methodologies are therefore needed to conduct toxicity and exposure assessment of nanoparticles in the environment. This study reviews several analytical techniques for nanoparticles and summarizes their principles, advantages and disadvantages, reviews the state of the art, and offers the perspectives of nanometrology in relation to ENP studies. Methods Nanometrology is divided into five techniques with regard to the instrumental principle: microscopy, light scattering, spectroscopy, separation, and single particle inductively coupled plasma-mass spectrometry. Results Each analytical method has its own drawbacks, such as detection limit, ability to quantify or qualify ENPs, and matrix effects. More than two different analytical methods should be used to better characterize ENPs. Conclusions In characterizing ENPs, the researchers should understand the nanometrology and its demerits, as well as its merits, to properly interpret their experimental results. Challenges lie in the nanometrology and pretreatment of ENPs from various matrices; in the extraction without dissolution or aggregation, and concentration of ENPs to satisfy the instrumental detection limit.

Automated On-Line Digestion System for the Determination of Total Phosphorus (총 인 분석을 위한 자동 전처리 시스템)

  • 정형근;조영일;김범식;박주형
    • Journal of Environmental Science International
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    • v.10 no.1
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    • pp.13-19
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    • 2001
  • An on-line digestion system based on the flow injection analysis technique was presented for the determination of total phosphorus. The system converts condensed and organic phosphoruses into orthophosphate that can be analyzed spectrophotometically. The reaction between orthophosphate and ammonium molybdate in a strong acid medium forms the yellow complex of phosphomolybdate which is next reduced to a molybdic blue complex by stannous chloride. The quantitation of orthophosphate is based on the absorbance of the molybdic blue. To determine total phosphorus, the digestion system was installed between the sample injector and the reaction coil with the added lines of digestion solution(potassium persulfate+sulfuric acid) and the $H_2O$ carrier. The system has shown that the digestion efficiencies were greater than 95% for the typical condensed and organic phosphoruses. When tripolyphosphate standards were used, the calibration data showed that the linear dynamic range extended to a concentration of 1.5ppm with the detection limit of 25ppb total phosphorus. The typical relative standard deviation was less than 2%. The proposed system was successfully applied to lake water, wastewater, and streamwater. The analytical variables such as digestion efficiency, analysis time, and reproducibility were evaluated and compared with the manual digestion method.

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Development of an Enzyme-Linked Immunosorbent Assay for the Organophosphorus Fungicide Tolclofos-methyl

  • Park, Kyung-Yi;Park, Won-Chul;Kim, Yoo-Jung;Lee, Yong-Tae
    • Bulletin of the Korean Chemical Society
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    • v.24 no.3
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    • pp.334-338
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    • 2003
  • A simple synthetic method for haptens of organophosphorus (OP) pesticides with a spacer arm (aminocarboxylic acid) attached at the pesticide thiophosphate group was developed and was applied to the synthesis of haptens for the OP fungicide tolclofos-methyl. Using the haptens, a selective enzyme-linked immunosorbent assay (ELISA) for tolclofos-methyl was developed. One of the haptens was coupled to BSA to use as an immunogen. Rabbits were immunized with this conjugate to obtain polyclonal antibodies to tolclofos-methyl. The antisera were screened against another hapten coupled to ovalbumin (OVA). Using the serum with highest specificity, an antigen-coated ELISA was developed, which showed an $IC_{50}$ of 160 ng/mL with the detection limit of 20 ng/mL. The antibodies showed negligible cross-reactivity with other OP pesticides. An antibody-coated ELISA was also developed, which showed an $IC_{50}$ of 410 ng/mL with a detection limit of 130 ng/mL.

Analysis of Volatile Organic Compounds in Water by Modified Injection Mode for Purge & Trap-GC/MS Method (Purge & Trap-GC/MS 분석법의 주입방식 개선에 의한 물 중의 휘발성 유기물 분석)

  • Jeon, Chi Wan;Lee, Sang Hak;Eum, Chul Hun
    • Journal of the Korean Chemical Society
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    • v.39 no.8
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    • pp.635-642
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    • 1995
  • Improved sample introduction system has been investigated for the determination of volatile organic compounds in water using a purge & trap preconcentration apparatus and a capillary gas chromatography/mass spectrometry. The present limitations associated with the moisture control module and cryorefocusing system suggested by EPA were discussed. To solve the problems such as improper separation of peaks due to the adsorption of water and contamination of purge & trap system, a more efficient connection system between the purge & trap apparatus and the gas chromatograph was introduced and the optimum operational conditions were suggested. A carbopack B/carboxen 1000 and 1001 trap was used for the purge & trap procedure and a custom made crosslinked dimethyldiphenylpolysiloxane capillary column was used for the separation of compounds. Accuracy and precision of the method suggested in this report were examined and the method detection limit of each compound was proposed for the simultaneous determination of 54 volatile organic compounds in water.

