• Title/Summary/Keyword: simultaneous analytical method

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Development of Simultaneous Analytical Method for Various Residual Pesticides Using GC-ECD (GC-ECD를 이용한 잔류 농약 다성분 동시 분석법 개발)

  • 김우성;손영욱;정지윤;안경아;홍무기;임무혁;이홍재;이봉헌;박흥재
    • Journal of Environmental Health Sciences
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    • v.27 no.1
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    • pp.88-92
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    • 2001
  • The simultaneous analytical method for 37 residual pesticides was developed by a gas chromatography with $^{63}$ Ni electron capture detector. Pesticides added in soybean sample were extracted with 70% acetone in water and methylene chloride in oder, and then cleaned up via open-column apparatus packed with florisil and alumina N. The Ultra-2 fused capillary column was used to separate the products. The resolution between the last isomeric peak of cypermethrin (56.398 min) and the first isomeric peak of flucythrinate (56.421 min) was not satisfactory and the last isomeric peak of fenvalerate(58.783 min) and the first isomeric peak of fluvalinate(58.835 min) was overlapped. Except for $\alpha$-BHC, dichlofluanid, captan, and captafol, most recoveries were showed over 70%.

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Analytical Quality by Design Methodology Approach for Simultaneous Quantitation of Paeoniflorin and Decursin in Herbal Medicine by RP-HPLC Analysis

  • Kim, Min Kyoung;Park, Geonha;Hong, Seon-Pyo;Jang, Young Pyo
    • Natural Product Sciences
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    • v.27 no.4
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    • pp.264-273
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    • 2021
  • Simultaneous quantification of multiple marker compounds in herbal medicine by high performance liquid chromatography (HPLC) analysis is still a challenge due to the complexity in various parameters to be considered and co-existing multi-components. As a case study, a reliable HPLC method for simultaneous quantification of paeoniflorin from Paeoniae Radix and decursin from Angelicae Gigantis Radix in various commercial herbal medicine was developed based on analytical quality by design (AQbD) strategy. As a first step, risk assessment was performed to select the critical method parameters (CMPs) which were decided as organic mobile phase ratio and column oven temperature. In order to evaluate the effect of the CMPs on critical method attributes (CMAs) of peak resolution and tailing, central composite design (CCD) was employed. The final chromatographic conditions were optimized as follows: column- C18, 4.6 × 250 mm, 5 ㎛ particle size; mobile phase- A: acetonitrile, B: 0.1% acetic acid water; detection wavelength- 235 nm for paeoniflorin, 325 nm for decursin; column oven temperature- 25℃; flow rate- 1.0 mL/min; gradient mobile phase system as Time (min) : % A, 0:14, 25:14, 30:50, 60:50, 61:100, 65:100, 66:14, 75:14. The method was successfully validated according to the International Conference on Harmonization (ICH) guidelines and piloted for ten commercial herbal medicines.

A Study on the Analytical Method of Trace Metal Ions in Sea Water by Inductively Coupled Plasma - Mass Spectrometry using Solid-Liquid Extraction Technique (유도결합 플라스마-질량분석법과 고체-액체 추출법을 이용한 해수중 미량금속의 분석에 관한 연구)

  • Lee, Won;Park, Kyung-Su;Kim, Eun Kyung;Hur, Young-Hoe
    • Analytical Science and Technology
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    • v.11 no.6
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    • pp.499-504
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    • 1998
  • An analytical method for the simultaneous measurement of trace Cu, Sn, and Bi in sea water has been investigated by Inductively Coupled Plasma-Mass Spectrometry. Amberlite IRC-718 resin was used as a solid phase in solid-liquid extraction technique for the removal of matrix interferences such as Na, S, P, and other polyatomic ion species. Recoveries of 99.8% for Cu, 99.6% for Sn, and 97.9% for Bi were obtained for the standard spiked sample. The developed method was applied to analysis of trace metals in sea water.

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Simultaneous Determination of 285 Chemicals in Water at ppt Levels by GC-Ion Trap Mass Spectrometry

  • Kadokami, Kiwao;Sato, Kenji;Koga, Minoru;Shinohara, Ryota
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.771-778
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    • 1995
  • The authors have developed an analytical method for determining trace amounts of 285 kinds of chemicals in natural waters by GC-ion trap MS. The results of overall recovery tests at $0.1{\mu}g/l$ showed that the mean recovery was 92.1% and the mean relative standard deviation was 10.8%. The mean of the method detection limits was $0.036{\mu}g/l$. From the results of analysis of real samples, it was confirmed that this method is useful to elucidate the concentration levels and the fate of chemicals in the aquatic environment.

