• Title/Summary/Keyword: DB-5 column

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Comparison of Dioxin Analytical Results Between SP-2331 and DB-5MS Capillary Columns in the HRGC/HRMS Analysis (HRGC/HRMS에 SP-2331 및 DB-5MS 컬럼 사용시 다이옥신 결과의 비교)

  • Hong, Jongki;Yang, Jeong-Soo;Shin, Jung-Hwa;Ahn, Yun-Gyong;Lee, Dai-Woon
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.184-191
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    • 2004
  • In this study, the separation of toxic dioxin 2,3,7,8-congeners by DB-5MS and SP-2331 GC columns which are widely used in HRGC/HRMS analysis was examined. Through the dioxin analysis of column performance check standard solution and fly ash sample, the isomer specific separation of 2,3,7,8-substituted dioxins from tetra to hexa-isomers on DB-5MS and SP-2331 columns were studied. The effect of I-TEQ value by these columns was also studied. The total concentrations of toxic dioxins for the column performance check standard solution were 508.4 ng/mL analyzed by DB-5MS and 515.8 ng/mL analyzed by SP-2331, respectively. The I-TEQ value obtained by both columns was shown to be almost equivalent for the column performance check standard solution and fly ash sample.

Quantification and Resolution of Dioxins on Capillary Columns (캐필러리 컬럼 종류에 따른 다이옥신 이성체 분리능과 정량 특성 변화)

  • Kim, Jong-Guk;Park, Jin-Soo;Kim, Kyoung-Sim;Lee, Geun-Hee;Kim, Shin-Jo
    • Analytical Science and Technology
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    • v.15 no.1
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    • pp.43-53
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    • 2002
  • The analysis of polychlorodibenzo-p-dioxins (PCDDs) and polychlorodibenzo furans(PCDFs) was performed by using four different gas chromatographic columns (SP-2331, DB-5, DB-17 and DB-DIOXIN). The data reported is pertaining to flue gas, fly ash, ambient air, soil and fish. The difference in quantification of samples according to four columns was observed, it was noted that major difference was observed in the flue gas when compared with soil, fly ash, ambient air and fish. The quantification of the same samples according to four columns it was also found that DB-5 column have the highest concentration whereas SP-2331 column showed the lowest concentration. The quantification of DB-17 column for 1,2,3,6,7,8-HxCDF was found to be twice and three times higher when compared with other columns, whereas the quantification of DB-DIOXIN column for 1,2,3,7,8-PeCDD was also found to be over estimated twice when compared with other columns.

Dual Capillary Column System for the Qualitative Gas Chromatography: 2. Comparison between Splitless and On-Column Injection Modes

  • Kim, Kyoung-Rae;Kim, Jung-Han;Park, Hyoung-Kook;Oh, Chang-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.14 no.2
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    • pp.250-255
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    • 1993
  • A dual capillary column system is described for the simultaneous analysis of a given sample and measurement of retention index (RI) and area ratio (AR) values of each peak on two capillary columns of different polarity, DB-5 & DB-1701 from a single injection. Both capillary columns were connected to either a splitless injector or an on-column injector via a deactivated fused-silica capillary tubing of 1 m length and a 'Y' splitter. Both injection modes allowed to measure RI and AR values with high reproducibility (<0.01% RSD) and high accuracy (<10% RE), respectively with the exception that the trace and high boiling solutes required the on-column mode for the accurate quantification and AR comparison. When the dual capillary column system in on-column injection mode was applied to the blind samples containing organic acids, each acid was positively indentified by the combined computer RI library search-AR comparison.

Evaluation of accuracy for measurement of Dioxins (PCDDs/PCDFs) by using certified reference material (CRM) (인증표준물질(Certified reference materials, CRM)을 이용한 이옥신류(PCDDs/PCDFs) 측정의 정확도 평가)

  • Youn, Yeu Young;Park, Deok Hie;Lim, Young Hee;Cho, Hye Sung
    • Analytical Science and Technology
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    • v.22 no.5
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    • pp.376-385
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    • 2009
  • In our study, the accuracy for measurement of seventeen 2,3,7,8-substituted PCDDs/PCDFs in certified reference material (CRM) which is the sample of homogeneous sediment matrix taken from an area known to have significant chemical contamination, particularly PCBs (polychlorinated biphenyls), was evaluated. Though the methodology in this study followed the official method of unintentionally produced persistent organic pollutants (UPOPs) announced by the Ministry of Environment of the Republic of Korea in 2007, there were slight changes using additional purification step by activated carbon column because the interferences of sample were not sufficiently removed when only multi-silica column and alumina column have been used for purification. The |En| number proposed by the Korea Research Institute of Standards and Science was used for a valuation basis of the accuracy. The |En| numbers of seventeen 2,3,7,8-substituted PCDDs/PCDFs have been indicated as 1 and below, they were decided "Pass" in this test, when DB-5MS column and SP-2331 column were used together. Because 1,2,3,7,8-PeCDD and #169-HxCB were not separated on DB-5MS column, the ions of 1,2,3,7,8-PeCDD were selected at M/M+2 instead of M+2/M+4 suggested by EPA 1613. It is possible to distinguish them in HRGC/HRMS analysis.

