• Title/Summary/Keyword: Detection limits

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Analysis of Ginsenosides by Thermospray LC/MS (열분무 LC/MS에 의한 인삼사포닌의 분석)

  • Park, Man-Ki;Park, Jeong-Hill;Hwang, Gwi-Seo;Lee, Mi-Young;Park, In-Jeong
    • Journal of Ginseng Research
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    • v.19 no.2
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    • pp.134-137
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    • 1995
  • Ginseng saponins were analyzed by thermospray (TSP) LCMS method using ODS column and with acetonitrile/ammonium acetate solution. Optimal condition for TSP Lchfs was found as follows: capillary temperature: 33$0^{\circ}C$ repelled voltage: 200 V, and concentration of ammonium acetate: 0. 05 M. Panaxadiol and panaxatriol type saponins showed characteristic fragment ions. The calibration curve of ginseng saponin showed good linearity with a correlation coefficient of 0.99. Detection limits using selected ion monitoring (SIM) technique were improved by 10~200 times compared to conventional HPLCnnr detection method.

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Simultaneous determination of low molecular weight amines and quaternary ammonium ions by IC/ESI-MS

  • Jung, Joo-Young;Park, Han-Seok;Kim, Kang-Jin
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.255-260
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    • 2007
  • A new method for the simultaneous determination of low molecular weight amines and quaternary ammonium ions based on the separation by IC with a suppressor and the detection by MS with ESI has been developed. The method has been applied to the analysis of a mixture containing tetramethylammonium ion, tetraethylammonium ion, tetrapropylammonium ion, triethanolamine, trimethylamine and triethylamine. The constituents were separated by isocratic elution using an IonPac CS17 column, a cation-exchange column, and detected by conductivity and mass spectrometry. The newly developed method for the six components demonstrated that the repeatability in terms of relative standard deviation for three measurements was in the range of 0.1-0.5 %. The detection limits were between 0.2 and $0.9{\mu}g/mL$ by the IC/ESI-MS.

Medical Image Processing with Local Variati on of the Image Quality (화질의 국소적 변화를 고려한 의용화상처리)

  • 홍승홍
    • Journal of the Korean Institute of Telematics and Electronics
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    • v.12 no.1
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    • pp.1-6
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    • 1975
  • The boundary has been one of the most important information in radiographic images and the degrees of difficulty involved varies greatly with the quality of the picture. These Buantifications are the means to diagnoses. The purpose of this paper is to quantify intensity variation and the threshold decision which is based on statistical principles and is developed to detect limits in liver scintigrams the entire picture is devide4 into 64 small regions. The kurtosis and variances for each smal region are used as indications to select the histograms the thresholds are computed according to the method o(maximum likelihood which minimizes the probability o( misclassification. Therefore Ive have demonstrated the applicability of the boundary detection and proved good agreement with human recognition, and we can use it for the diagnosis data of liver disease.

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Comparative Analyses of Bioactive Constituents from Forsythia suspensa and Forsythia viridissima by HPLC-DAD

  • Won, Tae-Hyung;Liao, Lijuan;Lee, Seung-Ho;Son, Jong-Keun;Shin, Jong-Heon
    • Natural Product Sciences
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    • v.17 no.4
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    • pp.328-336
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    • 2011
  • A high-performance liquid chromatography (HPLC) with diode array detector (DAD) method was established for the discrimination of a folk medicine Forsythia suspensa and Forsythia viridissima. Five and three representative metabolites of the lignan and phenolic glycoside classes were selected for the analysis from F. suspensa and F. viridissima, respectively. The optimal chromatographic conditions were obtained on an ODS column (5 ${\mu}m$, $4.6{\times}250$ mm) with the column temperature at $40^{\circ}C$. The mobile phase was composed of methanol and 0.3% acetic acid using an isocratic elution with the flow rate 1 mL/min. Detection wavelength was set at 280 nm. All calibration curves showed good linear regression ($r^2$ > 0.996) within test ranges. Limits of detection (LOD) and limits of quantitation (LOQ) values were lower than 0.096 and 0.291 ${\mu}g/mL$, respectively. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.07-0.63% and 0.14-0.62%, respectively, and the overall recoveries of 97.79-102.46% for all of the compounds analyzed. In addition, effectiveness of diverse extraction methods was compared to each other for the development of standard analytical method. The verified method was successfully applied to the quantitative determination of representative metabolites in fifty-three commercial F. suspensa samples and fifteen commercial F. viridissima samples from diverse sources. The overall analytical results showed the unequivocal differences in bioactive constituents between F. suspensa and F. viridissima.

