• Title/Summary/Keyword: gc/ms

Search Result 2,442, Processing Time 0.03 seconds

Analysis of Polycyclic Aromatic Hydrocarbons in Agricultural Waterways in Chungbuk and Gyeongbuk Provinces in Korea

  • Kim, Leesun;Lee, Jong-Hwa;Kim, Jeong-Han;Lee, Sung-Eun
    • Korean Journal of Environmental Biology
    • /
    • v.36 no.3
    • /
    • pp.345-351
    • /
    • 2018
  • An efficient, quick and low-cost extraction and clean up method for the determination of 14 polycyclic aromatic hydrocarbons (PAHs) in the agricultural water samples was optimized using gas chromatography-tandem mass spectrometry (GC-MS/MS). The extraction of the target compounds in water sample was carried out with acetonitrile, followed by partitioning promoted by the addition of salt. As a clean-up procedure, dispersive solid phase extraction was employed to purify the analytes of interest for GC-MS/MS analysis. This method was successfully applied for the quantification of PAHs in real water samples collected for the purpose of monitoring from the waterways located in Chungbuk (15 sites) and Gyeongbuk (6 sites), S. Korea. Phenanthrene (0.54 to $2.53{\mu}gL^{-1}$) was detected in all the water samples collected from both the sites. Fluoranthene was detected in the water samples collected from the two sites in Gyeongbuk province, but other PAHs were not determined in these water sampling sites. Based on these results, the determined PAHs were conducted using an environmental risk assessment. The risk characterization ratios (RCRs) for phenanthrene ranged from 0.37 to 3.21. These RCR values referred to as risk was not controlled because RCR values of some sites were greater than 1. In conclusion, it is proposed that the optimized method in combination with GC-MS/MS could be successfully employed for the determination of PAHs in any environmental samples including water samples.

Qualitative, Quantitative Analysis and Chiral Characterization of the Essential Oils of Juniperus phoenicea L. and Juniperus oxycedrus L.

  • Dahmane, Dahmane;Dahmane, Fahima Abdellatif;Dob, Tahar;Chelghoum, Chaabane
    • Natural Product Sciences
    • /
    • v.26 no.1
    • /
    • pp.97-107
    • /
    • 2020
  • Isolation of oils from leaves of Juniperus phoenicea and Juniperus oxycedrus was obtained by steam distillation extraction method. The compositions of essential oils (EOs) were studied by means of GC-MS and GC-FID, using the internal standard method and relative response factors. Around ninety eight compounds were determined in total, representing 98.25 g/100 g of EO of J. phoenicea and 98.48 g/100 g of EO of J. oxycedrus, respectively. The volatile leaf oils were dominated by the terpenic hydrocarbon fractions (79.87 g/100 g) and (61.27 g/100 g) characterized by high contents of α-pinene (64.6 g/100 g) and (54.0 g/100 g) in J. phoenicea and J. oxycedrus, respectively, as the main component. Also, the enantiomeric distribution of α-pinene, sabinene, camphene, δ-3-carene, β-pinene, limonene, linalool, terpinen-4-ol, bornyl acetate, and borneol in both oils is presented for the first time.

NEAR INFRARED TRANSFLECTANCE SPECTROSCOPY (NIRS) IN PHYTOCHEMISTRY

  • Huck, C.W.;W.Guggenbichler;Bonn, G.K.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
    • /
    • 2001.06a
    • /
    • pp.3114-3114
    • /
    • 2001
  • During the last years phytochemistry and phytopharmaceutical applications have developed rapidly and so there exists a high demand for faster and more efficient analysis techniques. Therefore we have established a near infrared transflectance spectroscopy (NIRS) method that allows a qualitative and quantitative determination of new polyphenolic pharmacological active leading compounds within a few seconds. As the NIR spectrometer has to be calibrated the compound of interest has at first to be characterized by using one or other a combination of chromatographic or electrophoretic separation techniques such as thin layer chromatography (TLC), high performance liquid chromatography (HPLC), capillary electrophoresis (CE), gas chromatography (GC) and capillary electrochromatography (CEC). Both structural elucidation and quantitative analysis of the phenolic compound is possible by direct coupling of the mentioned separation methods with a mass spectrometer (GC-MS, LC-MS/MS, CE-MS, CEC-MS) and a NMR spectrometer (LC-NMR). Furthermore the compound has to be isolated (NPLC, MPLC, prep. TLC, prep. HPLC) and its structure elucidated by spectroscopic techniques (UV, IR, HR-MS, NMR) and chemical synthesis. After that HPLC can be used to provide the reference data for the calibration step of the near infrared spectrometer. The NIRS calibration step is time consuming, which is compensated by short analysis times. After validation of the established NIRS method it is possible to determine the polyphenolic compound within seconds which allows to raise the efficiency in quality control and to reduce costs especially in the phytopharmaceutical industry.