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Simultaneous Analysis of Conazole Fungicides in Garlic by Q-TOF Mass Spectrometer Coupled with a Modified QuEChERS Method

  • Bong, Min-Sun;Yang, Si-Young;Lee, Seung-Ho;Seo, Jung-Mi;Kim, In-Seon
    • Korean Journal of Environmental Agriculture
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    • v.30 no.3
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    • pp.323-329
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    • 2011
  • BACKGROUND: The conazoles, difenoconazole, diniconazole, hexaconazole, penconazole and tetraconazole are a large class of synthetic fungicides used extensively for foliage and seed treatments in agricultural crops. The extensive use of conazoles has brought concerns on the potentiality of environmental contamination and toxicity. Thus studies on the development of methods for monitoring the conazoles are required. METHODS AND RESULTS: A modified quick, easy, effective, rugged and safe (QuEChERS) method was involved in sample preparation. Quadrapole time of flight mass spectrometer (Q-TOF MS) in electron spray ionization (ESI) mode was employed to determine conazoles in garlic samples. The limit of detection (LOD) and limit of quantification (LOQ) of conazoles by Q-TOF-MS ranged from 0.001 to 0.002 mg/L and 0.002 to 0.005 mg/L, respectively. Q-TOF-MS analysis exhibited less than 2.6 ppm error of accurate mass measurements for the detection of conazoles spiked at 0.05 mg/L in garlic matrix. Recovery values of conazoles fortified in garlic samples at 0.02, 0.05 and 0.1 mg/L were between 79.2 and 106.2% with a maximum 11.8% of standard deviation. No detectable conazoles were found in the domestic market samples by using the Q-TOF-MS method. CONCLUSION(s): High degree of confirmation for conazoles by accurate mass measurements demonstrated that Q-TOF-MS analysis combined with a QuEChERS method may be applicable to simultaneous determination of conazoles in garlic samples.

Rapid and Sensitive Detection of Lettuce Necrotic Yellows Virus and Cucumber Mosaic Virus Infecting Lettuce (Lactuca sativa L.) by Reverse Transcription Loop-Mediated Isothermal Amplification

  • Zhang, Yubao;Xie, Zhongkui;Fletcher, John D;Wang, Yajun;Wang, Ruoyu;Guo, Zhihong;He, Yuhui
    • The Plant Pathology Journal
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    • v.36 no.1
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    • pp.76-86
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    • 2020
  • Cucumber mosaic virus (CMV) is damaging to the growth and quality of lettuce crops in Lanzhou, China. Recently, however, for the first time an isolate of lettuce necrotic yellows virus (LNYV) has been detected in lettuce crops in China, and there is concern that this virus may also pose a threat to lettuce production in China. Consequently, there is a need to develop a rapid and efficient detection method to accurately identify LNYV and CMV infections and help limit their spread. Reverse transcription loop-mediated isothermal amplification (RT-LAMP) assays were developed to detect the nucleoprotein (N) and coat protein (CP) genes of LNYV and CMV, respectively. RT-LAMP amplification products were visually assessed in reaction tubes separately using green fluorescence and gel electrophoresis. The assays successfully detected both viruses in infected plants without cross reactivity recorded from either CMV or LNYV or four other related plant viruses. Optimum LAMP reactions were conducted in betaine-free media with 6 mM Mg2+ at 65℃ for LNYV and 60℃ for 60 min for CMV, respectively. The detection limit was 3.5 pg/ml and 20 fg/ml using RT-LAMP for LNYV and CMV plasmids, respectively. Detection sensitivity for both RT-LAMP assays was greater by a factor of 100 compared to the conventional reverse transcription polymerase chain reaction assays. This rapid, specific, and sensitive technique should be more widely applied due to its low cost and minimal equipment requirements.