• Title/Summary/Keyword: GC/MS/MS

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Identification of Volatile Flavor Components of Chinese chive and Baek-Seok Chie (중국 부추와 백석 부추의 휘발성 풍미 성분의 동정)

  • 이혜정;박희옥
    • The Korean Journal of Food And Nutrition
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    • v.10 no.4
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    • pp.539-543
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    • 1997
  • This study was carried out to investigate the Chinese and Baek-Seok chive. We collect the volatile components of Chinese and Baek-Seok chive by dynamic head space method. Chinese chive was analyzed by Gas chromatography-Mass Spectrometry(GC-MS). 28 components including 20 sulfides, 5 alcohols, 1 benzene and 2 aldehydes compounds were identified in samples, Also Baek-Seok chive was analyzed by GC-MS. 32 components including 19 sulfides, 10 alcohols, 2 benzonoides and 1 aldehyde compounds were confirmed.

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Occurrence of Castasterone, Brassinolide and Methyl 4-Chloroindole-3-acetate in Immature Vicia faba Seeds (잠두(Vicia faba L)가 생산하는 Brassinosteroid 활성물질)

  • Park, Keun-Hyung
    • Applied Biological Chemistry
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    • v.31 no.1
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    • pp.106-113
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    • 1988
  • The rice lamina inclination test indicated the presence of brassinosteroid-like active substances in immature Vicia faba seeds. Two of these were identified as castasterone and brassinolide by GC/MS and GC/SIM, respectively. Another active principle was identified as methyl 4-chloroindole-3-acetate by GC/MS and HPLC.

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Determination of N. N-dimethylaniline in penicillins by GC-MS

  • Choi, Jung-Kap;Park, Man-Ki
    • Archives of Pharmacal Research
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    • v.4 no.2
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    • pp.85-90
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    • 1981
  • A quantitative GC-MS spectrometric assay was used for the determination of residual N, N-dimethylaniline as a contaminant in commercial penicillin derivatives from various sources. The assay utilizes selective ion focusing to monitor in a GC effluent the molecular ions of DMA generated by electron impact ionization. This method includes dissolution of the sample in alkaline solution, extraction of organic base with cyclohexane and injection into GC-MS with a 3% OV-17 column. Levels of 50 ppb of DMA were easily measured with a coeffecient of varation less than 5 % and recoveries from spiked samples exceeded 97 %. The results of the determinations of DMA in various commercial penicillins were relatively free of this contaminant.

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Composition of volatile organic components on ballpoint pen inks by HS-SPME GC/MS (HS-SPME GC/MS를 이용한 볼펜잉크의 휘발성 성분 분석)

  • Choi, Mi-Jung;Kim, Chang-Seong;Sun, Yale-Shik;Park, Sung-Woo
    • Analytical Science and Technology
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    • v.23 no.4
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    • pp.414-422
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    • 2010
  • In forensic examinations of question document, analysis about inks components and the dating of ink entries is often of considerable importance and forensic examination of inks is principally concerned with the classification and comparison of chemically complex mixtures. The authenticity about inks analysis of a questioned document may be examined through the analysis of inks used to TLC, HPLC/MS, GC/MS, LDI/MS. We collected 56 difference types of black ballpoint pen inks manufactured from 5 country groups. We identified major 6 species volatile organic components (VOCs), ethylbenzene ($0.089-0.244\;{\mu}g$/mL), o-xylene ($0.072-0.331\;{\mu}g$/mL), m,p-xylene ($0.062-0.318\;{\mu}g$/mL), benzene ($0.003-0.173\;{\mu}g$/mL), 1,1-dichloroethylene ($0.003-0.295\;{\mu}g$/mL), toluene ($0.007-0.484\;{\mu}g$/mL) using HS-SPME GC/MS. The results of this study indicated that determined VOCs of black ballpoint pen inks could make a discriminating tool of inks analysis for forensic question document and can supply methodology for classification and identification of between ballpoints pen inks.

