• Title/Summary/Keyword: GC-MS/MS

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Quantitative Analysis and Qualification of Amitrole Using LC/ESI-MS (LC/ESI-MS를 이용한 아미트롤의 정성확인 및 정량분석)

  • Park, Chan-Koo;Eo, Soo-Mi;Kim, Min-Young;Sohn, Jong-Ryeul;Mo, Sae-Young
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.117-129
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    • 2004
  • Amitrole in environment, difficult to be analyzed by GC or GC/MS due to high polarity and low volatility, was analyzed by LC/ESI/MS in the study. Maximum peak intensity of amitrole in LC/MS/ESI mass spectrum is m/z 85 of protonated molecular ion $(M+H)^+$ with 30V of cone voltage at SIR mode. It was confirmed that ratios between main ion of amitrole, 85 of protonated molecular ion, and m/z 58 fragmented ion of amitrole, had increased corresponding with the increment of cone voltage from 20V to 70V. The isotope molecular weight of amitrole was $86([M+H])^+$ at LC/MS analysis and the mass spectrum ratio between 85 mass and 86 mass was not different by the change of concentration but similar to theoretical ratio(less than 10% standard deviation).The linearity of standard calibration curve under same condition with sample treatment method had $y=1.09354e^6X+26947.2$ and $r^2=0.99$. Recovery rates in water and soil samples were 77.64~83.44% and 71.11~79.44%, respectively. Reliability of the analysis was performed with 5 repeated measurements at each level of standard concentration and the result showed that relative standard deviation was less than 10%; therefore, the extraction and analysis method in the study suggested that it would be reliable to measure amitrole in water and soil media.

Gas Chromatography/Mass Spectrometry and Gas Chromatography/Tandem Mass Spectrometry of some s-Triazine Pesticides

  • Kim, Yoo-Joong;Kim, Myung-Soo
    • Bulletin of the Korean Chemical Society
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    • v.10 no.2
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    • pp.196-200
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    • 1989
  • Some s-triazine herbicides, namely simazine, atrazine, and propazine present as trace components in a complex mixture were analyzed by GC/MS and GC/MS/MS methods. Even though monitoring the molecular ions was the best in terms of sensitivity, adequate analysis could not be done when interfering species were present. When doubly charged ions which appeared at characteristic m/z values were monitored, chromatograms were rather free from interference. More importantly, selected reaction monitoring was found to provide a selective means of detection with general applicability.

Simultaneous Determination of Phthalates(DMP, DEP, DBP, BBP, DEHP, DnOP) by Solid Phase Microextraction-GC/MS (Solid Phase Microextraction-GC/MS에 의한 플라스틱가소제(DMP, DEP, DBP, BBP, DEHP, DnOP)의 동시분석)

  • Lee, Jae-Hee;Bae, Jun-Hyun;Kang, Jun-Gill;Kim, Youn-Doo
    • Journal of the Korean Chemical Society
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    • v.48 no.1
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    • pp.17-27
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    • 2004
  • A procedure based on solid phase microextraction extraction(SPME)-GC/MS has been developed for the simultaneous analysis of plasticizers. The plasticizers investigated in this study are dimethyl phthalate(DMP), diethyl phthalate(DEP), dibutyl phthalate(DBP), benzylbutyl phthalate(BBP), diethylhexyl phthalate (DEHP), di-n-octyl phthalate(DnOP). The limit of detection(LOD) was 0.163~0.299 with relative standard deciation(RSD) of 5.85~15.80% for these compounds. At water reserviors of Han, Geum, Nakdong and Sumjin rivers, only DBPand DEHP were detected at trace level, 0.192~1.270 ng/ml for DBP and 0.077~1.102 ng/ml for DEHP depending on the river.

Identification of Volatile Essential Oil, and Flavor Characterization and Antibacterial Effect of Fractions from Houttuynia cordata Thunb -I. Identification of Volatile Essential Oil Compounds from Houttuynia cordata Thunb -I. Identification of Volatile Essential Oil Compounds from Huttuynia cordata Thunb- (어성초 휘발성 정유성분의 동정과 분획물의 향특성 및 항균활성 -I. 어성초의 휘발성 정유성분의 동정-)

  • Kang, Jung-Mi;Cha, In-Ho;Lee, Young-Kuen;Ryu, Hong-Soo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.26 no.2
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    • pp.209-213
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    • 1997
  • Since Houttuynia cordata is well known as a medicinal herb, due to its antibacterial activity on various microorganisms, present investigation was performed to identify the flavor compounds for volatile essential oil. Volatile essential oil was collected by simultaneous distillation-extraction(SDE), and then the oil components were separated on HP-5 capilliary column$(25m{\times}0.25mm\; i.d.)$ and identified those components by GC-MS. Fifty two compounds were isolated from the volatile essential oil of Houttuynia cordata and forty four were positively identified by GC-MS. The volatile compounds were composed mainly of terpenoids(25 classes), aldehydes(7 classes), alcohols(4 classes), ketones(3 classes), acids(1 class) and miscellaneous compounds(4 classes). Of these, the major compounds were ${\beta}-myrcene$, ${\beta}-ocimene$, decanal, 2-undecanone and geranyl propionate.

