• Title/Summary/Keyword: GC/MS/MS

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Determination of Miliacin from Proso Millet Oil by GC/MS (GC/MS를 이용한 기장 기름의 밀리아신 함량 분석)

  • Yeon Ju An;Byeong Won Lee;Ji Ho Chu;Seok Bo Song;Ji Young Kim;Young Kwang Ju;Sang Ik Han
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.67 no.4
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    • pp.335-341
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    • 2022
  • Proso millet (Pacnicum miliaceum L.) has a various of functional substances, so the demand is increasing as interest in human health benefits. In particular, miliacin, a triterpenoid in proso millet, is known to be effective in hair loss due to its promoting metabolism and proliferation of keratinocytes and showing protective effects from apoptosis. In this study, proso millet oil was extracted and analyzed by GC/MS using the extraction method of unsaponifiable substances after saponification reaction. The components of proso millet oil were confirmed through qualitative analysis by GC/MS. The miliacin content of 5 varieties of proso millet and 2 varieties of foxtail for comparison was analyzed. In the result, components of pentacyclic triterpenes such as β-amyrine and lupeol were detected in proso millet, and the content of miliacin was highest in Hallachal at 370.38±0.04 ㎍/100 mg oil. In addition, the content of miliacin was not detected in Samdachal and Samdamae, which are varieties of foxtail millet.

Determination of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) in human urine by solid-phase extraction and GC/MS (고체상 추출과 GC/MS를 이용한 소변 중 대마 대사체 (THCCOOH) 분석)

  • Cheong, Jae Chul;Kim, Jin Young;In, Moon Kyo;Cheong, Won Jo
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.441-448
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    • 2006
  • 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH) is the major metabolite of tetrahydrocannabinol (THC) which is the primary psychoactive component of marijuana. It is also the target analyte for the discrimination marijuana use. A method using solid-phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) was developed for the determination of THCCOOH in human urine. Urine samples (3 mL) were extracted by SPE column with a cation exchange cartridge after basic hydrolysis. The eluents were then evaporated, derivatized, and injected into the GC/MS. The limits of detection (LOD) and quantitation (LOQ) were 0.4 and 1.2 ng/mL, respectively. The response was linear with a correlation coefficient of 0.999 within the concentration range of 1.2 (LLE 1.3)~50.0 ng/mL. The precision and accuracy were stable within 1.20% and the recovery was 83.6~90.7%. The recovery of SPE method was lower than that of liquid-liquid extraction (LLE), but there were no apparent differences in LOD, LOQ, precision and accuracy between the two methods. While SPE method is used as a very effective and rapid procedure for sample pretreatment, and clean extracts, LLE method was not suitable for the extraction procedure of THCCOOH in urine. The applicability of the method was proven by analyzing a urine samples from a marijuana abusers.

Primary study of sterols composition of Rhodiola sachalinensis by using GC/MS (GC/MS를 이용한 고산 홍경천의 스테롤 구성에 대한 초기연구)

  • Jin, Yinzhe;Li, Xifeng;Li, Donghao;Row, Kyung Ho
    • Analytical Science and Technology
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    • v.22 no.3
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    • pp.219-227
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    • 2009
  • The steroid compounds in Rhodiola sachalinensis were determined with adsorption column chromatographic purification and GC/MS. Sterols were extracted by sonication and Soxhlet with ethanol and dichloromethane, respectively. The extract was partitioned with chloroform and water using liquid-liquid extraction, and purified with a silica column after the sterols had been converted to the corresponding silyl derivatives with BSTFA. Eighteen free sterols, including $\beta$-sitosterol, stigmasterol and cycloartenol, and nine sterol conjugates were found from Rhodiola sachalinensis by GC/MS. Among them, cholest-5-ene-3-ol, cholesterol, stigmasterol, $\beta$-sitosterol were confirmed and quantified with sterol standards. Most sterols were presented in the chloroform part, with $C_{29}$ being the most abundant group in this sterol group. $\beta$-sitosterol was the most abundant compound with a relative content of 45.94% followed by ergost-7-ene-3-ol (11.33%), 4,14-dimethyl-ergosta-8,24(28)-diene-3-ol (7.07%), stigmasterol (6.09%), cycloartenol (5.43%) and 4-methyl-cholest-5-ene-3-ol (5.39%).