Simultaneous Determination of 11 Marker Compounds in Gumiganghwal-tang by HPLC-DAD and LC-MS

  • Weon, Jin Bae;Jung, Youn Sik;Ryu, Gahee;Yang, Woo Seung;Ma, Choong Je
    • Natural Product Sciences
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    • v.22 no.4
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    • pp.238-245
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    • 2016
  • Gumiganghwal-tang has been used for the treatment of common cold for a long-time. We developed an accurate and sensitive high performance liquid chromatography-diode array detection (HPLC-DAD) and electrospray ionization mass spectrometry method for the simultaneous determination of ferulic acid, baicalin, bergapten, methyl eugenol, glycyrrhizin, oxypeucedanin, wogonin, nodakenin, atractylenolide III, imperatorin, and atractylenolide I in Gumiganghwal-tang samples. The analytes were separated on a Shiseido C18 column ($5{\mu}m$, $4.6mm\;I.D.{\times}250mm$) with gradient elution with acetonitrile and 0.1% trifluoroacetic acid. Eleven compounds were quantitatively determined by HPLC-DAD and identified by LC-MS data. We also validated this method. The calibration curves of all the compounds showed good linear regression. The limits of detection and the limits of quantification ranged from 0.04 to 0.63 and from 0.12 to $1.92{\mu}g/mL$, respectively. The relative standard deviation values of intra- and inter-days of this method represented less than 2.9%. The recoveries were found to be in the range of 90.06 - 107.66%. The developed method has been successfully applied to the analysis of Gumiganghwaltang samples. The established HPLC method could be used to quality control of Gumiganghwal-tang.

Analytical Method of Polybrominated Biphenyl Ethers(PBDEs) in Environmental Samples (환경시료 중 폴리브롬화비페닐에테르(Polybrominated Biphenyl Ethers) 분석법)

  • Kim, T.S.;Hwang, S.Y.;Shin, S.K.
    • Analytical Science and Technology
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    • v.15 no.4
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    • pp.346-359
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    • 2002
  • The brominated flame retardants (BFRs) are one of the unregulated pollutants in Korea, which is recently highlighted the new pollutants of environmental contamination. In this study, the previous research papers related the BFRs were surveyed, and the analytical methods of BFRs were established. The results are followed; The 40 kinds of PBDEs standards were used to establish the analytical methods to perform the experiments of recoveries and detection limits in water and soil. The detection limits of PBDEs using GC/MS represented 5.0~10.0 pg/L for water and 0.5~2.0 ng/g for soil samples. The average recoveries of water samples were 89~98% with ethylacetate, n-hexane and dichloromethane, and 89~103% in combined solvent with n-hexane and acetone. In soxhlet extraction, the higher recoveries obtained the acetone:n-hexane(1:1) comparing with acetone:dichloromethane(1:1).