Flavor Components of Poncirus trifoliata (탱자(Poncirus trifoliata)의 향기성분 분석에 관한 연구)

  • Oh, Chang-Hwan;Kim, Jung-Han;Kim, Kyoung-Rae;Ahn, Hey-Joon
    • Korean Journal of Food Science and Technology
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    • v.21 no.6
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    • pp.749-754
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    • 1989
  • The essential oil was prepared by a gas co-distillation method from flavedo of Poncirus trifoliata and was analyzed by GC/ retention index (RI) and GC/MS. The essential oil prepared by a gas co-distillation gave a whole fragrance of Poncirus trifoliata. The identification of the flavor components was performed by multi-dimensional analysis using GC/RI and GC/MS. GC/RI and GC/MS were complementary to each other. In applying GC/RI for identification, it was more effective when two columns of different polarities were used. Thirty volatile flavor constituents were identified in Poncirus trifoliata. Limonene, myrcene, ${\beta}-caryophyllene,\;trans-{\beta}-ocimene$, ${\beta}-pinene$, 3-thujene and 7-geranyloxycoumarin were the major constituents and cis-3-hexenyl acetate, n-hexyl acetate, 2-methyl acetophenone, elixene and elemicine had not been reported earlier as citrus components.

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Identification of Lignan Compounds in Fruits of Schisandra chinensis BAILLON by Gas Chromatography/Mass Spectrometry (GC/MS에 의한 오미자 Lignan성분의 동정)

  • Sohn, Hyun-Joo;Bock, Jin-Young
    • Applied Biological Chemistry
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    • v.32 no.4
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    • pp.344-349
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    • 1989
  • Eleven lignan compounds in fruits of Schisandra chinensis BAILLON were identified by gas chromatography/mass spectrometry(GC/MS). The GC/MS conditions were as followed: the GC column used was SPB-1 fused silica capillary $(0.25mm\;id{\times}30m,Supelco)$ and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute; the MS ionization voltage was 70eV (EI mode). The compounds identified were gomisin J $(M^+;\;388)$, deoxyschizandrin$(M^+;\;416)$, gomisin N $(M^+;\;400)$, schizandrin$(M^+;\;432)$, wuweizisu C $(M^+;\;384)$, gomisin A $(M^+;\;416)$, angeloylgomisin H $(M^+;\;500)$, tigloylgomisin H $(M^+;\;500)$, angeloylgomisin Q $(M^+;\;530)$, gomisin B $(M^+;\;514)$ and benzoylgomisin H $(M^+;\;522)$, peaks of which were separated well on the GC chromatogram.

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Comparative GC-MS Based In vitro Assays of 5α-Reductase Activity Using Rat Liver S9 Fraction

  • Lee, Su-Hyeon;Lee, Dong-Hyoung;Lee, Jeong-Ae;Lee, Won-Yong;Chung, Bong-Chul;Choi, Man-Ho
    • Mass Spectrometry Letters
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    • v.3 no.1
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    • pp.21-24
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    • 2012
  • $5{\alpha}$-Dihydrotestosterone (DHT) is the primary active metabolite of testosterone, catalyzed by $5{\alpha}$-reductase ($5{\alpha}R$) in the skin, prostate, and liver. In this study, the $5{\alpha}R$ activity in rat liver S9 fraction in the presence of a NADPH-generating system was evaluated and compared by gas chromatography-mass spectrometry (GC-MS)-based in vitro assays. Testosterone and a $5{\alpha}R$ inhibitor, finasteride, were added to the S9 fractions and incubated at $37^{\circ}C$ for 1 h. Both testosterone and DHT were quantitatively measured and compared with two different GC-MS-based steroid profiling techniques. DHT was not detected by conventional GC-MS analysis in the absence of finasteride when the concentration of testosterone in the S9 fraction was less than $0.2{\mu}M$, whereas the isotope-dilution GC-MS (GC-IDMS) system was able to evaluate the $5{\alpha}R$ activity. Because the S9 fraction contains more reactive enzymes and is easier to collect from tissues compared with a microsomal solution, the combination of the S9 fraction and GC-IDMS technique may be a promising assay for evaluating the $5{\alpha}R$ activity in large-scale clinical studies.