  • PDF

A Study on the Qualitative Characteristics of Non-Regulated Organic Pollutants in Municipal Wastewater (하수성분중 비규제대상 유기오염물질의 정성적 특성에 관한 연구)

  • Shin, Jinhwan;Jeoung, Youngdo
    • Journal of the Korean GEO-environmental Society
    • /
    • v.8 no.3
    • /
    • pp.5-10
    • /
    • 2007
  • The paper presents results of qualitative analysis of non-regulated organic pollutants in municipal wastewater and treated municipal wastewater with flocculation, ozone and UV process using GC-MS. The majority of the pollutants in the influent of the municipal wastewater treatment facility were either food related or due to the diffuse discharge from products used both in households and in industry. In the case of biological treatment process removed some organic pollutants effectively. But some organic pollutants were not removed with biological treatment. Thus, additional steps to improve the quality of effluent municipal wastewater will require a more rigorous control of consumer products used in household and municipal wastewater process using advanced treatment processs. The obtained data contributed to the evaluation of pollutants discharges to the ecosystem as well as to the characterization of pollution sources in the basin.

  • PDF

Separation and recovery of semi-volatile substances of Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus by reduced pressure collections and GC-MS

  • Lee, In-Ho;Byun, Chang Kyu;Eum, Chul Hun;Kim, Taewook;Lee, Sam-Keun
    • Analytical Science and Technology
    • /
    • v.33 no.1
    • /
    • pp.11-22
    • /
    • 2020
  • When extracting semi-volatile components of herbal medicines using hot water vapor, some substances may react with water vapor or oxygen, and some volatile substances may be lost, when using an organic solvent extraction method has the disadvantage that it may contain a non-volatile material and residual organic solvent. In addition, it is inefficient to separate semi-volatile substances from herbal medicines into each single component and conduct biological activity research for each component to determine the effective ingredient, and some components may be lost in the separation process. In this study, semi-volatile substances evaporated under two pressure-reduced conditions in Chinese herbal medicines such as Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were separated by cooling with liquid nitrogen. Those were analyzed by gas chromatography-mass spectrometry (GC-MS) to identify the components, and this method may be used to study biological activities at the cellular level. The substances separated under reduced pressure, essential oil obtained by simultaneous distillation extraction (SDE) method and substances by using solid phase micro-extraction (SPME) from Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were analyzed by GC-MS. In the case of Cnidii Rhizoma and Aucklandiae Radix, there were some differences among the essential oil components obtained by SDE and those identified by low temperature capture (CT) and SPME method, these were believed to be produced by some volatiles reacting with water or oxygen at the boiling point temperature of water.

Quantitative Analysis of Pentachlorophenol in Paper Products (종이재 중의 Pentachlorophenol 정량 분석)

  • Hahn, Airan;Park, Jihye;Choi, Hyeongki;Hong, Sungyeap;Han, Hyechul;Jo, Byoungmuk;Oh, Jungsoo
    • Applied Chemistry for Engineering
    • /
    • v.16 no.3
    • /
    • pp.323-327
    • /
    • 2005
  • Pentachlorophenol (PCP) is a representative compound of chlorophenol derivatives which are especially toxic and potentially carcinogenic compounds in the priority pollutant list of the EPA (Environmental Protection Agency, USA). The aim of this study was to investigate an analysis method of PCP in infinitesimal quantity retained in paper. PCP in paper was pretreated by solid phase extraction (SPE) in a phenyl cartridge. The extracted sample was acetylated or silylated and analyzed with GC/MS-SIM. The detection sensitivity of silylated PCP was improved significantly when compared with those of PCP itself and acetylated PCP. As a test specimen, an office paper and a wallpaper were used.

Analysis of Amineptine and its Metabolites in Human Urine by Gas Chromatography/Mass Spectrometry (Gas Chromatography/Mass Spectrometry를 이용한 뇨중 Amineptine과 그 대사체 분석방법에 관한 연구)