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Slope Stability Analysis Considering Multi Failure Mode (다중파괴모드를 고려한 사면안정해석)

  • Kim, Hyun-Ki;Kim, Soo-Sam
    • Journal of the Korean Society for Railway
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    • v.14 no.1
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    • pp.24-30
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    • 2011
  • Conventional slope stability analysis is focused on calculating minimum factor of safety or maximum probability of failure. To minimize inherent uncertainty of soil properties and analytical model and to reflect various analytical models and its failure shape in slope stability analysis, slope stability analysis method considering simultaneous failure probability for multi failure mode was proposed. Linear programming recently introduced in system reliability analysis was used for calculation of simultaneous failure probability. System reliability analysis for various analytical models could be executed by this method. For application analysis for embankment, the results of this method shows that system stability of embankment calculate quantitatively.

골프장 농약 검사를 위한 다성분동시시험방법 확립에 관한 연구

  • 이민효;노회정;박종겸;윤정기;김찬섭
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2002.09a
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    • pp.81-85
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    • 2002
  • The possibility of simultaneous analysis of 24 pesticides out of 30 residual pesticides which are subjected to test in the golf courses was examined. The utility of the simultaneous analysis of multi-residue pesticides was evaluated by recovery test through a standard addition method of pesticides in water, soil, and lawn grass. The experimental results of the recovery rates for individual pesticides are as follows : The number of pesticide of which average recovery was over 70% regardless of medium was 16 pesticides. These pesticides were composed of 8 organophosphorus pesticides(Chlorpyrifos, Chlorpyrifos-methyl, Diazinon, EPN, Fenitrothion, Phenthoate, Phosalone, and Toclofos-methyl). 4 organochlorinated pesticides(Daconil, Captan, Endosulfan, and Tetradifon), 2 pyrethroid pesticides(Fepropathrin, Lambda-cyhalothrin) and 2 other pesticides(Bromopropylate, Pendimethalin). On the other hand, in case of Dicofol, average recovery by medium was over 70% for water and lawn grass but was only 53.3% for soil. Therefore, the simultaneous analytical method applied in this experiment is not appropriate for analysis of Dicofol in soil. Furthermore, among 7 pesticides, 2 pesticides(Amitraz and Pyraclofos) showed that theirs average recovery rates deviated from criteria(70~130%) at almost all media, while 5 pesticides(Bensulide, Deltamethrin, Iprodione, Phosphamidon and Tralomethlin) were not detected from all media by selected GC detector(NPD or ECD).

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Simultaneous Determination of 4-Nitrotoluene and Benzophenone in Ground Water and Soil by Gas Chromatography-Mass Spectroscopy

  • Kwon, Oh-Seung;Kim, Eun-Young;Ryu, Jae-Chun
    • Analytical Science and Technology
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    • v.16 no.1
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    • pp.59-69
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    • 2003
  • Benzophenone (BZP) and 4-nitrotoluene (4-NT) listed as endocrine disrupting chemicals are suspected to contaminate ground water sites and soil. Analytical method for simultaneous determination of the two chemicals in soil and ground water was developed by gas chromatography-mass spectrometry. Water (100 ml) was extracted with hexane, and soil (10 g) was extracted with methanol and hexane. Recovery in water was >72% for BZP and 90-118% for 4-NT. Recovery for 4-NT and BZP in soil was 51-59% with coefficient variation of less than 19.5%. Calibration curves showed a good linearity with $r^2=0.997$. In water and soil collected at nation-wide sites, BZP was found at 5 sites among 43 water sites at the concentration of $14.87{\pm}3.83ng/100 ml$. No 4-NT was found. It is suggested that this method is appropriate to the simultaneous quantitation of 4-NT and BZP in ground water and soil samples.

Simultaneous Analytical Method of Organochlorine and Pyrethroid Pesticides using GC(ECD) (GC-ECD를 이용한 유기염소계 밑 Pyrethroid계 농약 동시 분석법)

  • 김우성;이선화;김재이;정지윤;이명자;박영채;이영자;정성욱;이봉헌
    • Journal of Environmental Science International
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    • v.12 no.4
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    • pp.477-480
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    • 2003
  • Pesticides were extracted from samples with 70% acetone and methylene chloride in order, and then cleaned up via open-column chromatography apparatus packed with florisil, and finally analyzed simultaneously the organochlorine and pyrethroid pesticides using GC(ECD). An ultra-2 fused silica capillary column was used to separate and identify the products. The resolution between the last isomeric peak of cypermethrin(59.987min) and the first isomeric peak of flucythrinate(60.043min) was not satisfactory. The last isomeric peak of fenvalerate(62.344min) and the first isomeric peak of fluvalinate(62.397min) were overlapped. Recoveries of soybean sample fer the most pesticides were 73.3% to 102.4%. Detection limits were between 0.004 and 0.063 ${\mu}$g/mg when this method was used.

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.