• Title/Summary/Keyword: GC and GC-MS method

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Analysis of Asarone, Coumarin and Thujone in Medicinal Plants Used in Brewing a Korean Traditional Folk Wine (민속주 부재료로 이용되는 식물성 방향재료 및 약용재료중의 Asarone, Coumarin, Thujone의 분석)

  • Jo, Jung-Ok;Kim, Sun-Min;Kim, Kyong-Su
    • Applied Biological Chemistry
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    • v.42 no.3
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    • pp.210-217
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    • 1999
  • To detect the toxic relevant components, asarone, coumarin and thujone, in the 87 medicinal plants used in brewing a Korean traditional folk wine, their 20% ethanol extracts were prepared and purified by a SPE(solid phase extraction) method. The toxic components in the purified extracts were identified by GC-FID and GC/MS analysis. On analyses, asarone was detected in 6 species, Acorus gramineus Solander, Acorus asiaticus Nakai, Angelia gigus Nakai, Santalum album, etc.; coumarin in 22 species, Anethum graveolens, Foeniculum vulgare Gaertner, Lithosperum erythrorhizon Siebold et Zuccarinii, etc.; thujone in 24 species, Achyranthes japonica Nakai, Amomum xanthiodes Wallich, Artemisia asiatia Nakai, seed of Cannabis sativa L., Caragana sinica R., Chrysanthemum morifolium Ramat, Codonopsis lanceolata Bentham et flooker, Foeniculum vulgare Gaertner, etc.

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Anaerobic Biodegradation of Lignin by BMP Test and Measurement of Lignin-derived Compound Using GC & GC/MS (BMP법에 의한 리그닌의 혐기성 분해 및 GC와 GC/MS을 이용한 리그닌 분해산물 측정)

  • Kim, Seog-Ku
    • Journal of the Korea Organic Resources Recycling Association
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    • v.16 no.3
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    • pp.46-51
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    • 2008
  • The traditional view of the fate of lignin under anaerobic conditions is that it is recalcitrant because molecular oxygen is required for depolymerization. The presence of lignin is apparently the most important factor affecting the biodegradability of ligneous materials. The initial step in the degradation of ligneous material to smaller intermediates is catalyzed by enzymes secreted by microorganisms and is generally regarded as the rate limiting step in the microbial mineralization of organic matter. Biochemical methane potential (BMP) test, typically used to assess anaerobic biodegradability of liquid wastes with added nutrients and bacteria, have been adapted to assess initial biodegradation of ligneous material under anaerobic conditions. A method based on selective inhibition of microorganism activity, by 3% toluene, has been used to measure using the initial degradation rate of ligneous material and the accumulation of lignin-derived compounds.

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Poly(dimethylsiloxane) Mini-disk Extraction

  • Cha, Eun-Ju;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.32 no.10
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    • pp.3603-3609
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    • 2011
  • A novel sampling method of the headspace poly(dimethylsiloxane) (PDMS) mini-disk extraction (HS-PDE) was developed, optimized, validated and applied for the GC/MS analysis of spices flavors. A prototype PDMS mini-disk (8 mm outer diameter, 0.157 mm thickness, 9.4 mg weight) has been designed and fabricated as a sorption device. The technique uses a small PDMS mini-disk and very small volume of organic solvent and less sample size than the solvent extraction. This new HS-PDE method is very simple to use, inexpensive, rapid, requires less labor. Linearities of calibration curves for ${\alpha}$-pinene, ${\beta}$-pinene, limonene and ${\gamma}$-terpinene by HS-PDE combined with GC/MS were excellent having $r^2$ values greater than 0.99 at the dynamic range of 6.06~3500 ng/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) showed very low values. This method exhibited good precision and accuracy. The overall extraction efficiency of this method was evaluated by using partition coefficients ($K_p$) and concentration factors (CF) for several characteristic components from nutmeg and mace. Partition coefficients were in the range from $2.04{\times}10^4$ to $4.42{\times}10^5$, while CF values were 0.88-15.03. HS-PDE was applied successfully for the analysis of flavors compositions from nutmeg, mace and cumin. The HS-PDE method is a very promising sampling technique for the characterization of volatile flavors.

Studies on the Terpenoids in the Volatile Constituents of Liaoning Schisandra Chinensis Baillon

  • Hou, Dongyan;Zhang, Weihua;Hui, Ruihua
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.505-509
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    • 1995
  • The terpenoids in the volatile constituents of Liaoning Shcisandra Chinesis Baillon have been determined by the analytical method of GC/MS. Thirty terpenoids molecular structure were characterized. They are 11.89% monterpenes, 4.60% monoterpene oxides, 58.74% sesquiterpene hydrocarbons, and 1.62% oxygen-containing sesquiterpenoids in the total volatile constituents quantified by chromatograph. Among them, the sesquiterpene make up the characteristic constituents. Every terpenoid constituent percent content was obtained using area normalization method of HP-59970 chemstation.

