• Title/Summary/Keyword: GC-MS analysis

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Development of Multi-residue Analysis of 320 Pesticides in Apple and Rice Using LC-MS/MS and GC-MS/MS (LC-MS/MS와 GC-MS/MS를 이용한 사과와 쌀 시료에서 320종 농약의 다성분 분석)

  • Kim, Jong-Hwan;Kim, Yeong-Jin;Kwon, Young-Sang;Seo, Jong-Su
    • The Korean Journal of Pesticide Science
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    • v.20 no.2
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    • pp.104-127
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    • 2016
  • A new analytical method has been developed to determine 320 pesticides in apple and rice. The extraction of pesticides was carried out based on QuEChERS sample extraction, and determination was performed using LC-MS/MS and GC-MS/MS. 320 pesticides were selected for experiments. 251 and 110 pesticides among them were analysed by LC-MS/MS and GC-MS/MS, respectively. 41 pesticides of them were analyzed by both GC-MS/MS and LC-MS/MS. Among pesticides analysed by LC, 242 pesticides (96% of total number) in apple and 237 pesticides (94% of total number) in rice showed recoveries in the range of 70~120% with RSD ${\leq}20%$. In case of pesticides analyzed by GC-MS/MS, 103 pesticides (94% of total number) in apple and 83 pesticides (76% of total number) in rice were successfully validated. These results indicated that LC-MS/MS and GC-MS/MS analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in agricultural products.

GC/MS and GC/ECD Analysis of Residual Pesticides in Herbal drugs (GC/MS와 GC/ECD를 이용한 한약재 중 잔류 농약의 분석)

  • Kim, Ho-Kyoung;Park, So-Yeon;Ko, Byoung-Seob
    • The Journal of Korean Medicine
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    • v.20 no.1 s.37
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    • pp.44-51
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    • 1999
  • Analysis of residual pesticides in herbal drugs was performed by GC-ECD and GC-MS. Especially, selected ion monitoring(SIM) technique was applied to increase the GC/MS sensitivity. Analysis of residual pesticides was determined sensitivity and selectively without any internal standard by setting the SIM technique to their characteristic fragments for quantitation ion and confirmation ion. The combination of two detector, GC-ECD and MS-SIM technique, is abailable for determining a multiclass residual pesticides in herbal drugs. The average recoveries through the method were $65.9%{\sim}99.7%$ in herbal drugs. The data of gas chromatographic analysis was compared with the limits of residual pesticides in herbal drugs and agricultural foods. 4. 4-DDT was detected above the limits to the residual pesticides in herbal drugs. Diazinon and EPN were detected, but the limits of residual pesticides were less than that of agricultural foods.

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Analysis of Residual Pesticides in Herbal Drugs: GC/MS Analysis of 27 Controlled Pesticides (생약 중 잔류 농약의 분석법: GC/MS에 의한 27종 잔류 규제 농약의 분석)

  • Park, Man-Ki;Park, Jeong-Hill;Yoon, Hye-Ran;Yoon, In-Byoung;Cho, Sool-Yeon;Hwang, Gwi-Seo
    • YAKHAK HOEJI
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    • v.40 no.2
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    • pp.141-148
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    • 1996
  • GC/MS analysis of 27 controlled pesticides in herbal drugs was studied. Selected ion monitoring(sim) technique was applied to increase the GC/MS sensitivity. Typical peaks in th e mass spectrum of each pesticides were selected as quantitation, comfirmation or alternate ion. Twenty seven pesticides were divided into five groups according to their retention time and the peaks for SIM were programmed accordingly. The combination of two ionization methods, electron impact(EI)-SIM-MS and negative ion chemical ionization(NCI)-SIM-MS, were well-fitted for the detection, confirmation and quantitation of multiclass residual pesticides in herbal drugs.

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GC/MS and its applications for the analysis of cosmetic produtcts (GC/MS와 화장품 분석의 응용)

  • 노경원
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.19 no.1
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    • pp.1-19
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    • 1993
  • Gas chromatography serves to separate the mixtures into its components, and mass spectrometer is used to analyzing of unknown compounds. But there are many problems the identification of horn compounds using by GC only. As this reason GC/MS a very powerful analyzing technique. Mass spectrometer consists of 1) inlet stem 2) ion source 3) Bass filter 4) detectors and 5) data system. There are two analyzing modes in the GC/MS, those are scan and SIM(selected ion mom toping) modes. Scan mode is used when analyzing unknown compounds and SIM mode al lows the mass spectrometer to detect specific compound with very high sensitivity. As GC/MS applications for the analysis of cosmetic products, volatile compounds in lotion, earn foundation and hair color, and carbon distribution of fatty acids in soap were performed. Also as a new sample pre-treatment technique, head space sampler/GC/MS introduced in order to analyze the volatile compounds in a toothpaste.