Separation properties of 209 PCB congeners on capillary columns and identification of PCBs congeners in aroclor standards for source identification (오염원 해석을 위한 폴리염화비페닐류(PCBs) 209 이성체의 컬럼별 분리 특성과 Aroclor 표준품의 이성체 확인)

  • Kim, Kyoung-Soo;Kim, Kyeo-Keun;Kim, Jong-Guk
    • Analytical Science and Technology
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    • v.19 no.4
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    • pp.352-364
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    • 2006
  • This study was performed to search for useful separation properties and elution orders of three GC columns (DB-1, DB-5MS, SPB-Octyl) for 209 PCBs congeners using M-1668A-0.01X-SET of the AccuStandard Inc.. In addition, to confirm the quantitative peak in peak pattern method, the IUPAC Nos. of PCBs congener peaks were identified with 4 Aroclor standards (Aroclor-1242, 1248, 1254 and 1260). The separation property of dioxin-like PCBs congeners by four columns (DB-1, DB-5MS, SP-2331 and SPB-Octyl) was excellent in SP-2331. DB-1 and SPB-Octyl columns are necessary to use with a column of other types.

Identification of Fatty Acids in the Oils of Pine Nuts by GC-MS of Their Picolinyl Esters and 4,4-dimethyloxazoline Derivatives in Combination with Silver-Ion Chromatography

  • Kim, Seong-Jin;Woo, Hyo-Kyeng;Seo, Min-Young;Joh, Yong-Goe
    • Journal of the Korean Applied Science and Technology
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    • v.19 no.3
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    • pp.222-244
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    • 2002
  • A mixture of methyl ester derivatives of fatty acids from the oils of pine nuts was well resolved to five fractions differing by degree of unsaturation by silver ion solid-phase extraction column chromatography ($Ag^{+}$-SEC). Polyunsaturated fatty acid with non-methylene interrupted conjugated double bond (NMiDB) radical held more strongly to silver ions in the column than methylene interrupted conjugated double bond (MiDB) one when they had the same number of double bonds. Although both the picolinyl ester and DMOX derivative provided clear mass ion species powerful enough to elucidate the structure of the polyunsaturated fatty acid (PUFA) with NMiDB and/or methylene interrupted conjugated double bond (MiDB) radical in the oils, the picolinyl ester of PUFA with NMiDB radical did not provide a cluster of mass ions neighboring diagnostic mass ions induced by the double bond in the proximal to the carboxyl group. However, the DMOX derivative of PUFA with NMiDB group as well as MiDB showed abundant mass ion species differing by gaps of 12 amu, which made it possible with greater ease to locate the double bonds in the molecule. The oil contained $C_{18:2{\omega}6}$ (46.2 %) and $C_{18:1{\omega}9}$ (25.4 %) as main components, and considerable amounts of PUFAs with NMiDB radical such as ${\Delta}^{5.\;9.\;12}-C_{18:3}$ (16.0 %), ${\Delta}^{5.\;9}-C_{18:2}$ (2.3 %) and ${\Delta}^{5.\;11.\;14}-C_{20:3}$ (0.8 %).

Isolation and Characterization of Intestinal Immune System Modulating and Anticancer Active Fractions from the Herbal Prescriptions

  • Hwang, Jong-Hyun;Jeong, Jae-Hyun;Yu, Kwang-Won
    • Food Science and Biotechnology
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    • v.18 no.2
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    • pp.323-329
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    • 2009
  • The prescriptions (DB-1-DB-5) were prepared with the active herbal medicines, Acanthopanax senticosus, Glycyrrhiza uralensis, Polygonatum odoratum, and Cichorium intybus. The most active crude polysaccharide fraction (DB-2-3), which was isolated through the fractionation of hot-water extract from DB-2, was significantly reduced by periodate oxidation (52.7 and 63.7%) on intestinal immune system modulating and anticancer activity. When DB-2-3 was further fractionated by column chromatographies, DB-2-3IIc-2 showed the most potent activities. In addition, DB-2-3IIc stimulated the proliferation of bone marrow cells via Peyer's patch in dose-dependent pattern by oral administration. The metastasis of colon 26-M3.1 lung carcinoma had significantly inhibited in mice fed DB-2-3IIc at 1 mg/mouse (43.8%). DB-2-3IIc-2 mainly contained uronic acid (46.1%) and 42.5% of neutral sugar with a small amount of protein (7.6%), and component sugar analysis also showed that DB-2-3IIc-2 was composed Ara, Gal, and GalA (molar ratio; 0.50:0.63:1.00). It may be suggested that activities of DB-2-3IIc-2 are resulted from pectic polysaccharides containing a polygalacturonan moiety with side chain of neutral sugars, such as Ara and Gal.