Removal of residual VOCs in a collection chamber using decompression for analysis of large volatile sample

  • Lee, In-Ho;Byun, Chang Kyu;Eum, Chul Hun;Kim, Taewook;Lee, Sam-Keun
    • Analytical Science and Technology
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    • v.34 no.1
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    • pp.23-35
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    • 2021
  • In order to measure the volatile organic compounds (VOCs) of a sample which is too large to use commercially available chamber, a stainless steel vacuum chamber (VC) (with an internal diameter of 205 mm and a height of 50 mm) was manufactured and the temperature of the chamber was controlled using an oven. After concentrating the volatiles of the sample in the chamber by helium gas, it was made possible to remove residual volatile substances present in the chamber under reduced pressure ((2 ± 1) × 10-2 mmHg). The chamber was connected to a purge & trap (P&T) using a 6 port valve to concentrate the VOCs, which were analyzed by gas chromatography-mass spectrometry (GC-MS) after thermal desorption (VC-P&T-GC-MS). Using toluene, the toluene recovery rate of this device was 85 ± 2 %, reproducibility was 5 ± 2 %, and the detection limit was 0.01 ng L-1. The method of removing VOCs remaining in the chamber with helium and the method of removing those with reduced pressure was compared using Korean drinking water regulation (KDWR) VOC Mix A (5 μL of 100 ㎍ mL-1) and butylated hydroxytoluene (BHT, 2 μL of 500 ㎍ mL-1). In case of using helium, which requires a large amount of gas and time, reduced pressure ((2 ± 1) × 10-2 mmHg) only during the GC-MS running time, could remove VOCs and BHT to less than 0.1 % of the original injection concentration. As a result of analyzing volatile substances using VC-P&T-GC-MS of six types of cell phone case, BHT was detected in four types and quantitatively analyzed. Maintaining the chamber at reduced pressure during the GC-MS analysis time eliminated memory effect and did not affect the next sample analysis. The volatile substances in a cell phone case were also analyzed by dynamic headspace (HT3) and GC-MS, and the results of the analysis were compared with those of VC-P&T-GC-MS. Considering the chamber volume and sample weight, the VC-P&T configuration was able to collect volatile substances more efficiently than the HT3. The VC-P&T-GC-MS system is believed to be useful for VOCs measurement of inhomogeneous large sample or devices used inside clean rooms.

Simultaneous GC/MS Analyses of Organic acids and Amino acids in Urine using TMS-TFA derivative (TMS-TFA 유도체화를 이용한 소변여지 중 유기산과 아미노산의 GC/MS 동시분석)

  • Yoon, Hye-Ran
    • Analytical Science and Technology
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    • v.19 no.1
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    • pp.107-114
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    • 2006
  • Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

Evaluation of TVOC contribution from Raw materials of PVC wallpaper using the Headspace-SPME-GC/MS (HS-SPME-GC/MS 법을 이용한 PVC벽지 원자재의 TVOC 기여도 평가)

  • Jang, Mi-Ok;Jeong, Tak-Kyo;Jeong, Yung-Rim;Kim, Man-Goo
    • Analytical Science and Technology
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    • v.20 no.6
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    • pp.488-495
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    • 2007
  • A wallpaper having many surfaces in indoor is composed of various raw materials. In this study, TVOC contribution from raw materials of PVC wallpaper was evaluated by using headspace-solid phase microextraction (HS-SPME)-GC/MS. Samples were diluent, resin stabilizer, plasticizer, filler, blowing agent and PVC resin. 9 mL of each sample was put into 22 mL glass vial and they were equilibrated for 1 hour at $100^{\circ}C$. Headspace in vial was absorbed to $75{\mu}m$ Carboxen-PDMS fiber and analyzed by GC/MS. Aromatic compounds like a toluene, ethylbenzene and xylene, ketones compounds like a acetone, methoxyacetone and 2-butanone and alkane compounds like a nonane decane and undecane were identified from raw materials. And alcohol compounds like a ethanol and butanol and aldehydes were detected. TVOC emission of diluent, resin stabilizer, plasticizer, PVC resin, blowing agent and filler were $54.20{\mu}g/g$, $32.88{\mu}g/g$, $0.50{\mu}g/g$, $0.88{\mu}g/g$, $0.22{\mu}g/g$ and $0.11{\mu}g/g$, respectively. Contribution of TVOC emission of diluent, resin stabilizer and PVC resin that were concerned about add ratio were 0.708, 0.129, 0.115, respectively. In conclusion, it's necessary to reduce TVOC emission through improvement of diluent, resin stabilizer and PVC resin. Also, HS-SPME-GC/MS method which was developed in this study will be used for raw materials analysis effectively.