• 제목/요약/키워드: gas-liquid chromatography

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Hippuric Acid Levels in Paint Workers at Steel Furniture Manufacturers in Thailand

  • Decharat, Somsiri
    • Safety and Health at Work
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    • 제5권4호
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    • pp.227-233
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    • 2014
  • Background: The aims of this study were to determine hippuric acid levels in urine samples, airborne toluene levels, acute and chronic neurological symptoms, and to describe any correlation between urinary hippuric acid and airborne toluene. Methods: The hippuric acid concentration in the urine of 87 paint workers exposed to toluene at work (exposed group), and 87 nonexposed people (control group) was studied. Study participants were selected from similar factories in the same region. Urine samples were collected at the end of a shift and analyzed for hippuric acid by high performance liquid chromatography. Air samples for the estimation of toluene exposure were collected with diffusive personal samplers and the toluene quantified using gas-liquid chromatography. The two groups were also interviewed and observed about their work practices and health. Results: The median of the 87 airborne toluene levels was 55 ppm (range, 12-198 ppm). The median urinary hippuric acid level was 800 mg/g creatinine (range, 90-2547 mg/g creatinine). A statistically significant positive correlation was found between airborne toluene exposure and urine hippuric acid levels (r = 0.548, p < 0.01). Workers with acute symptoms had significantly higher hippuric acid levels than those who did not (p < 0.05). It was concluded that there was a significant correlation between toluene exposure, hippuric acid levels, and health (p < 0.001). Conclusion: There appears to be a significant correlation between workers exposure to toluene at work, their urine hippuric acid levels, and resulting symptoms of poor health. Improvements in working conditions and occupational health education are required at these workplaces. There was good correlation between urinary hippuric acid and airborne toluene levels.

하천수에서 LC-ESI-MS/MS에 의한 극미량 농약류 및 합성원료의 동시분석법 (Simultaneous Determination of Ultra-Trace Pesticides and Synthetic Materials in Surface Water by LC-ESI-MS/MS)

  • 홍선화;이준배;이수형;조영환;신호상
    • 대한화학회지
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    • 제59권3호
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    • pp.225-232
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    • 2015
  • 하천수 중에 7가지의 농약류(2,4-dichlorophenoxyacetic acid, 메소밀, 알디캅, MCPA, molinate, 카바릴, 카보퓨란)와 2가지의 합성원료(quinoline, 비스페놀-A)를 액체크로마토그래피 전자분무 이온화 질량분석법(liquid chromatography-electrospray ionization-tandem mass spectrometry, LC-ESI-MS/MS)을 사용하여 분석하였다. 분석물질들은 고체상 추출법(solid-phase extraction, SPE)을 사용하여 추출하였다. 용리액은 질소가스로 농축하였다. 잔여물에 30% 메탄올 수용액 100 μL를 재 용해시켜 0.2 μm PTFE 실린지 필터로 거른 후 그 일부를 LC-ESI-MS/MS에 직접 주입하여 분석하였다. 확립된 조건에서 검정곡선은 0.997 이상의 상관계수를 갖는 직선성을 보였다. 정량한계는 0.002~0.011 μg/L 이었고, 정밀도는 16.4% 이하였다. 또한 정확도는 84~107%의 범위를 보였고, 회수율은 56.2~98.6% 값을 나타내었다. 본 연구에서 개발한 분석법을 실제 하천수 분석에 적용하였다.

Determination of Betaine in Fructus Lycii Using Hydrophilic Interaction Liquid Chromatography with Evaporative Light Scattering Detection

  • Shin, Hyun-Du;Suh, Joon-Hyuk;Kim, Jung-Hyun;Lee, Hye-Yeon;Eom, Han-Young;Kim, Un-Yong;Yang, Dong-Hyug;Han, Sang-Beom;Youm, Jeong-Rok
    • Bulletin of the Korean Chemical Society
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    • 제33권2호
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    • pp.553-558
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    • 2012
  • A simple new method was developed for the determination of betaine in Fructus Lycii using hydrophilic interaction liquid chromatography with evaporative light scattering detection (HILIC-ELSD). Good chromatographic separation and reasonable betaine retention was achieved on a Kinetex HILIC column ($2.1{\times}100mm$, $2.6{\mu}m$) packed with fused-core particle. The mobile phase consisted of (A) acetonitrile and (B) 10 mM ammonium formate (pH 3.0)/acetonitrile (90/10, v/v). It was used with gradient elution at a flow rate of 0.7 mL/min. The column temperature was set at $27.5^{\circ}C$ and the injection volume was $10{\mu}L$. The ELSD drift tube temperature was $50^{\circ}C$ and the nebulizing gas (nitrogen) pressure was 3.0 bar. Stachydrine, a zwitterionic compound, was used as an internal standard. Calibration curve over $10-250{\mu}g/mL$ showed good linearity ($R^2$ > 0.9992) and betaine in the 70% methanol extract of Fructus Lycii was well separated from other peaks. Intraand inter-day precision ranged from 1.1 to 3.0% and from 2.4 to 5.3%, respectively, while intra- and inter-day accuracy ranged from 100.0 to 107.0% and from 94.3 to 103.9%, respectively. The limit of quantification (LOQ) was $10{\mu}g/mL$ and the recoveries were in the range of 98.2-102.7%. The developed HILIC-ELSD method was successfully applied to quantitatively determine the amount of betaine in fourteen Fructus Lycii samples from different locations, demonstrating that this method is simple, rapid, and suitable for the quality control of Fructus Lycii.