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Analytical Characteristics of GC/MS and HPLC according to the Concentration Distribution of PAHs (PAHs 농도 분포에 따른 GC/MS와 HPLC의 분석특성에 관한 연구)

  • Hong, Jwa-Ryung;Choi, Kwang-Min
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.25 no.3
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    • pp.312-321
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    • 2015
  • Objectives: The purpose of this study was to determine the best method to analyze PAHs at extremely low concentrations. To this end, 16 PAHswere analyzed simultaneously by GC/MS, HPLC/FLD and HPLC/UVD, and the analytical characteristics of HPLC and GC/MS were compared. Methods: This study was conducted by GC/MS and HPLC/FLD/UVD, and evaluated linearity, precision and detection limit. Standard solutions were prepared for 21 samples in the range of $0.00001{\sim}1.0{\mu}g/mL$ and the samples were divided into four groups. All samples were made in three sets and analysis was replicated seven times. Results: Sixteen PAHs could be simultaneously separated by HPLC and GC/MS, and the adequate equipment was HPLC/FLD. The retention times by HPLC were shorter than GC/MS, and HPLC had better separation for most PAHs than GC/MS. The peaks of naphthalene and naphthalene-D8 partially overlapped for GC/MS. HPLC/FLD had a 20-2000 times lower limit of detection than GC/MS and UVD. However FLD was not adequate for analyzing acenaphthylene because it has too low a fluorescence quantum yield to be detected. The precision of HPLC/FLD/UVD and GC/MS showed less than 20% at $0.001{\mu}g/mL$ PAHs and when the concentration was higher, the coefficient of variation was decreased. HPLC/FLD was better for the overall detection of limits. Conclusions: The results indicate that the HPLC/FLD method has good linear range, precision and a detection of limits from $0.00001{\sim}0.0001{\mu}g/mL$ for all 16 PAHs. This study contributes to providing useful data for analysis technology and can be applied to occupational exposure measurement for PAHs in workplaces.

Analysis of Binding Media Used in Mural Painting of Temple Wall by Pyrolysis/GC/MS and IR (열분해/GC/MS와 IR을 이용한 사찰 벽화 시편 교착제 분석)

  • Park, Jongseo;Lee, Jeong Won
    • Journal of Conservation Science
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    • v.33 no.5
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    • pp.345-354
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    • 2017
  • A mural was discovered in the Ssanggyesa temple located in Jindo island, during repair of the Daeungjeon Hall. A study was conducted to determine the binding medium used for preparing the mural. Pyrolysis/GC/MS and IR spectrometry were used to analyze a painting specimen. Direct approach and on-line methylation approach were attempted for the pyrolysis/GC/MS. In IR analysis, the spectra of the specimen were found to be different from those of Asian lacquer, yellow lacquer, animal glue, and acrylic emulsion resin. They were also not identical to the standard IR spectra of drying oils such as linseed oil. Pyrolysis/GC/MS results of the specimen were different from those of Asian lacquer, yellow lacquer, animal glue, and acrylic emulsion resin. In the mean time, palmitic acid, octadecanoic acid, nonanedioic acid, and octadecenoic acid, which are characteristic pyrolysis products of dried drying oil, were detected. In addition, the pyrolysis/GC/MS chromatograms of the specimen and dried drying oil were also very similar. Therefore, it was concluded that the painting was prepared using drying oil as a binding medium.

Analysis of Plant Hormones using GC-MS (GC-MS를 이용한 식물홀몬 분석)

  • 조광연
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.34 no.s01
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    • pp.26-32
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    • 1989
  • The analytic principles of GC and MS were explained in relation to plant hormone analyses and the characteristics of two instruments were compared. The selection of column, condition of measurement and the method of ionization to get a good spectrum were also briefly described. Finally, the pre-treatment of sample by solvent extraction method to remove the unnecessary part of sample and the synthetic method, especially reagents and reaction condition, for the preparation of ether or ester derivative which can be easily vaporized in GC were explained.

