• Title/Summary/Keyword: (GC-MS) gas chromatography-mass spectrometry analysis

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Analysis of the essential oil composition of fresh Panax ginseng root and identification of novel phenylalkenal compounds

  • Dae-Woon Kim;Young-Hoi Kim;Tae-Young Kim;Han-Suk Choi;Myung-Kon Kim
    • Food Science and Preservation
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    • v.30 no.6
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    • pp.944-959
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    • 2023
  • This study investigated the essential oil composition of fresh Panax ginseng root and identified novel compounds from ginseng oil. The oil was divided into five fractions (neutral, basic, phenolic, acidic, and aldehydic). In total, 149 constituents, including 29, 19, and 38 compounds in the basic, phenolic, and aldehydic fractions, respectively, were identified by gas chromatography (GC) and GC-mass spectrometry (MS). The primary constituents of the total ginseng volatile oil were α-humulene (13.91% as a peak area), bicyclogermacrene (13.59%), β-caryophyllene (8.24%), α-neoclovene (7.78%), and α- and β-panasinsenes (5.14% and 7.53%). The primary constituents of the basic fraction were 2-isopropyl-3-methoxypyrazine (35.51%), 3-sec-butyl-2-methoxy-5-methylpyrazine (31.54%), 2-isobutyl-3-methoxypyrazine (8.64%), and 2-methoxy-3-methylpyrazine (8.40%), whereas in the phenolic fraction, these were benzoic (25.40%), octanoic (11.57%), nonanoic (9.16%), propionic (6.35%), and decanoic acids (6.16%). The primary constituents of the aldehydic fraction were 4-(2-furyl)-3-buten-2-one (23.41%), benzaldehyde (10.18%), cis-2-heptanal (9.42%), 3-(α-furyl)-propenal (8.51%), and 2-phenyl-2-butenal (7.28%). Among these, the phenylalkenal compounds, including 2-phenyl-2-butenal, 2-methyl-3-phenyl-2-propenal, 5-methyl-2-phenyl-2-pentenal, 5-methyl-2-phenyl-2-hexenals, 2-phenyl-2-octenal, and 2-phenyl-2-nonenal, were newly identified in this study as ginseng volatile constituents. Furthermore, 2-phenyl-2-nonenal was identified as a plant-based volatile constituent for the first time in this study.

Performance Evaluation of Hazardous Substances using Measurement Vehicle of Field Mode through Emergency Response of Chemical Incidents

  • Lee, Yeon-Hee;Hwang, Seung-Ryul;Kim, Jae-Young;Kim, Kyun;Kwak, Ji Hyun;Kim, Min Sun;Park, Joong Don;Jeon, Junho;Kim, Ki Joon;Lee, Jin Hwan
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.294-302
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    • 2015
  • BACKGROUND: Chemical accidents have increased owing to chemical usage, human error and technical failures during the last decades. Many countries have organized supervisory authorities in charge of enforcing related rules and regulations to prevent chemical accidents. A very important part in chemical accidents has been coping with comprehensive first aid tool. Therefore, the present research has provided information with the initial applications concern to the rapid analysis of hazardous material using instruments in vehicle of field mode after chemical accidents. METHODS AND RESULTS: Mobile measurement vehicle was manufactured to obtain information regarding field assessments of chemical accidents. This vehicle was equipped with four instruments including gas chromatography with mass spectrometry (GC/MS), Fourier Transform Infrared Spectroscopy (FT-IR), Ion Chromatography (IC), and UV/Vis spectrometer (UV) to analyses of accident preparedness substances, volatile compounds, and organic gases. Moreover, this work was the first examined the evaluation of applicability for analysis instruments using 20 chemicals in various accident preparedness substances (GC/MS; 6 chemicals, FT-IR; 2 chemicals, IC; 11 chemicals, and UV; 1 chemical) and their calibration curves were obtained with high linearity ( r 2 > 0.991). Our results were observed the advantage of the high chromatographic peak capacity, fast analysis, and good sensitivity as well as resolution. CONCLUSION: When chemical accidents are occurred, the posted measurement vehicle may be utilized as tool an effective for qualitative and quantitative information in the scene of an accident owing to the rapid analysis of hazardous material.

