• 제목/요약/키워드: quantitative GC analysis

검색결과 197건 처리시간 0.028초

미생물 세포 기반의 에폭사이드 가수분해효소 활성 측정을 위한 분광학적 분석법 최적화 (Optimization of Microbial Cell-Based Spectrometric Assay for the Analysis of Epoxide Hydrolase Activity)

  • 김희숙;이은열
    • 생명과학회지
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    • 제15권1호
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    • pp.136-140
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    • 2005
  • 다양한 라세믹 에폭사이드 기질에 대한 입체선택적 가수분해 반응을 촉매하는 epoxide hydrolase 활성을 측정할 수 있는 미생물 세포 기반의 자외선 활성 분석법을 최적화하였다. 2.5 mg/ml의 세포 농도에서도 비교적 쉽게 흡광도 변화량을 인식할 수 있는 흡광도 범위인 0.5 이상을 얻을 수 있고, 반응 동력학 분석에도 응용할 수 있었다. 기존의 GC, HPLC 분석 법 보다 분석 시간을 줄일 수 있으며, 효소를 별도로 분리$\cdot$정제하지 않고 미생물 세포 자체의 epoxide hydrolase활성 분석이 가능하므로 상업적 특성이 우수한 epoxide hydrolase을 가진 미생물을 효율적으로 선별하는데 응용될 수 있을 것으로 기대된다.

Standardizing GC-FID Measurement of Nonmethane Hydrocarbons in Air for International Intercomparison Using Retention Index and Effective Carbon Number Concept

  • Liaw, Sheng-Ju;Tso, Tai-Ly
    • 분석과학
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    • 제8권4호
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    • pp.807-814
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    • 1995
  • Accurate measurements of ozone precursors are required to understand the process and extent of ozone formation in rural and urban areas. Nonmethane hydrocarbons (NMHCs) have been identified as important ozone precursors. Identification and quantification of NMHCs are difficult because of the large number present and the wide molecular weight range encountered in typical air samples. A major plan of the research team of the Climate and Air Quality Taiwan Station (CATs) was the measurement of atmospheric nonmethane hydrocarbons. An analytical method has been development for the analysis of the individual nonmethane hydrocarbons in ambient air at ppb (v) and subppb(v) levels. The whole ambient air samples were collected in canisters and analyzed by GC-FID with $Al_2O_3$/KCl PLOT column. Our targeted for quantitative analysis 43 compounds that may be substantial contributors to ozone formation. The retention indices and molar response factors of some commercially available $C_2{\sim}C_{10}$ hydrocarbons were determined and used to identify and quantify air samples. A quality assurance program was instituted to ensure that good measurements were made by participating in the International Nonmethane Hydrocarbon Intercomparison Experiments (NOMHICE).

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A High-speed Miniature Screening Gaschromatograph with Flame Ionization Detector

  • Banik Rahul;Lee Dong-Yeon;Gweon Dae-Gab
    • Journal of Mechanical Science and Technology
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    • 제19권12호
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    • pp.2197-2204
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    • 2005
  • The combination of Gas chromatography (GC) for separation and Flame Ionization Detection (FID) for detection and identification of the components of a mixture of compounds is a fast and strongly proved method of analytic chemistry. The objective of this research was to design a combined High-speed miniature screening Gas chromatograph along with a Flame Ionization Detector for quick, quantitative and qualitative analysis of gas components. This combined GC-FID system is suitable to detect the volatile and semi-volatile hydrocarbons present in a gas mixture. The construction made it less expensive, easy to use and movable. The complete gas path was developed. On/off valves, temperature and flow sensors and their interface electronics were used for controlling purpose. A Microcontroller was programmed to measure the temperature and gas flow using the sensors and to control and regulate them using the electronics and valves. A pocket PC with its touch screen served as a user interface for the system. Software was developed for the pocket PC, which makes the communication possible with the Microcontroller. The system parameters can be indicated in the Pocket PC as simple text and also the analysis result can be displayed.