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Optimization of Analytical Methods for Octacosanol in Related Health-functional Foods with GC-MS (GC-MS를 이용한 건강기능식품 중 옥타코사놀 분석법 개발 연구)

  • Lee, Jin Hee;Oh, Mi Hyune;Lee, Kyung Jin;Kim, Yang Sun;Keum, Eun Hee;Park, Ji Eun;Cho, Mee Hyun;Seong, Min Hye;Kim, Sang A;Kim, Mee hye
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.266-271
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    • 2018
  • The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health-functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we continue our research on developing analytical methods for the items. Octacosanol is the major component of polycosanol and is a high-molecular-mass primary fatty alcohol, obtained from sugar cane wax. Previous researchers have shown that octacosanol can lower cholesterol and has antiaggregatory properties, cytoprotective uses, and ergogenic properties for human health. Recently, octacosanol products have been actively introduced into the domestic market because of their functional biological activity. We have developed a sensitive and selective test method for octacosanol that the TMS derivatives by means of gas-chromatographic-tandem mass spectrometry (GC-MS). The trimethylsilyl ether derivative of the target analyte showed excellent chromatographic properties. The procedure was validated in the range of $12.5{\sim}200{\mu}g/L$. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.999, and the limits of detection (LOD) and limits of quantitation (LOQ) were $4.5{\mu}g/L$ and $13.8{\mu}g/L$, respectively. The high recoveries (92.5 to 108.8%) and precision (1.8 to 2.4%) obtained are in accordance with the established validation criteria. Our research can provide scientific evidence to amend the octacosanol test method for the Health-Functional Food Code.

Effective determination of nicotine enantiomers from e-liquids and biological fluids by high performance liquid chromatography (HPLC) using dispersive liquid-liquid microextraction (DLLME)

  • Song, Seunghoon;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.34 no.4
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    • pp.180-190
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    • 2021
  • This study compared the efficacy of chiral GC and chiral HPLC for the analysis of nicotine. To develop a suitable dispersive liquid-liquid microextraction (DLLME) method, the following parameters were optimized: pH, extraction solvent, dispersive solvent, type and quantity of salt, and laboratory temperature. The validation of the method was carried out by the established HPLC method. The LODs were 0.11 ㎍/mL and 0.17 ㎍/mL for the (S)- and (R)- enantiomers, respectively. The LOQs were 0.30 ㎍/mL and 0.44 ㎍/mL, respectively. The optimal calibration range was between 0.30-18 ㎍/mL and 0.44-4.40 ㎍/mL, respectively, and the correlation coefficient (r2) was 0.9978-0.9996. The intra-day accuracy was 79.9-110.6 %, and the intra-day precision was 1.3-12.0 %. The inter-day accuracy was 87.8-108.0 %, and the inter-day precision was 4.0-12.8 %. E-liquid and biological fluids (urine and saliva) were analyzed using the established method.

A Study on 10 Metabolites Separated from DNA Adduce of Blood Lymphocytes in Rats Exposed Orally with 3,3-dichlorobenzidine(DCB) by GC/MS-SIM

  • Shin, Ueon-Sang;Lee, Jin-Heon
    • Journal of Environmental Health Sciences
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    • v.28 no.4
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    • pp.6-11
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    • 2002
  • 3.3'-Dichlorobenzidine(DCB) has be shown carcinogenic in several animals, and the development of non-invasive biomonitoring method in workers exposed with it is a very important subject. DNA adduct is a good biomarker for biomonitoring about carcinogens exposure, and lymphocytes is a good non-invasive samples. So we studied to analyze metabolites in blood lymphocytes of female Sprague-Dawley rats exposed orally with DCB(20, 30, and 40 mg/kg wt.) for 3 weeks. For analysis of them, we isolated DNA adducts from blood lymphocytes by using the enzymes method in /sup 32/P-postlabeling, and measured them by using gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM). 4-aminobiphenyl and phenanthrene-d/sub 10/ were added as internal standard for blank sample. Standard metabolites of DCB were synthesized with using pyridine and acetic acid which were promoter and controller in acetylation of DCB. And they were used for calibration curve. Our results showed two kinds of metabolites in DNA adducts of blood lymphocytes. They were N-acetyl 3,3'-dichlorobenzidine(acDCB) and N,N'-diacetyl 3,3'-dichiorobenzidine(di-acDCB ). They were combined with DNA at the same time as an acetyl of it was removed. So we measured DCB and acDCB for two kinds of metabolites in DNA adducts of blood lymphocytes. Our results showed the levels of DCB were 1.46∼2.26 times more than that of acDCB. And also the levels of metabolites in 20, 30 and 40 mg/kg wt. were gradually increased with going days from 1st to 3rd week. They are 1.66, 1.38 and 0.90 times in total metabolites, 1.76, 1.49 and 1.02 times in DCB, and 1.51, 1.22 and 1.28 times in acDCB. In conclusion, the results of this study showed DCB exposed to rats formed DNA adduct in blood lymphocytes after acetylated to N-acetyl 3.3'-dichloro benzidine(acDCB) and N,N'-diacetyl 3,3'-dichlorobenzidine(di-acDCB), and they could be analyzed by us ing gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM).