Monitoring of Methanol Levels in Commercial Detergents and Rinse Aids (시판 세척제 및 헹굼보조제 중 메탄올 함량 모니터링)

  • Park, Na-youn;Yang, Heedeuk;Lee, Jeoungsun;Kim, Junghoan;Park, Se-Jong;Choi, Jae Chun;Kim, MeeKyung;Kho, Younglim
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.263-268
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    • 2019
  • Methanol is a toxic alcohol used in various products such as antifreeze, detergent, disinfectant and industrial solvent. In the human body, methanol is oxidized to formaldehyde and formic acid, which can lead to metabolic acidosis, optic nerve impairment, and death. In this study, the methanol levels in detergents (n=191) and rinse aids (n=13) were analyzed by gas chromatography-headspace-mass spectrometry (GC-HS-MS). Limit of detection was 1.09 mg/kg, accuracy and precision were 91.1-97.9% and <10%, and it was suitable for quantitative analysis. This analysis method was simple and fast with a higher recovery rate than the conventional MFDS (Ministry of Food and Drug Safety) method of diluting the sample in water and putting it in a headspace vial.

High-Performance Liquid Chromatographic Determination of Phenothrin and Silafluofen Residues in Crops with Mass Spectrometric Confirmation (고성능 액체크로마토그래피와 질량분석법을 이용한 농산물 중 Phenothrin 및 Silafuofen의 정밀 잔류분석법 개발)

  • Lee, Young-Deuk;Oh, Jae-Ho;Jang, Sang-Won
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.389-400
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    • 2011
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of phenothrin and silafluofen, known as synthetic pyrethroids, in agricultural commodities. Insecticide residues were extracted with acetone from representative samples of four crops which comprised rice, apple, pepper and cabbage. The extract was purified serially by liquid-liquid partition and Florisil column chromatography. For rice and pepper samples, acetonitrile/n-hexane partition was additionally adopted to remove nonpolar interferences. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate two phenothrin isomers and silafluofen from sample co-extractives. Intact parent compounds were sensitively detected by ultraviolet absorption at 226 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine phenothrin and silafluofen residues at 0.02 and 0.01 mg/kg, respectively. Mean recoveries of phenothrin and silafluofen from four crop samples fortified at three levels in triplicate were in the range of 82.4~109.8% and 83.7~109.8%, respectively. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types and spiking levels. A selected-ion monitoring (SIM) LC/mass spectrometry (MS) with electrospray ionization was provided to confirm the suspected residue of phenothrin, even though no sufficient ionization of silafluofen was obtained. Both phenothrin and silafluofen could be successfully confirmed by gas chromatography/MS SIM with electron impact at 70 eV. The proposed method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products.

Antimicrobial Activity of Pseudomonas aeruginosa BCNU 1204 and Its Active Compound (Pseudomonas aeruginosa BCNU 1204의 항균활성과 활성 물질)

  • Shin, Hwa Jin;Joo, Woo Hong
    • Journal of Life Science
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    • v.29 no.1
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    • pp.84-89
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    • 2019
  • Previous screening of novel antibacterial agents revealed that some bacterial isolates exhibited antibiotic activity against both gram-positive and gram-negative bacteria and that they showed antibacterial activity, even against methicillin-resistant Staphylococcus aureus (MRSA). Among these isolates, one bacterial strain, BCNU 1204, was identified as Pseudomonas aeruginosa using phenetic and phylogenetic analysis, based on 16S ribosomal RNA gene sequences. The maximum productivities of antimicrobial substances of BCNU 1204 were obtained after being cultured at $35^{\circ}C$ and pH 7.0 for 4 d in King's medium B (KMB). Dichloromethane (DCM) and ethylacetate (EA) extracts of P. aeruginosa BCNU 1204 exhibited strong antimicrobial activity, particularly against gram-positive bacteria. The EA extracts exhibited broad-spectrum activity against antibiotic resistant strains. Fraction 5-2, was obtained by recycling preparative liquid chromatography (LC) and preparative thin-layer chromatography (TLC) and was identified as phenazine-1-carboxylic acid belonging to phenazines using gas chromatography and mass spectrometry (GC/MS). Its minimum inhibitory concentration (MIC) values were $25{\mu}g/ml$, $50{\mu}g/ml$, ${\geq}25{\mu}g/ml$, and ${\geq}50{\mu}g/ml$ for MRSA CCARM 3089, 3090, 3091, and 3095 strains, respectively. P. aeruginosa BCNU 1204 may be a potential resource for the development of anti-MRSA antibiotics. Additional research is required to identify the active substance from P. aeruginosa BCNU 1204.