GC-NCI-MS/MS를 이용한 모발 중 대마 대사체 분석의 측정불확도 평가 (Uncertainty evaluation of the analysis of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol in hair by GC-NCI-MS/MS)

  • 김진영;이재일;정재철;서용준;인문교
    • 분석과학
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    • 제24권1호
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    • pp.1-9
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    • 2011
  • 대마 흡연 여부 확인을 위해 사용되는 모발 중 대마 대사체 정량분석 결과의 측정불확도를 평가하였다. 대마초 성분 중 활성물질은 ${\Delta}^9$-tetrahydrocannabinol이며 대사과정을 거쳐 생성된 주요 대사체는 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THC-COOH)이다. 따라서 생체 대사물질인 THC-COOH는 대마 흡연 여부를 판단하는 지표물질로 사용되고 있다. 실험방법은 모발의 세척, 건조, 질량측정, 세절, 가수분해, 비드를 이용한 액체-액체 추출, 유도체화 반응 및 기기분석 과정으로 구성되었다. 측정의 소급성이 유지될 수 있도록 상위 규정기로부터 하위 측정기까지 교정을 통해 확보하였다. 측정불확도 평가에 앞서 정량분석시 측정값에 영향을 주는 인자들을 찾아내고 각각의 요소들이 측정결과에 어떤 영향을 주는가를 살펴보았다. 산출 결과, 재현성, 회수율, 검정곡선, 표준물질, 질량측정의 요소 순으로 불확도에 영향을 미치고 있음을 확인하였고 재현성의 요소가 측정불확도에 가장 큰 영향을 미치고 있었다. 실제 대마 복용자의 모발을 분석한 결과 대마 대사체 농도 측정값에 대한 오차 범위의 상대불확도는 17% 이였으며, 본 연구의 측정불확도 평가 결과는 향후 분석방법의 개선 및 측정결과의 신뢰도 제고를 위한 근거자료로 활용할 예정이다.

Exosomal miR-181b-5p Downregulation in Ascites Serves as a Potential Diagnostic Biomarker for Gastric Cancer-associated Malignant Ascites

  • Yun, Jieun;Han, Sang-Bae;Kim, Hong Jun;Go, Se-il;Lee, Won Sup;Bae, Woo Kyun;Cho, Sang-Hee;Song, Eun-Kee;Lee, Ok-Jun;Kim, Hee Kyung;Yang, Yaewon;Kwon, Jihyun;Chae, Hee Bok;Lee, Ki Hyeong;Han, Hye Sook
    • Journal of Gastric Cancer
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    • 제19권3호
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    • pp.301-314
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    • 2019
  • Purpose: Peritoneal carcinomatosis in gastric cancer (GC) patients results in extremely poor prognosis. Malignant ascites samples are the most appropriate biological material to use to evaluate biomarkers for peritoneal carcinomatosis. This study identified exosomal MicroRNAs (miRNAs) differently expressed between benign liver cirrhosis-associated ascites (LC-ascites) and malignant gastric cancer-associated ascites (GC-ascites), and validated their role as diagnostic biomarkers for GC-ascites. Materials and Methods: Total RNA was extracted from exosomes isolated from 165 ascites samples (73 LC-ascites and 92 GC-ascites). Initially, microarrays were used to screen the expression levels of 2,006 miRNAs in the discovery cohort (n=22). Subsequently, quantitative reverse transcriptase-polymerase chain reaction (qRT-PCR) analyses were performed to validate the expression levels of selected exosomal miRNAs in the training (n=70) and validation (n=73) cohorts. Furthermore, carcinoembryonic antigen (CEA) levels were determined in ascites samples. Results: The miR-574-3p, miR-181b-5p, miR-4481, and miR-181d were significantly downregulated in the GC-ascites samples compared to the LC-ascites samples, and miR-181b-5p showed the best diagnostic performance for GC-ascites (area under the curve [AUC]=0.798 and 0.846 for the training and validation cohorts, respectively). The diagnostic performance of CEA for GC-ascites was improved by the combined analysis of miR-181b-5p and CEA (AUC=0.981 and 0.946 for the training and validation cohorts, respectively). Conclusions: We identified exosomal miRNAs capable of distinguishing between non-malignant and GC-ascites, showing that the combined use of miR-181b-5p and CEA could improve diagnosis.

Discrimination of American ginseng and Asian ginseng using electronic nose and gas chromatography-mass spectrometry coupled with chemometrics