In situ isolation and characterization of the biosurfactants of B. Subtilis

  • Akthar, Wasim S.;Aadham, Mohamed Sheik;Nisha, Arif S.
    • Advances in environmental research
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    • v.9 no.3
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    • pp.215-232
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    • 2020
  • Crude oils are essential source of energy. It is majorly found in geographical locations beneath the earth's surface and crude oil is the main factor for the economic developments in the world. Natural crude oil contains unrefined petroleum composed of hydrocarbons of various molecular weights and it contains other organic materials like aromatic compounds, sulphur compounds, and many other organic compounds. These hydrocarbons are rapidly getting degraded by biosurfactant producing microorganisms. The present study deals with the isolation, purification, and characterization of biosurfactant producing microorganism from oil-contaminated soil. The ability of the microorganism producing biosurfactant was investigated by well diffusion method, drop collapse test, emulsification test, oil displacement activity, and blue agar plate method. The isolate obtained from the oil contaminated soil was identified as Bacillus subtilis. The identification was done by microscopic examinations and further characterization was done by Biochemical tests and 16SrRNA gene sequencing. Purification of the biosurfactant was performed by simple liquid-liquid extraction, and characterization of extracted biosurfactants was done using Fourier transform infrared spectroscopy (FTIR). The degradation of crude oil upon treatment with the partially purified biosurfactant was analyzed by FTIR spectroscopy and Gas-chromatography mass spectroscopy (GC-MS).

Analysis of Mineral and Volatile Flavor Compounds in Pimpinella brachycarpa N. by ICP-AES and SDE, HS-SPME-GC/MS (ICP-AES와 SDE, HS-SPME-GC/MS를 이용한 참나물의 무기성분과 향기성분)

  • Chang, Kyung-Mi;Chung, Mi-Sook;Kim, Mi-Kyung;Kim, Gun-Hee
    • Journal of the Korean Society of Food Culture
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    • v.22 no.2
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    • pp.246-253
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    • 2007
  • Mineral and volatile flavor compounds of Pimpinella brochycarpa N., a perennial Korean medicinal plant of the Umbelliferae family, were analyzed by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and simultaneous steam distillation extract (SDE)-gas chromatography mass spectrometry (GC/MS), head space solid phase micro-extraction (HS-SPME)-GC/MS. Mineral contents of the stalks and leaves were compared and the flavor patterns of the fresh and the shady air-dried samples were obtained by the electronic nose (EN) with 6 metal oxide sensors. Principal component analysis (PCA) was carried out using the data obtained from EN. The 1st principal values of the fresh samples have + values and the shady air-dried have - values. The essential oil extracted from the fresh and the shady air-dried by SDE method contain 58 and 31 flavor compounds. When HS-SPME method with CAR/PDMS fiber and PDMS fiber were used, 34 and 21 flavor compounds. The principal volatile components of Pimpinella brachycarpa N. were ${\alpha}$-selinene, germacrene D, and myrcene.

Development and validation of an analytical method for the quantification of 2,6-diisopropylnaphthalene in agricultural products using GC-MS/MS

  • Lee, Han Sol;Park, Ji-Su;Lee, Su Jung;Shin, Hye-Sun;Chung, Yun mi;Choi, Ha na;Yun, Sang Soon;Jung, Yong-hyun;Oh, Jae-Ho
    • Analytical Science and Technology
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    • v.34 no.1
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    • pp.1-8
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    • 2021
  • An analytical method was developed and optimized for the quantification of a plant growth regulator, 2,6-diisopropylnaphthalene (2,6-DIPN), in agricultural products using gas chromatography-tandem mass spectrometry. The samples were extracted, partitioned, and were purified using a Florisil® cartridge. To validate the analytical method, its specificity, linearity, limit of detection (LOD) and limit of quantification (LOQ) of the instrument, LOQ of the analytical method (MLOQ), accuracy, and repeatability were considered. The method displayed excellent results during validation, and is suitable for the determination and quantification of the low residual levels of the analyte in the agricultural samples. All of the results with the optimized method were satisfactory and within the criteria ranges requested in the Codex Alimentarius Commission guidelines and the Ministry of Food and Drug Safety guidelines for pesticide residue analysis. The developed method is simple and accurate and can be used as a basis for safety management of 2,6-DIPN.