Comparative Analyses of the Flavors from Hallabong (Citrus sphaerocarpa) with Lemon, Orange and Grapefruit by SPTE and HS-SPME Combined with GC-MS

  • Yoo, Zoo-Won;Kim, Nam-Sun;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.25 no.2
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    • pp.271-279
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    • 2004
  • The aroma component of Hallabong peel has been characterized by GC-MS with two different extraction techniques: solid-phase trapping solvent extraction (SPTE) and headspace solid-phase microextraction (HSSPME). Aroma components emitted from Hallabong peel were compared with those of other citrus varieties: lemon, orange and grapefruit by SPTE and GC-MS. d-Limonene (96.98%) in Hallabong was the main component, and relatively higher peaks of cis- ${\beta}$-ocimene, valencene and -farnesene were observed. Other volatile aromas, such as sabinene, isothujol and ${\delta}$-elemene were observed as small peaks. Also, principal components analysis was employed to distinguish citrus aromas based on their chromatographic data. For HSSPME, the fiber efficiency was evaluated by comparing the partition coefficient ($K_{gs}$Kgs) between the HS gaseous phase and HS-SPME fiber coating, and the relative concentration factors (CF) of the five characteristic compounds of the four citrus varieties. 50/30 ${\mu}$m DVB/CAR/PDMS fiber was verified as the best choice among the four fibers evaluated for all the samples.

GC/MS Determination of Monosaccharides in Yoqurt Products (GC/MS 법에 의한 요쿠르트 제품의 구성 단당류의 조성 비교분석에 관한 연구)

  • Nam, Sang-Kyu;Cheong, Won-Jo
    • Journal of the Korean Chemical Society
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    • v.44 no.1
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    • pp.24-29
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    • 2000
  • Yoqurt products are known to be effective for enhancing health and preventing diseases such as cancers. Such effects are generally believed to be due to actions of polysacchmides in yoqurt products. In this study we have determined compositions of monosaccharides in hydrolysates of commercial yoqrtrt products as the first step of understanding structures of polysaccharides. The yoqtrrt products were ttltracentrifuged, filtered, hydrolyzed in 1M sulfuric acid and neutralized. A portion of the solution was taken and evaporated to dryness, denvatized with TMSI (trimethly- silylimidazole) and analyzed by GC/MS. We found that the monosaccharides were fructose, glucose, and galactose. Their compositions were variant among several yoqtrrt products.

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Quantitative Analysis of Ethyl Carbamate in Korean Alcoholic Beverages by Chromatography with Mass Selective Detection (GC/MS 를 이용한 한국 주류 중의 Ethyl Carbamate 정량)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.15 no.1
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    • pp.26-30
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    • 2002
  • In order to determine the contents of ethyl carbamate in Korean traditional alcoholic beverages and general beverages, GC/MS-SIM method was used after extraction of beverages with dichloromethane. The contents of ethyl carbamate in Korean traditional alcoholic beverages, non-distilled alcohol, and whisky were detected in the range of $4.6-50.2{\mu}g/L$, $27.8-45.4{\mu}g/L$, and $24.8-55.1{\mu}g/L$, respectively. The recoveries were ranged from 83.3 to 104.8 %. The values of relative standard deviation were ranged from 1.8 to 14.8 % and the detection limit was $0.3{\mu}g/L$.

Determination of agrochemical residues in tobacco using matrix solid-phase dispersion and GC/MS

  • Lee, Jeong-Min;Min, Hye-Jeong;Park, Jin-Won;Lee, Moon-Young;Jang, Gi-Chul
    • Journal of the Korean Society of Tobacco Science
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    • v.36 no.1
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    • pp.12-19
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    • 2014
  • A matrix solid-phase dispersion (MSPD) method was developed for extracting and cleaning-up the selected agrochemicals in tobacco using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS-SIM). Different parameters of the method were investigated and optimized, such as the type of solid-phase (alumina, $C_{18}$ and Florisil) and eluent (acetone, acetonitrile, ethylacetate and n-hexane). The best results were obtained using 0.5 g of tobacco sample, 1.0 g of $C_{18}$ as dispersant sorbent, 1.0 g of Florisil as clean-up sorbent and acetonitile saturated with n-hexane as eluting solvent. The method was validated using tobacco samples fortified with agrochemicals at their different concentration levels. This method gave good linearity for the selected agrochemicals of ranging from $0.01{\mu}g/mL$ to $0.1{\mu}g/mL$. Recoveries of the selected agrochemicals in tobacco were more than 80 % and reproducibilities were found to be better than 10 % RSD. Those results suggested that the analytical procedure including MSPD method in combining with GC/MS could be applicable to the rapid determination often the selected agrochemicals in tobacco.