  • Cui, Shaoqing;Wu, Jianfeng;Wang, Jun;Wang, Xinlei
    • Journal of Ginseng Research
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    • 제41권1호
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    • pp.85-95
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    • 2017
  • Background: American ginseng (Panax quinquefolius L.) and Asian ginseng (Panax ginseng Meyer) products, such as slices, have a similar appearance, but they have significantly different prices, leading to widespread adulteration in the commercial market. Their aroma characteristics are attracting increasing attention and are supposed to be effective and nondestructive markers to determine adulteration. Methods: The aroma characteristics of American and Asian ginseng were investigated using gas chromatography-mass spectrometry(GC-MS) and an electronic nose (E-nose). Their volatile organic compounds were separated, classified, compared, and analyzed with different pattern recognition. Results: The E-nose showed a good performance in grouping with a principle component analysis explaining 94.45% of variance. A total of 69 aroma components were identified by GC-MS, with 35.6% common components and 64.6% special ingredients between the two ginsengs. It was observed that the components and the number of terpenes and alcohols were markedly different, indicating possible reasons for their difference. The results of pattern recognition confirmed that the E-nose processing result is similar to that of GC-MS. The interrelation between aroma constituents and sensors indicated that special sensors were highly related to some terpenes and alcohols. Accordingly, the contents of selected constituents were accurately predicted by corresponding sensors with most $R^2$ reaching 90%. Conclusion: Combined with advanced chemometrics, the E-nose is capable of discriminating between American and Asian ginseng in both qualitative and quantitative angles, presenting an accurate, rapid, and nondestructive reference approach.

가스크로마토그래피/질량분석기를 이용한 약물의 확인 및 간이 정량분석 프로그램 개발 (Development of Rapid and Simple Drug Identification and Semi Quantitative Analytical Program by Gas Chromatography-Mass Spectrometry)

  • 김은미;한은영;홍효정;정수진;최상길;이종숙;정진미;염혜선;이한선;이상기
    • 약학회지
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    • 제55권2호
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    • pp.106-115
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    • 2011
  • Systematic toxicological analysis (STA) means the process for general unknown screening of drugs and toxic compounds in biological fluids. In order to establish STA, in previous study we investigated pattern of drugs & poisons in autopsy cases during 2007~2009 in Korea, and finally selected 62 drugs as target drugs for STA. In this study, rapid and simple drug identification and quantitative analytical program by gas chromatography-mass spectrometry(GC-MS) was developed. The in-house program, "DrugMan", consisted of modified chemstation data analysis menu and newly developed macro modules. Total 55 drugs among 62 target drugs were applied to this program, they were 14 antidepressants, 8 anti-histamines, 5 sedatives/hypnotics, 5 narcotic analgesics, 3 antipsychotic drugs, and etc. For calibration curves, fifty five drugs were divided into four groups of range considering their therapeutic or toxic concentrations in blood specimen, i.e. 0.05~1 mg/l, 0.1~1 mg/l, 0.1~5 mg/l or 0.5~10 mg/l. Standards spiked bloods were extracted by solid-phase extraction (SPE) with trimipramine-D3 as internal standard. Parameters such as retention times, 3 mass fragment ions, and calibration curves for each drug were registered to DrugMan. A series of identification, semi quantitation of target drugs and reporting the results were performed automatically. Calibration curves for most drugs were linear with correlation coefficients exceeding 0.98. Sensitivity rate of DrugMan was 0.90 (90%) for 55 drugs at the level of 0.5 mg/l. For standard spiked bloods at the level of 0.5 mg/l for 29 drugs, semi quantitative concentrations were ranged 0.36~0.64 mg/l by DrugMan. If more drugs are registered to database in DrugMan in further study, it will be useful tools for STA in forensic toxicology.

QuEChERS법과 PTV-GC/TOFMS 이용 잔류농약 분석법 개발을 위한 사과시료 중 236종 농약의 동시분석 (Analysis of 236 Pesticides in Apple for Validation of Multiresidue Method using QuEChERS Sample Preparation and PTV-GC/TOFMS Analysis)

  • 주옥정;권혜영;박병준;김찬섭;진용덕;이제봉;윤서희;손경애;홍수명;임건재
    • 농약과학회지
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    • 제15권4호
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    • pp.401-416
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    • 2011
  • 최근 농식품 중 잔류농약의 분석을 위해서 전처리를 빠르고 단순하게 하면서 고감도의 정밀기기를 이용하여 정성 및 정량을 동시에 행하는 분석방법의 개발이 확대되고 있다. 따라서 신속한 전처리법으로 빠르게 확산되고 있는 QuEChERS(quick, easy, cheap, effective, rugged and safe)법과 PTV(programmable temperature vaporizer)가 장착된 GC/TOFMS을 이용하여 분석법을 개발하였다. PTV조건을 확립했으며 사과 시료를 대상으로 3농도 수준에서(50, 100, 400 ng/g) QuEChERS법(acetate buffer법)으로 전처리 한 후 PTV-GC/TOFMS로 분석하여 회수율 및 RSD를 조사한 결과 400 ng/g 농도에서는 230성분(97%)이 80-120%의 회수율을 보였으며 5성분(2.1%)을 제외한 모든 성분에서 RSD값이 10%미만으로 양호한 재현성을 보였다. 가장 낮은 농도인 50 ng/g의 경우에서는 검출되지 않은 33성분을 제외한 203성분 중 197성분(97%)에서 70-120%의 회수율을 보였으며, 4성분(2.0%)을 제외한 모든 성분에서 RSD값이 20%미만으로 나타났다. 따라서 본 연구에서 확립된 QuEChERS 전처리법과 PTV-GC/TOFMS 분석조건을 이용하여 과일과 야채중의 잔류농약 분석이 가능할 것으로 보였다.