Development of Analytical Method for the Determination and Identification of Unregistered Pesticides in Domestic for Orange and Brown Rice(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide- (식품공전 분석법 미설정 농약의 잔류분석법 확립(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide-)

  • Chang, Hee-Ra;Kang, Hae-Rim;Kim, Jong-Hwan;Do, Jung-A;Oh, Jae-Ho;Kwon, Ki-Sung;Im, Moo-Hyeog;Kim, Kyun
    • Korean Journal of Environmental Agriculture
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    • v.31 no.2
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    • pp.157-163
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    • 2012
  • BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.

Analysis of radiation induced hydrocarbons by electron-beam irradiation in dried squid (Todarodes pacificus) and octopus (Paroctopus dofleini) (전자선 조사한 건조된 오징어와 문어에서 유도된 지방분해산물의 분석)

  • Hong, Young Shin;Ryu, Keun Young;Kim, Kyong Su
    • Food Science and Preservation
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    • v.21 no.3
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    • pp.381-387
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    • 2014
  • Food irradiation is one of the successful modern techniques used to preserve food. However, it needs very careful control. Detection of irradiated food is of prime importance to facilitate global trade and consumer assurance, choice, and protection. This study was performed to evaluate the radiation-induced hydrocarbon content of dried squid and octopus by e-beam irradiation. The samples were collected from supermarkets all over South Korea and irradiated with an e-beam at 0, 1, 3, 5, 7, and 10 kGy doses. Lipids were extracted with soxhelt, and the hydrocarbons induced with irradiation were separated via solid phase extraction (SPE) and identified via gas chromatography mass spectrometry (GC/MS). The major induced hydrocarbons in the irradiated dried squid and octopus were 1-tetradecene and pentadecane derived from palmitic acid and 1-hexadecene and heptadecane from stearic acid. The concentration of hydrocarbons differed from the composition of the fatty acid at the same radiation and increased according to the level of the radiation dose. The hydrocarbons induced by e-beam irradiation, including 1-tetradecene, 1-hexadecene, and heptadecane, were confirmed to have been the irradiation marker compounds. Therefore, they can be used to distinguish the e-beam-irradiated dried squid and octopus from the non-irradiated ones.

Volatile Components of Pine Needle(Pinus densiflora S.) by Purge and Trap Headspace (Purge and Trap Headspace 법에 의한 솔잎(Pinus densiflora S.)의 휘발성 성분)

  • Lee Jae-Gon;Lee Chang-Gook;Jang Hee-Jin;Kwag Jae-Jin
    • The Korean Journal of Food And Nutrition
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    • v.17 no.3
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    • pp.260-265
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    • 2004
  • Volatile components of pine needle(Pinus densiflora S.) were isolated by purge & trap headspace technique and analyzed by gas chromatography-mass spectrometry(GC-MS). And then volatile components were extracted for 2 hr and 20 hr at the two different temperature settings: room temperature and 60$^{\circ}C$. A total of 61 volatile components were identified by the four different conditions. These compounds are classified into six categories in terms of chemical functionality: 35 hydrocarbons, 16 alcohols, 4 carbonyls, 2 esters, 1 acid and 3 ethers. The major components were ${\alpha}$-pinene(1.5~15.7%), ${\beta}$-myrcene(13.2~15.6%), ${\beta}$-phellandrene(l2.0~16.0%) and cis-3-hexenol(4.0~18.3%). In the comparison of the four extraction conditions, longer extraction can be effective to extract components that have a high boiling point, but proved useless in obtaining low boiling point components. As a result of these experiments under the four different conditions, the 20 hr extraction at room temperature appeared to be the most optimized condition for the analysis of volatile compounds by using the purge & trap headspace technique.