Changes of Flavor Components in Chewing Gum during Storage by Gas Chromatography/Mass Spectrometry (GC/MS에 의한 저장중 츄잉껌 향기성분 변화연구)

  • Shin, Seong-Kee;Kim, Sang-Ho;Lee, Yoon-Hyung;Rhee, Kyu-Soon
    • Korean Journal of Food Science and Technology
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    • v.24 no.1
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    • pp.25-28
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    • 1992
  • The changes of amount in flavor components of chewing gum during storage of various relative humidity were studied by GC/MS. The volatile components in chewing gum were extracted by sample preperation and 15 volatile components were identified by NIST/NBS library searching. According to the period of storage, quantities of major volatile components extracted by tetrahydrofuran-methanol solutions were determined by using tetradecane as internal standard. Until 4 weeks, comparing with starting peak area ratio, the decrease of chewing gum flavor components were rapid at 33, 75 than 53 R.H(%). And after 16 weeks, amount of chewing gum flavor at all storage conditions similarly decreased to $45{\sim}49%$ of the initial amount.

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Butyrylcholinesterase Inhibitory Activity and GC-MS Analysis of Carica papaya Leaves

  • Khaw, Kooi-Yeong;Chear, Nelson Jeng Yeou;Maran, Sathiya;Yeong, Keng Yoon;Ong, Yong Sze;Goh, Bey Hing
    • Natural Product Sciences
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    • v.26 no.2
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    • pp.165-170
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    • 2020
  • Carica papaya is a medicinal and fruit plant owing biological activities including antioxidant, antiviral, antibacterial and anticancer. The present study aims to investigate the acetyl (AChE) and butyryl (BChE) cholinesterase inhibitory potentials of C. papaya extracts as well as their chemical compositions. The chemical composition of the active extract was identified using a gas chromatography-mass spectrometry (GC-MS). Ellman enzyme inhibition assay showed that the alkaloid-enriched leaf extract of C. papaya possessed significant anti-BChE activity with an enzyme inhibition of 75.9%. GC-MS analysis showed that the alkaloid extract composed mainly the carpaine (64.9%) - a major papaya alkaloid, and some minor constituents such as aliphatic hydrocarbons, terpenes and phenolics. Molecular docking of carpaine revealed that this molecule formed hydrogen bond and hydrophobic interactions with choline binding site and acyl pocket. This study provides some preliminary findings on the potential use of C. papaya leaf as an herbal supplement for the prevention and treatment of Alzheimer's disease.

Determination of Volatile Organic Compounds (VOCs) Using Tedlar Bag/Solid-phase Microextraction/Gas Chromatography/Mass Spectrometry (SPME/GC/MS) in Ambient and Workplace Air

  • Lee, Jae-Hwan;Hwang, Seung-Man;Lee, Dai-Woon;Heo, Gwi-Suk
    • Bulletin of the Korean Chemical Society
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    • v.23 no.3
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    • pp.488-496
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    • 2002
  • SPME techniques have proven to be very useful tools in the analysis of wide VOCs in the air. In this study, we estimated VOCs in ambient and workplace air using a Tedlar ba /SPME/GC/MS system. The calibration curve was set to be linear over the range of 1-30 ppbv. The detection limits ranged from 10 pptv to 0.93 ppbv for all VOCs. Reproducibility of TO-14 target gas mixtures by SPME/GC/MS averaged at 8.8 R.S.D (%). Air toxic VOCs (hazardous air pollutants, HAPs) containing a total of forty halohydrocarbons, aromatics, and haloaro-matic carbons could be analyzed with significant accuracy, detection limit and linearity at low ppbv level. Only reactive VOCs with low molecular weight, such as chloromethane, vinylchloride, ethylchloride and 1,2-dichloro-ethane, yielded relatively poor results using this technique. In ambient air samples, ten VOCs were identified and quantified after external calibration. VOC concentration in ambient and workplace air ranged from 0.04 to 1.85 ppbv. The overall process was successfully applied to identify and quantify VOCs in ambient/workplace air.