Simultaneous Determination of the Flavonoids and Limonoids in Citrus junos Seed Shells Using a UPLC-DAD-ESI/MS

  • Jo, Ara;Shin, Ji hun;Song, Hwa young;Lee, Ye Eun;Jeong, Da Eun;Oh, Sung Hwa;Mun, Myung Jae;Lee, Mina
    • Natural Product Sciences
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    • v.26 no.1
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    • pp.64-70
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    • 2020
  • Citrus junos seeds (CS) have been traditionally used for the treatment of cancer and neuralgia. They are also used to manufacture edible oil and cosmetic perfume. A large amount of CS shells without oil (CSS) are discarded after the oil in CS is used as foods or herbal remedy. To efficiently utilize CSS as a by-products, it needs to be studied through chemical analysis. Therefore, we developed an ultra-performance liquid chromatography (UPLC)-diode array detection (DAD) method for simultaneous determination and quantitative analysis of five components (two flavonoids and threes limonoids) in CSS. A Waters Acquity UPLC HSS T3 column C18 (2.1 × 100 mm, 1.8 ㎛) was used for this separation. It was maintained at 40 ℃. The mobile phase used for the analysis was distilled water and acetonitrile with gradient elution. To identify the quantity of the five components, a mass spectrometer (MS) with an electrospray ionization (ESI) source was used. The regression equation showed great linearity, with correlation coefficient ≥ 0.9912. Limits of detection (LOD) and limits of quantification (LOQ) of the five compounds were 0.09 - 0.13 and 0.26 - 0.38 ㎍/mL, respectively. Recoveries of extraction ranged from 97.45% to 101.91%. Relative standard deviation (RSD) values of intra- and inter-day precision were 0.06 - 1.15% and 0.19 - 0.25%, respectively. This UPLC-DAD method can be validated to simultaneously analyze quantities of marker flavonoids and limonoids in CSS.

Method for the Analysis of Polybrominated Biphenyls(PBBs) in Environmental Samples (환경시료 중 폴리브롬화비페닐(Polybrominated Biphenyls) 분석법)

  • Shin, S.K.;Kim, T.S.;Hwang, S.Y.;Lee, W.S.;Chung, Y.H.;Na, J.G.
    • Analytical Science and Technology
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    • v.15 no.3
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    • pp.300-316
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    • 2002
  • The extraction methods of PBBs from environmental samples by soxhlet extraction for solid phase and liquid-liquid extraction for liquid phase were compared. After extraction, silicagel and florisil as column clean up methods were used for the comparison of cleanup efficiency with different solvent system. Also, the analytical instruments were used GC/MSD. The 22 kinds of PBBs standards were used to establish the analytical methods to perform the experiments of recoveries and detection limits in water and soil. The detection limits of PBBs represented 5~10 ng/L for water and 0.5~3.5 ng/g for soil samples, respectively. The recoveries of water samples represented 96~107% in n-hexane, dichloromethane and toluene for water, and 60~80% in combined solvent with n-hexane and acetone. The recoveries of soil sample were surveyed 67~97% in soxhlet extraction and 64~76% in ultrasonic extraction with selected solvents.

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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Study on the Level of Organochlorine Pesticide Residues in Agricultural Products (농산물 중 유기염소계 잔류 농약에 관한 연구)

  • 엄미나;장재철;정진아;유영희;지의상
    • The Korean Journal of Food And Nutrition
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    • v.14 no.5
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    • pp.446-456
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    • 2001
  • This study was carried out for the dietry safely based on the level of pesticide residues In 13 kinds of agricultural products consumed in Kyonggi-Do. Korea. From June to October 2000, sixteen organochlorine pesticides in 397 samples were analyzed by using GC/ECD and GC/MSD. According to the results, endosulfan were detected in 27(7.8%) samples and chlorothalonil were detected in 4(1.0%) samples. Detection ranges of endosulfan were 3.7437∼ 0.0488ppm for lettuce, 2.1902 ∼0.1423ppm for spinach, 2.4909 ∼0.0786ppm for mallow and 3.2333∼0.3997ppm for mustard leaf, respectively Chlorothalonil were 5.8097 for lettuce and 0.8962ppm for spinach. Consequently, six agricutural products were detected more than the maximum residue limits in Korea Endosulfan were detected In 5(1.8%) samples and cholrothalonil were detected in 1(0.3%) sample. Detection rates of endosulfan sulfate(45.9%) of agricultural products were more than $\alpha$-endosulfan(28.5% ) and $\beta$-endosulfan (23.9% ) .

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