Analytical Determination of Vitamin B12 Content in Infant and Toddler Milk Formulas by Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)

  • Lee, Jung-Hoon;Shin, Jin-Ho;Park, Jung-Min;Kim, Ha-Jung;Ahn, Jang-Hyuk;Kwak, Byung-Man;Kim, Jin-Man
    • 한국축산식품학회지
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    • 제35권6호
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    • pp.765-771
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    • 2015
  • The development of a sample preparation method and optimization of the analytical instrumentation conditions were performed for the determination of the vitamin B12 content in emulsified baby foods sold on the Korea market. After removal of the milk protein and fats by chloroform extraction and centrifugation, the vitamin B12 was water extracted from the sample. Following filtration of the solution through a nylon filter, the water-soluble extract was purified by solid-phase extraction using a Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS). The solution eluted from the cartridge was dried under a stream of nitrogen gas and reconstituted with 1 mL of water. The sample solution was injected into an LC-MS/MS system after optimizing the mobile phase for vitamin B12 detection. The calibration curve showed good linearity with the coefficient of correlation (r2) value of 0.9999. The limit of detection was 0.03 µg/L and the limit of quantitation was 0.1 µg/L. The method of detection limit was 0.02 µg/kg. The vitamin B12 recovery from a spiking test was 99.62% for infant formula and 99.46% for cereal-based baby food. The sample preparation method developed in this study would be appropriate for the rapid determination of the vitamin B12 content in infant formula and baby foods with emulsified milk characteristics. The ability to obtain stable results more quickly and efficiently would also allow governments to exercise a more extensive quality control inspection and monitoring of products expected to contain vitamin B12. This method could be implemented in laboratories that require time and labor saving.

액체크로마토그래피-사중극 비행시간형 탠덤질량분석기를 이용한 Bacillus mojavensis 균주 속 사이드로포어 규명 (Determination of Siderophore from Bacillus Mojavensis Using Liquid Chromatography quadrupole Time-of-flight Tandem Mass Spectrometry)

  • 천해인;여미선;김강민;강재선;표재성
    • 생명과학회지
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    • 제29권2호
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    • pp.198-201
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    • 2019
  • Bacillus mojavensis를 이용한 항진균성 및 식물 생장 촉진 활성이 최근 보고되었다. 이런 활성은 사이드로포어의 일반적 특성과 일치하여, 본 연구에서는 Bacillus mojavensis가 생산하는 사이드로포어를 고체상추출 카트리지와 액체크로마토그래피-사중극 비행시간형 탠덤 질량분석기를 이용하여 규명하였다. Bacillus mojavensis를 페놀 배지에서 16시간 동안 배양하고 동결 건조 시킨 후, 물에 용해시켜 고상추출 카트리지에 로딩하였다. 카트리지는 5% 메탄올로 세척하고 2% 포름산을 이용해 용출 시켰다. 용출액은 메탄올에 재용해 후 분석을 하였다. Bacillus mojavensis의 사이드로포어는 질량 스펙트럼의 결과를 바탕으로 882.2556의 분자량을 갖는 카테콜타입의 사이드로포어 중 하나인 bacillibactin으로 확인되었다. 이 사이드로포어 분석은 Bacillus 연구 및 기능성 식품 그리고 Bacillus mojavensis의 약학 응용 분야에 큰 기여를 할 것으로 예상된다.

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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    • 제9권3호
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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).

방사선 조사 돼지고기에서 휘발성 조사물질의 구명 (Identification of Irradiation-induced Volatile Flavor Compounds in Irradiated Pork Meats)

  • 차용준;김훈;조우진;정연정;변명우;유영재
    • 생명과학회지
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    • 제11권1호
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    • pp.35-42
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    • 2001
  • Irradiation-induced volatile flavor compounds in irradiated (0, 1, 3, 5, 10 kGy) pork meats were analyzed by liquid liquid continuous extraction (LLCE) and gas chromatography/mass spectrometry (GC/MS) methods. One hundred nine volatile compounds were detected in irradiated pork meats. These compounds were mainly composed of hydrocarbons (42 compounds), aromatic compounds (39), aldehydes(9), ketones(5) and miscellaneous compounds (14). Among these, three volatile compounds, such as decene, 1,2,3,4,-tetrahydro-6-methylnaphthalene and 1,2,3,4-tetrahydro-dimethylnaphthalene were selected as irradiation-induced compounds comparing with irradiation dosages in irradiated pork meats. By the high correlation coefficient with the increment of irradiation dose, however, decene (r=0.93) was considered as marker compound for detecting irradiation dosage in fresh pork meats.

