• Title/Summary/Keyword: RSD

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Simultaneous Determination of (-)-Menthone and (-)-Menthol in Menthae Herba by Gas Chromatography and Principal Component Analysis

  • Kim, Jung-Hoon;Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Natural Product Sciences
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    • v.16 no.3
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    • pp.180-184
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    • 2010
  • The simple and accurate method was established for the simultaneous determination of (-)-menthone and (-)-menthol in Menthae herba obtained from Korea and China. A quantitative analysis was performed with a gas chromatography-flame ionization detector and reference compounds were separated on a capillary HP-Innowax column (30 m $\times$ 0.23 mm, 0.50 ${\mu}m$, Agilent, MA, USA). The correlation coefficients of the compounds showed good linearity ($r^2$ > 0.9997) over the linear range. The precision, repeatability and stability showed less than 1.7% of relative standard deviation (RSD) values for two compounds. Recovery rates were within the range of 95.72 - 103.76%. The method was applied successfully to analyze 15 samples of Menthae herba and achieved sufficient and specific separation of reference compounds. The principal component analysis (PCA) exhibited the classification of 15 samples according to their locations of origin.

Effective Analysis of Dicyclanil in Lamb and Chicken Muscle using HPLCUV/Vis and LC/MS/MS

  • Kim, Byung-Ju;Myung, Seung-Woon
    • Mass Spectrometry Letters
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    • v.2 no.2
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    • pp.45-48
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    • 2011
  • The authors describe a method for monitoring dicyclanil levels in lamb and chicken muscle tissues. The devised procedure involves dicyclanyl extraction by SPE and its detection HPLC-UV/Vis and LC/MS/MS. The method was found to have LOD and LOQ values of $0.02\;mg\;kg^{-1}$ and $0.05\sim0.06\;mg\;kg^{-1}$, respectively. The intraday precision and an accuracy of spiked samples were found to have 2.3~10.4 RSD% and 80.9~105.7%, respectively.

기체크로마토그래피-질량분석검출기와 고체상미량추출법을 이용한 물 중의 MTBE 미량분석

  • Jeon Chi-Wan;Lee Jeong-Hwa;Jeong Yeong-Uk
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2005.04a
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    • pp.195-198
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    • 2005
  • A solid-phase microextraction and gas chromatography-mass spectrometry for the extraction and analysis of methyl-tert-butyl ether has been described. methyl-tert-butyl ether was extracted from aqueous solution using SPME fiber coated polydimethylsiloxane and analysed by GC-MS with capillary column. Extraction parameters and chromatographic separation conditions were optimized. The applied method represented good analytical performance in terms of precision (3-8%, RSD) and accuracy(93-102%, mean recovery) with a method detection limit of 0.03 ppb.

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Analysis of Agrochemical Residues in Tobacco Using QuEChERS Method by GC-MS/MS

  • Lee, Jeong-Min;Jang, Gi-Chul;Hwang, Keon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.29 no.2
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    • pp.132-139
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    • 2007
  • This study was performed to apply the more rapid and accurate sample preparation, and the high selectivity and sensitivity of the analyte detection by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). QuEChERS (quick, easy, cheap, effective, rugged and safe) method was validated for 49 agrochemicals in the CORESTA Agrochemical Advisory Committee guide and amenable to GC-MS/MS determination. In QuEChERS method, the effects of sorbents (PSA, $C_{18}$ and GCB) and matrix of the analytes in tobacco types (flue-cured, burley and oriental) were investigated. MS/MS acquisition provided high specificity and selectivity for agrochemicals and low limit of quantification. QuEChERS by using PSA alone and the matrix-matched standards gave good recoveries and RSD values in three types of tobaccos. QuEChERS method was no needed to be complex clean-up procedure and would be used as the fast and easy method for agrochemical residue analysis in tobacco.

Enantioseparation of Flurbiprofen and Ketoprofen in Patches and in Urine Excretions by Achiral Gas Chromatography

  • Paik, Man-Jeong;Nguyen, Duc-Toan;Kim , Kyoung-Rae
    • Archives of Pharmacal Research
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    • v.27 no.12
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    • pp.1295-1301
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    • 2004
  • The enantiomeric composition tests on flurbiprofen and ketoprofen present in patch products and in urine excretions following patch applications were performed as diastereomeric (R)-(+)- 1-phenylethylamides by achiral gas chromatography and by gas chromatography-mass spectrometry in selected ion monitoring mode. The method for determination of (R)- and (S)-enantiomers in the range from 0.1 to 5.0 ${\mu}$g was linear (r ${\ge}$ 0.9996) with acceptable precision (% RSD ${\le}$5.2) and accuracy (% RE = 0.6 ~ -2.4). The enantiomeric compositions of flurbiprofen in one patch product and of ketoprofen in five different products were identified to be racemic with relatively good precision (${\le}$ 6.4%). The urinary excretion level of (R)-flurbiprofen was two times higher than its antipode, while the comparable excretion levels of (R)- and (S)-enantiomers for ketoprofen were observed.