PC/Monitor 구성 전자부품에서 방출되는 휘발성 유기화합물의 분석 (Analysis of Volatile Organic Compounds Emitted from Electronic Parts in PC/Monitor Set)

  • 이창섭;최정우;백규원
    • 대한화학회지
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    • 제44권4호
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    • pp.343-349
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    • 2000
  • PC/Monitor의 구성 전자부품으로부터 방출되는 휘발성 유기화합물(Volatile Organic Com-pounds,VOCs)를 분석하였다. Mpnitor를 구성하는 전자부품으로부터 연속으로 방출되는 VOCs의 경향을 시료챔버에 직접 연결되어있는 잔류가스 분석기(Residual Gas Analyzer,RG A)로 분석하였으며, 이들 전자부품에서 방출되는 VOCs의 성분을 RGA와 GC-MS로 분석하였다. 정성분석된 VOCs 중 소량으로 방출되거라도 불쾌한냄새와 건강상의 장해를 초래할 수 있는 toluene. xylene, cyclohexanone 및 benzofuran에 대하여 GC-MS로 정량분석하였다. 이러한 분석결과, 전자부품중 PCB(CEM-1)을제외하고 나머지 부품들은 가열시작 후 30분에서 1시간동안 toluene, xylene, cyclohexanone 및 phenol이 다량으로 연속 방출되는 경향을 나타내었으며, 거의 모든 전자부품에서 toluene, xylene, phenol, cyclohexanone 및 benzofuran 등의 물질들이측정시간 범위내에서 가장 빈번하게 방출되었다. 부품들 중 Trans가 가장 높은 VOCs의 방출농도를 보였으며, 전자부품으로부터 정량분석된 VOCs중에는 xylene의 방출농도가 550~2482 ${\mu}g/m^2$로 가장 크게 나타났다.

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가스크로마토그라피/질량분석기에 의한 모발중 대마성분 분석 (Analysis of $\triangle^9$-Tetrahydrocannabinol and 11-nor-9-carboxytetrahydrocannabinol in Hair by Gas Chromatography/Mass Spectrometry)

  • 양원경;한은영;박용훈;임미애;정희선
    • 약학회지
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    • 제48권3호
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    • pp.207-212
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    • 2004
  • An analytic method was developed for the quantitation of $\Delta$$^{9}-$ tetrahydrocannabinol (THC) and 11-nor-9-carboxy THC (THC-COOH) in human hair. After hair samples were pulverized using Freezer Mill, deuterated internal standards were added and digested in 1 N NaOH at $100^{\circ}C$ water bath for 30 min. Digest solutions were extracted by 5 ml hexane:ethyl acetate (90:10) after acidification with acetic acid. The organic phase was evaporated under N 2 and derivatized by BSTFA (with 1% TMCS) at $85^{\circ}C$ for 45 min. The derivatized solution was separated on HP-5MS column ($30m{\times}0.25mm{\times}0.25mm$) and detected using EI-GC-MS with selective ion monitoring mode. The assay of calibration was ranged from 5 to 100 ng/50 mg hair ($r^2$>0.99) for THC and THC-COOH. Within and between-run precision were calculated at 6, 30, 60 ng/50 mg hair with coefficients of variation less than 11%. Within and between run accuracies at the same concentrations were$\pm$14% and $\pm$30% of target for both analytes, respectively. Absolute and relative recovery at 10 and 100 ng were 60∼91%. The method was used to detect and quantify THC and THC-COOH in cannabis abuser's hairs (N = 16) and SRM (N=5, THC 1 ng/mg, NIST). We detected THC and THC-COOH in only one hair sample. In SRM, % accuracy was 93% (range 86∼103%) and precision (% CV) was 8.14. We began to set up a quantitative analysis of THC and THC-COOH using EI-GC-MS. Continuously, we need to modify and develop this method in order to apply for identification in cannanbis users' hair.