  • Lee, Jeong Ae;Kim, Younglim;Lho, Dong-Seok
    • Analytical Science and Technology
    • /
    • v.13 no.3
    • /
    • pp.385-393
    • /
    • 2000
  • A gas chromatography-mass spectrometric (GC/MS) procedure for the determination of amineptine (dihydro-10, 11-dibenzo[a, d] cycloheptenyl-5-amino-7-heptanoic acid) and its main metabolites in human urine was described. Amineptine has been known to be extensively metabolized by the ${\beta}$-oxidation of the heptanoic side chain with formation of pentanoic side chain metabolite ($C_5$-metabolite), and lactamizarion by internal dehydration of (${\beta}$-oxidized metabolite (${\delta}$-lactam). The detection of these compounds was based on acid hydrolysis, liquid-liquid extraction and trimethylsilylated derivatization of the carboxylic acid group. For the determination of amineptine and its metabolites in biological fluids, selected ions at the m/ 192, molecular ion and one of the characteristic ions were monitored by GC/MS. On the excretion study of amineptine in human urine, 70-90% of amineptine, ${\delta}$-lactam, and $C_5$-metabolite were found to be excreted within 4 hours and their excretion completed within 20 hours.

  • PDF

Determination of allyl isothiocyanate, capsaicin and dihydrocapsaicin in pungent liquid samples (자극성 액체시료 중 Allyl Isothiocyanate, Capsaicin and Dihydrocapsaicin 정량에 관한 연구)

  • Kim, Sang-Soo;Choi, Jong-Moon
    • Analytical Science and Technology
    • /
    • v.26 no.1
    • /
    • pp.73-79
    • /
    • 2013
  • The allyl isothiocyanate, capsaicin and dihydrocapsaicin as main components in self defense sprays were determined by gas chromatography-mass spectrometer (GC-MS). Although self defense spray was used to protect by myself, a social problem could be caused by the hazard of spray chemical due to use pungent liquid. To identify this, the pH of pungent liquid solutions, solubility to detergents, the existence of other materials and the types and amounts of pungent material in spray chemicals were investigated in this work. Finally, the amounts of allyl isothiocyanate, capsaicin and dihydrocapsaicin as pungent materials in them were determined by GC-MS. The pH of chemicals were about 5.7 as weak acid, the detergents can emulsify them with water well. And they did not contain fluorescent materials and hazard organic solvents. The pungent components in three real samples were only allyl isothiocyanate [47,600 mg/kg (47.6%)] in one sample, and mixtures with capsaicin [228 mg/kg~368 mg/kg (1.14%~1.84%)] and dihydrocapsaicin [224 mg/kg~414 mg/kg (1.12%~2.07%)] in the others, respectively.

A Study on the Thermal Decomposition Characteristics of Waste PVC Wire Added with CaO (CaO를 첨가한 폐PVC전선의 열적분해 특성에 관한 연구)

  • Shah, Malesh;Park, Ho;Kwon, Woo-Teck;Lee, Hae-Pyeong;Oh, Sea-Cheon
    • Journal of the Korean Applied Science and Technology
    • /
    • v.29 no.2
    • /
    • pp.268-277
    • /
    • 2012
  • The thermal decomposition characteristic of waste PVC wires has been studied by using TGA and fixed-bed reactor. The experimental conditions of decomposition temperatures, air flow rates and weight ratio of CaO/PVC were considered in this work. To verify the effectiveness of CaO addition to remove HCl and toxic gases generated from thermal decomposition of PVC wire, the gaseous products obtained from the thermal decomposition of PVC were analyzed by GC/MS(Gas Chromatograph and Mass Spectrometry). To investigate the effect of CaO in thermal decomposition of PVC, liquid products were also analyzed by GC/MS. And the effect of decomposition temperature, air flow rate and CaO/ PVC weight ratio on the yield of liquid, gas and residue fraction have been also studied. From this work, it was found that the removal amount of HCl generated from thermal decomposition of PVC increased with increase of CaO addition.

Evaluation of Exposure to Organophosphorus Pesticides According to Application Type and the Protective Equipment among Farmers in South Korea (일부 농업인에서의 농약살포방식 및 보호구 착용에 따른 유기인계 농약노출평가)

  • Lee, Jeeyoung;Roh, Sangchul
    • The Korean Journal of Pesticide Science
    • /
    • v.20 no.2
    • /
    • pp.172-180
    • /
    • 2016
  • This study was conducted to evaluate the relations between the exposure level of organophosphates (OPs) pesticide and application factors among rural farmers. The urinary dialkylphosphates, metabolites of organophosphorus pesticides, including DMP, DEP, DMTP and DETP were analyzed by GC/MSD and GC/MS/MS. The DMP and DMTP were detected more in the use of a speed sprayer without cap than with a capped one. Also, the less farmers wore the personal protective equipment (PPE), the more these were detected. The amount of organophosphorus exposure was the highest in the use of a power sprayer. However, it was low when a farmer applied pesticides with a speed sprayer with cap and wore more PPE. In this study, the detection rate was analyzed by chi-square test, the exposure level of OPs was analyzed by a generalized linear model.