Determination of Trace Aldehydes in Ambient Air by Liquid Chromatography (액체 크로마토그래프법에 의한 대기시료중 미량 알데히드류의 정량)

  • 이용근;정태우
    • Journal of Korean Society for Atmospheric Environment
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    • v.11 no.4
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    • pp.339-349
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    • 1995
  • The purpose on this study is to optimize the chromatographic determination method of trace aldehydes in ambient air. Carbonyl compounds in urban air were trapped at $C_{18}$ DNPH-coated cartridges, and generated hydrazone derivatives were separated by HPLC and detected by UV-vis spectroscopic detector at 360nm. Formaldehyde and acetaldehyde compounds could be isolated from urban(Seoul) air with more than 95% collection efficiency. The analytical detection limits for formaldehyde and acetaldehyde are 0.06pp $b_{v}$, 0.08pp $b_{v}$ for 108 L air samples, respectively. The precision of this method are 3 .sim. 4%(RSD) for mutiple injection of hydrazone standards. Separation of seven dinitrophenylhydrazones could be achieved in appoximately 20 minutes operation time using $C_{18}$ column with apprepriate eluent. The method was applied to the analysis of aldehydes and ketone in Seoul ambient air. The 24-h ambient levels of formaldehyde, acetaldehyde reached up to 6 .sim. 14 and 3 .sim. 8ppbv, respectively. The daily average concentration ratio were 0.60 for acetaldehyde/formaldehyde.yde.

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Automated Determination of SOx in Air by Diffusion Scrubber-lon Chromatography (확산포집-이온크로마토그래프법을 이용한 대기중 SOx의 자동정량)

  • 이용근;이동수;백선영
    • Journal of Korean Society for Atmospheric Environment
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    • v.11 no.4
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    • pp.307-313
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    • 1995
  • An automatic method is developed for the determination of SOx in atmosphere. The method involves SOx sampling in diffusion scrubber followed by ion chromatographic analysis. Filtered air is withdrawn at 1.8.ell./min through a diffusion scrubber of which inner tube is made of PTFE(Gore-tex) membrane tubing. 1mM $H_{2}$ $O_{2}$ is used as absorbing solution so that SOx is oxidized to S $O_{4}$$^{2-}$. The scrubbered solution is automatically injected into ion chromatograhpy eith conductivity detection for sulphate determination. Replacement of commonly used polyproplene membrane with PTFE gives several merits such as easy preparation of diffusion scrubber, better collection efficiency. No measurable memory effect is experienced, and this isin contrast to previous work for ammonia. Detection limit of this method defined by three times standard deviation is 0.56ppbv. The precision is 0.4% RSD at SOx concentration of 7.3ppbv Results for Seoulatmosphere ate presented.

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Simultaneous HPLC Determination of Preservatives in Cosmetics (화장품중 살균ㆍ보존제의 동시분리 및 정량)

  • 양성준;김영옥;손경훈;이정표;정래석;양원준;백옥진;이현경;최상숙
    • YAKHAK HOEJI
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    • v.46 no.4
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    • pp.231-236
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    • 2002
  • A high-performance liquid chromatographic method for the simultaneous quantitative analysis of methylparaben (MP), ethylparaben (EP), propylparaben (PP), butylparaben (BP) and imidazolidinyl urea(IU) or diazolidinyl urea(DU) in cosmetics was studied by using a cyano-propyl column and 0.05M hexanesulfonic acid at 228 nm. Calibration curves were found to be linear in the 60-1000 $\mu\textrm{g}$/mL range (parabens), 100-1,250 $\mu\textrm{g}$/mL range (IU) and the 120-2000 $\mu\textrm{g}$/mL range (DU). Linear regression analysis of the data demonstrates the efficacy of the method in terms of precision and accuracy. An extraction method is developed and validated in order to apply this chromatographic method to a commercial cosmetic cream. The precision of this method, calculated as the relative standard deviation (RSD) of the recoveries (0.46-2.71%) was excellent for all compounds.

Development of Alternative Assay Method without Hazardous Reagent, Chloroform for Urazamide Tablets in Korean Pharmaceutical Codex (우라자미드 정의 유해시약 대체 시험법의 개발)

  • Lee, Yoo Rim;Kim, Hyun Ji;Seo, Narae;Kim, Kyeong Ho
    • YAKHAK HOEJI
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    • v.58 no.2
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    • pp.125-128
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    • 2014
  • We developed an alternative assay method without hazardous reagent of chloroform for urazamide tablets in Korean Pharmaceutical Codex. The HPLC analytical method was validated by system suitability, linearity, precision, accuracy and robustness. The linearity of the calibration curves in the desired concentration range is good ($r^2$ >0.999). Precision was obtained less than RSD 1.17%. Accuracy was obtained with recoveries in range of 98.12% and 99.47%. The developed assay could be expected to become valuable tools for revising the Korean Pharmaceutical Codex.

Determination of Fluorescent Whitening Agents in Paper Materials by Ion-Pair Reversed-Phase High-Performance Liquid Chromatography

  • Kim, Jeong Soo;Kim, Do Hwan;Kim, Keon
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.3971-3976
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    • 2012
  • A simple method was developed for the analysis of seven stilbene-type fluorescent whitening agents (FWAs) in paper materials by ion-pair reversed-phase high-performance liquid chromatography with fluorescence detection. These stilbene-type FWAs included two disulfonate, two tetrasulfonate, and three hexasulfonate compounds. After optimization of chromatographic conditions, the FWAs were satisfactorily separated using a reversed-phase column (RP-18) with the following isocratic mobile phase: methanol-water (60:40) containing 17.5 mM TBABr and 10 mM citrate buffer (pH = 7.0). The calibration plot was linear in the range from 5 to 500 ng/mL for two disulfo-FWAs and from 1 to 500 ng/mL for the other five FWAs. Precision levels of the calibration curve as indicated by RSD of response factors were 1.2 and 8.1%. Limits of quantitation (LOQ) ranged from 1.2 to 11 ng/mL.