Trace Analysis as TBDMS Derivatives of Organic Acids in Aqueous Samples (TBDMS 유도체로서 수용액 시료중의 유기산 미량분석 연구)

  • Kim, Gyeong Rye;Kim, Jeong Han;Park, Hyeong Guk
    • Journal of the Korean Chemical Society
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    • v.34 no.4
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    • pp.352-359
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    • 1990
  • An effecient gas chromatographic method is described to be used routinely for the rapid profiling and identification of biochemically important organic acids. It involves the solid-phase extraction of organic acids from aqueous samples using Chromosorb P as the solid sorbent and diethyl ether as the eluting solvent, with subsequent triethylamine treatment. The resulting triethylammonium salts of acids were directly converted to volatile tert-butyldimethylsiyl derivatives, which were simultaneously analyzed by two capillary columns of different polarity, DB-5 and DB-1701, under the identical temperature programming condition. The retention index (RI) and area ratio (AR) values of each peak measured on DB-5 and DB-1701 enabled rapid identification of acids by computer RI library search and AR comparison. The application of the present method to the organic acid profiling of various complex samples is demonstrated.

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Gas chromatographic profiles of rose essential oils: a round-robin test on oil of rose, Chinese Kushui type (Rosa sertata × Rosa rugosa) (장미 정유의 기체 크로마토그래피 분석표: 중국산 쿠스이형 장미유에 대한 재현정밀도 시험)

  • Son, Hyun-Hwa;Lee, Dong-Sun
    • Analytical Science and Technology
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    • v.25 no.4
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    • pp.207-213
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    • 2012
  • Analysis of the aroma constituents present in the rose essential oil of Chinese Kushui type (Rosa sertata ${\times}$ Rosa rugosa) by GC-FID and GC-MS was performed independently as an expert for the inter-laboratory round-robin test to verify reproducibility according to the decision of the preliminary meeting of ISO/TC-54 (Shanghai, Sep. 14-15, 2010). Total 179 peaks (using SPB-1 apolar column), 165 peaks (using DB-624 intermediate polar column), and 162 peaks (using Supelcowax-10 polar column) were separated by GC-FID, respectively. Major constituents (over 5%) by GC-FID were ${\beta}$-citronellol (41.6~46.7%), geraniol (9.7~11.0%), and nerol (3.4~4.5%). ${\beta}$-Citronellol peak was overlapped with nerol peak on SPB-1 and DB-624 columns, whereas the two peaks were separated each other on Supelcowax-10 column. Our results were generally consistent with Chinese data (ISO/DIS 25175); however, a peak of phenethyl alcohol separated by using PEG (Supelco wax) column was found at the quite different retention time. Comparative analysis was conducted using Bulgarian rose (Rosa damascena Miller) oil and perfume. Bulgarian rose oil showed rich amounts of characteristic aroma constituents than the essential oil of Chinese Kushui type.

Analysis of all PCB Congeners in Air Samples by HRGC/HRMS (대기 시료 중 PCBs 전 이성체 분석에 관한 연구)

  • Kim, Kyoung-Soo;Song, Byung-Joo;Kim, Jong-Guk
    • Analytical Science and Technology
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    • v.16 no.4
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    • pp.309-319
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    • 2003
  • This study was performed to describe analysis method of 209 PCB congeners in ambient air samples. The samples were collected by high volume air sampler in Chonju city. Extracted samples were cleaned by silicagel cleanup modified with sulfuric acid and activated carbon cleanup processing. The cleaned samples were analyzed by high resolution gas chromatography and high resolution mass spectrometry (HRGC/HRMS) with DB-5 column (60 m, 0.25 mm i.d., 0.25 m film thickness) to analyze the 209 kinds of PCB congeners. PCBs levels of air samples were detected to the range between 0.003 and $0.163pg-TEQ/m^3$. The PCBs congener of 162 kinds were detected in samples analysed using DB-5 column and 37 kinds peaks were overlapped with congeners more than one. It is difficult to isolate PCB 118/106 and PCB 105/127 in coplanar PCB, so it is likely to overestimate the concentration.. The distribution of coplanar-PCB congeners in origin source samples (Kanechlor and exhaust gas from incinerator) was compared with that in air samples, and PCB 81, PCB 77, PCB 126, and PCB 169 were higher in incinerator samples.