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Characterisation of the pyrolysis oil derived from bael shell (aegle marmelos)

  • Bardalai, Monoj;Mahanta, Dimbendra Kumar
    • Environmental Engineering Research
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    • 제21권2호
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    • pp.180-187
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    • 2016
  • In the present work, bael shell (aegle marmelos) is used as the feedstock for pyrolysis, using a fixed bed reactor to investigate the characteristics of the pyrolysis oil. The product yields, e.g., liquid, char and gases are produced from the biomass at different temperatures with the particle size of 0.5-1.0 mm, at the heating rate of $150^{\circ}C/min$. The maximum liquid yield, i.e., 36.23 wt.%, was found at $5500^{\circ}C$. Some physical properties of the pyrolysis oil such as calorific value, viscosity, density, pH, flash point and fire point are evaluated. The calorific value of the bael shell pyrolysis oil was 20.4 MJ/kg, which is slightly higher than the biomass, i.e., 18.24 MJ/kg. The H/C and O/C ratios of the bio-oil were found as 2.3 and 0.56 respectively, which are quite higher than some other bio-oils. Gas Chromatography and Mass Spectroscopy (GC-MS) and Fourier Transform Infra-red (FTIR) analyses showed that the pyrolysis oil of bael shell is mostly composed by phenolic and acidic compounds. The results of the properties of the bael shell pyrolysis oil reveal the potential of the oil as an alternate fuel with the essential upgradation of some properties.

Identification of Character-impact Aroma Compounds and Comparisons of Sensory Attributes of Traditional Korean Medicinal Rice Wines Brewed with Functional Herbal Powders or Extracts

  • Lee, Gyu-Hee;Shin, Young;Chang, Yeong-Il;Jeong, Jae-Hong;Chang, Kyu-Seob;O, Man-Jin
    • Preventive Nutrition and Food Science
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    • 제7권4호
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    • pp.405-410
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    • 2002
  • Rice wine was prepared with medicinal plants or plant extracts to obtain a value added nutritious alcoholic tonics. Powders of ten medicinal plants (PTM) or aqueous extracts prepared from them (ATM) were added during the initial stage of fermentation. Aroma compounds of rice wine (control) and wines containing PTM or ATM were isolated by liquid-liquid continuous solvent extraction (LLCSE) and analyzed by gas chromatography-olfactometry and aroma extract dilution analysis (AEDA). Desirable aroma compounds: acetaldehyde (sweet, ethereal), benzaldehyde (sweet, fragrant), ethyl acetate (sweet) and ethyl octanoate (sweet, ethanolic) had the highest log$_3$-flavor dilution (FD) factors in ATM. Results of sensory evaluation demonstrated that intensities of undesirable aroma attributes, such as koji and yeasty notes in control, and raw medicinal herb notes in PTM, were lowest in wine with ATM. Wines made with ATM had the most attractive aroma attributes among the three different traditional Korean medicinal wines.

전통주의 품질 특성 규명을 위한 향기 성분 분석 (Determination of the Volatile Flavor Compounds for the Quality Characteristics in Traditional Alcoholic Beverages)

  • 안윤경;송영순;신정화
    • 한국지역사회생활과학회지
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    • 제23권2호
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    • pp.199-206
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    • 2012
  • In order to evaluate the aroma compounds in Korean traditional alcoholic beverages, volatile compounds of the commercial wines, Makgeolli were analyzed and quantified using the conventional method. Eight volatile compounds including three kinds of alcohols, two kinds of organic acids and three kinds of ether were extracted by Liquid-Liquid Extraction with Dichloromethane. For the separation and quantification, Gas chromatography coupled with mass spectrometry (GC/MS) was used to analyze these compounds. Also, the separation efficiency of these compounds was performed and compared with GC column. The results of this study were as follows ; Eight kinds of volatile compounds were separated well on the HP-88 column better than on the DB-5MS column. Short chain fatty acids, butyric acid and isovaleric acid were not detected in two brands of makgeolli samples. The higher alcohols were detected in the range of 0.86~225.68 ${\mu}g/mL$ and ethyl esters were detected in the range of 0.86~225.68 ${\mu}g/mL$, respectively. There compounds are known to be associated with sensory and odorant.