Monitoring of Benzoic Acid, Sorbic Acid, and Propionic Acid in Spices (향신료에서 유래되는 안식향산, 소브산, 프로피온산의 함유량 조사)

  • Yun, Sang Soon;Lee, Sang Jin;Lim, Do Yeon;Lim, Ho Soo;Lee, Gunyoung;Kim, MeeKyung
    • Journal of Food Hygiene and Safety
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    • v.32 no.5
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    • pp.381-388
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    • 2017
  • In this study, we investigated the levels of natural preservatives of benzoic acid, sorbic acid, and propionic acid in spices. The quantitative analysis was performed using high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for benzoic acid and sorbic acid and gas chromatography-mass spectrometry (GC-MS) for propionic acid. The sample was extracted with ethanol using sonication, then centrifuged and evaporated to dryness and redissolved to 1 mL with ethanol to use for the instrumental analysis. The analytical method was validated based on linearity, recovery, limit of detection (LOD), and limit of quantification (LOQ). This method was suitable to determine low amounts of naturally occurring preservatives (benzoic acid, sorbic acid, and propionic acid) in various spices. Benzoic acid, sorbic acid, and propionic acid were found in 165 samples, 88 samples, and 398 samples, respectively from the total of 493 samples. The concentration of benzoic acid, sorbic acid, and propionic acid were ranged at ND-391.99 mg/L, ND-57.70 mg/L, and ND-188.21 mg/L in spices, respectively. The highest mean levels of benzoic acid, sorbic acid, and propionic acid were found in cinnamon (167.15 mg/L), basil leaves (22.79 mg/L), and white pepper (51.48 mg/L), respectively. The results in this study provide ranges of concentration regarding naturally occurring benzoic acid, sorbic acid, and propionic acid in spices. Moreover, the results may use to the case of consumer complaint or trade friction due to the inspection services of standard criteria for the preservatives of spices.

Quality Evaluation of the Cinnamon Essential Oils Based on Gas Chromatographic Analysis and Cytotoxicity (가스 크로마토그래피 분석과 세포독성에 의한 계피 정유의 품질평가)

  • Jung, Hyun-Ju;Jung, Won-Tae;Choi, Jong-Won;Nam, Jung-Hwan;Lee, Kyung-Tae;Kwon, Byung-Mok;Park, Hee-Juhn
    • Korean Journal of Pharmacognosy
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    • v.35 no.4 s.139
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    • pp.288-292
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    • 2004
  • To evaluate the quality of the crude drugs using three kinds of Cinnamomum Cortex (CC), Vietnamese CC (VCC, the stem bark of Cinnamomum obtusifolium), periderm-peeled Chinese CC (PPCC, periderm-peeled stem bark of C. cassia), Chinese CC (CCC, stem bark of C. cassia) and a Cinnamomi Ramulus (CR, the twig of C. cassia), the four essential oils were prepared by steam distillation method. Cinnamaldehdye (CAN) and an unknown substance tentatively named hydroxy-cinnamaldehdye(HCNA) were detected in the four essential oils by gas chromatography-mass spectrometry, the contents of which are significantly different one another. Vietnamese CC had the highest content of HCNA whereas CR had the highest CAN content and the lowest HCNA. Vietnamese CC exhibited the greatest cytotoxic activity against the cancer cell lines, A549, HepG-2, HL-60, P-388, U-937, and KB and CR the lowest cytotoxicity. Contents of CAN and HCNA in CCC and PPCC are positioned between VCC and CR. These results suggest that measurement of HCNA and cytotoxicity may determine the quality of CC and CR.