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Simultaneous Analysis of 17 Organophosphorous Pesticides in Blood by Automated Head Space-SPME GC/MS (HS-SPME-GC/MS에 의한 혈액중 17종 유기인계 농약의 동시분석법)

  • Rhee, Jong-Sook;Jung, Jin-Mi;Lee, Han-Sun;Yeom, Hye-Sun;Lee, Sang-Ki;Park, Yoo-Sin;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.54 no.6
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    • pp.429-440
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    • 2010
  • HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 ${\mu}m$ polyacrylate), pH effect (0.5 N HCl), salt effect ($Na_2SO_4$, 0.2 g; 20%), headspace incubation temperature ($80^{\circ}C$), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l ($r^2$=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.

Studies on the Volatile Components of Platycodon grandiflorus (jacquin) A.De Candolle (도라지의 휘발성분에 관한 연구)

  • Sun, Woo-Sun;Kwon, Jae-Sang;Shin, Pyung-Gyun;Cho, Sung-Hwan;Chung, Jin-Hwan
    • Applied Biological Chemistry
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    • v.39 no.6
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    • pp.517-520
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    • 1996
  • To identify the volatiles of Platycodon roots, the three-year-old and the 24-year-old Platycodon roots cultivated in a local farm were extracted with ethyl ether by SDE method. 54.71mg% and 80.01mg% of volatile components were collected in the three-year-old and in 24-year-old Platycodon roots, respectively. As a result of GC/MS(TIC) analysis, 24 and 28 compounds were identified, respectively; The amounts of volatile components such as hexanol, trans-2-hexenol and nonanal in 24-year-old roots were detected above ten times than those in 3-year-old roots. The Volatiles of 24-year-old roots were fractionated by SCC and identified by GC/MS to be 10 hydrocarbons, 8 alcohols, 10 aldehydes, 5 esters, 6 acids and 1 unknown compound as the major components. The species and total amounts of volatile component in 24-year-old Platycodon roots were considered to be higher than those in 3-year-old Platycodon roots. *Abbreviations 1. Platycodon : platycodon grandiflorus (jacquin) A. De Candolle. 2. SDE : Simultaneous Distillation Extraction 3. SCC : Silicagel Column Chromatography 4. GC : gas chromatography 5. GC/MS : Gas Chromatography-Mass Spectrometer 6. TIC : Total Ion Chromatogoraphy

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Food safety analytical techniques used in food industry (식품산업에서 활용되는 식품안전 분석기술의 현황)

  • Kim, Young-Jun
    • Food Science and Industry
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    • v.51 no.1
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    • pp.16-25
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    • 2018
  • Recently, the importance of analytical techniques related to food safety is emerging in the food industry due to changes in diet patterns, environmental changes, climate change and consumer's interest in food safety. In particular, food safety accidents in the food industry may cause economic losses such as media reports, product recalls, consumer distrust, and so on. Therefore, a systematic, proactive and comprehensive food safety management system is increasingly required to prevent food safety issues. Efforts to ensure the reliability of food safety are essential by introducing various analysis instruments such as LC, GC, ICP, LC/MS/MS, GC/MS/MS, ICP/MS, PCR, and RT-PCR. In addition, recent food safety analytical techniques used in food industry should be shifted paradigm by developing multi-component simultaneous analytical method, low cost with high efficient analytical method, and eco-friendly method.

Development of Analytical Technology Using the HS-SPME-GC/FID for Monitoring Aromatic Solvents in Urine

  • Lee, Mi-Young;Chung, Yun Kyung;Shin, Kyong-Sok
    • Mass Spectrometry Letters
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    • v.4 no.1
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    • pp.18-20
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    • 2013
  • Headspace solid phase micro-extraction gas chromatography/flame ionization detection (HS-SPME-GC/FID) method was compared with headspace gas chromatography/mass selective detection (HS-GC/MS). Organic solvent-spiked urine as well as urine samples from workspace was analyzed under optimal condition of each method. Detection limit of each compound by HS-SPME-GC/FID was $3.4-9.5{\mu}g/L$, which enabled trace analysis of organic solvents in urine. Linear range of each organic solvent was $10-400{\mu}g/L$, with fair correlation coefficient between 0.992 and 0.999. The detection sensitivity was 4 times better than HS-GC/MS in selected ion monitoring (SIM) mode. Accuracy and precision was confirmed using commercial reference material, with accuracy around 90% and precision less than 4.6% of coefficient of variance. Among 48 urine samples from workplace, toluene was detected from 45 samples in the range of $20-324{\mu}g/L$, but no other solvents were found. As a method for trace analysis, SPME HS GC/FID showed high sensitivity for biological monitoring of organic solvent in urine.

GC/MS analysis of volatile constituents from woody plants (목본성 식물의 휘발성 성분 GC/MS 분석)

  • Lee, Dong-Gu;Choi, Kyung;Lee, Sang-Hyun
    • Korean Journal of Agricultural Science
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    • v.38 no.4
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    • pp.723-730
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    • 2011
  • To search for the new development of industrial application of woody plants, the chemical composition of the volatile constituents from woody plants (Evodia daniellii, Clerodendron trichotomum, Prunus padus, and Zanthoxylum ailanthoides) was determined by GC and GC/MS spectrometric analysis with the aid of NBS, Wiley Library and RI indice searches. The major constituents were t-ocimene from the leaves of E. daniellii, linalool from the leaves of C. trichotomum, benzaldehyde from the leaves and twigs of P. padus, ${\beta}$-thujene from the leaves of Z. ailanthoides, and 2-undecanone from the stems of Z. ailanthoides. These results suggested that the major volatile constituents of woody plants could be a useful lead compound in the development of functional materials for industrial application.