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Determination of N-nitrosamines in Water by Gas Chromatography Coupled with Electron Impact Ionization Tandem Mass Spectrometry (EI-GC/MS/MS를 이용한 니트로사민류의 수질분석)

  • Lee, Ki-Chang;Park, Jae-Hyung;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.36 no.11
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    • pp.764-770
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    • 2014
  • This study assessed analysis of N-nitrosamines by separation, identification, and quantification using a gas chromatography (GC) mass spectrometer (MS) with electron impact (EI) mode. Samples were pretreated by a automated solid phase extraction (SPE) and a nitrogen concentration technique to detect low concentration ranges. The analysis results by EI-GC/MS (SIM) and EI-GC/MS/MS (MRM) on standard samples with no pretreatment exhibited similar results. On the other hand, the analysis of pretreated samples at low concentrations (i.e. ng/L levels) were not reliable with a EI-GC/MS due to the interferences from impurity peaks. The method detection limits of eight (8) N-nitrosamines by EI-GC/MS/MS analysis ranged from 0.76 to 2.09 ng/L, and the limits of quantification ranged from 2.41 to 6.65 ng/L. The precision and accuracy of the method were evaluated using spiked samples at concentrations of 10, 20 and 100 ng/L. The precision were 1.2~13.6%, and the accuracy were 80.4~121.8%. The $R^2$ of the calibration curves were greater than 0.999. The recovery rates for various environmental samples were evaluated with a surrogate material (NDPA-$d_{14}$) and ranged 86.2~122.3%. Thus, this method can be used to determine low (ng/L) levels of N-nitrosamines in water samples.

Development of a GC-MS Automatic Analysis Program to Provide Information on Exposure to Chemical Substances (화학물질 노출정보 제공을 위한 GC-MS 분석자동화 프로그램 개발)

  • Park, Seung-Hyun;Park, Hae Dong;Jang, Miyeon;Ro, Jiwon;Cho, Hyounmin
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.31 no.1
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    • pp.1-12
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    • 2021
  • Objective: The purpose of this study was to contribute to the prevention of occupational diseases through the development of an automatic analysis program for evaluating workers' exposure to hazardous chemical substances. Methods: The authors selected chemical substances that caused occupational disease in Korea and chemical substances that are frequently used in industrial sites as target substances for a GC-MS automatic analysis program. The target substances are organic compounds which can be measured by a passive sampler. The automatic analysis program was studied using various raw data obtained from GC-MS analysis for the target substances. Results: A total of 48 organic compounds that can be measured with a passive sampler were selected as target substances for the GC-MS automatic analysis program. The selected compounds included substances that caused occupational disease, substances related to C1 and D1 in special health examinations, and substances for which work environment measurements have been frequently conducted. The GC-MS automatic analysis program was developed by combining information mainly on retention time and mass spectrum. The GC-MS automatic analysis program is designed to analyze unknown samples by comparing the mass spectrum and retention time of the samples to those of reference materials. To evaluate the stability of the program, samples at about the 30-50% level of OELs were prepared and analyzed with the GC-MS automatic analysis program, resulting in stable results for all 48 organic compounds. Conclusion: An automatic analysis program for a total of 48 organic compounds was developed using a GC-MS system that can analyze organic compounds. Unknown samples that contain the 48 organic compounds can be automatically analyzed by the developed program. It is anticipated that it can contribute to the prevention of occupational diseases through an GC-MS automatic analysis program that can quickly provide workers with information on exposure to chemical substances.

Quantitative Analysis of the Seven Marker Components in Asarum sieboldii using the LC-MS/MS and GC-MS (LC-MS/MS와 GC-MS를 이용한 세신 추출물 중 7종 성분의 함량분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.44 no.4
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    • pp.350-361
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    • 2013
  • Asarum sieboldii has been used for treatment of fever, pain, common cold, and chronic sinusitis in Korea. In this study, we performed quantification analysis of seven major constituents including aristolochic acid I, aristolochic acid II, ${\alpha}$-asarone, ${\beta}$-asarone, elemicin, methyl eugenol, and safrole in the 70% ethanol extract of Asarum sieboldii and its solvent fractions, n-hexane, ethylacetate, n-butanol, and water ones using a ultra-performance liquid chromatography-electrospray ionization-mass spectrometer(UPLC-ESI-MS) and gas chromatography-mass spectrometer(GC-MS). Regression equations of seven components were acquired with $r^2$ values >0.99. The values of limit of detection(LOD) and quantification(LOQ) were 0.1-3.9 ng/mL and 0.3-11.7 mg/mL, respectively. The amount of the seven compounds in Asarum sieboldii were not detected -143.66 mg/g. The established LC-MS/MS and GC-MS methods will be helpful to improve quality control of Asarum sieboldii.