In this study, the performance of fast gas chromatography system was evaluated using VOC standards prepared in both liquid and gaseous phase. When the liquid‐phase VOC standards were analyzed by both direct injection and HS‐SPME method, all the chromatographic separation was completed within 4 minutes. The calibration experiments were conducted further using gaseous standard of BTX. The calibration results derived by direct injection method generally showed good linearities, regardless of phases, while it was not the case for HS‐SPME method. In case of liquid‐phase standard, MDL values for direct injection and HSSPME method were calculated in the range of 0.07~0.19 to 0.63~3.76 ng, respectively. In contrast, MDL values for gaseous standard were 0.27~0.45 and 1.94~6.90, respectively. The reproducibility of our method, when expressed in terms RSE, showed above 5 %. When the sensitivity of different techniques is compared, the calibration slope values of BTX decreased on the order: direct injection of liquid‐phase standard > HSSPME method of liquid‐phase standard > direct injection of gaseous standard > HS‐SPME method of gaseous standard. Although fast GC is very efficient to reduce the total running time significantly, extended studies are desirable to improve its reproducibility.

Gas release behavior from aluminum and Al 7075 alloy powders during heating in argon was investigated by in-situ gas chromatography. Water vapor, hydrogen, carbon mono-oxide were detected as individual evolution spectra against heating temperature and time. The mechanisms of water and hydrogen evolutions were studied in detail for the determination of effective degassing condition. Magnesium in the alloy powder was found to lower the hydrogen evolution temperature to enhance overall hydrogen release.

실리카 입자를 기공 형성제로 사용하여 다공성 키토산 및 키틴 막을 제조하였다. 다공성 막의 제조는 다음의 3단계 절차로서 수행되었다: (1) 키토산 용액에 실리카 입자를 첨가시켜 필름을 형성시킨 후, (2) 이 필름을 알카리 용액에 침지시켜 실리카 입자를 제거하여 다공성의 키토산 막을 제조하였으며, (3) 다공성 키토산 막을 acetic anhydride를 사용하여 아세틸화시킴으로서 다공성 키틴 막을 제조하였다. 물리적 강도가 우수하고, 적절한 순수 투과량을 갖는 다공성 키토산 막과 키틴 막의 최적 제막조건이 제시되었다. 단백질 친화성을 부여하기 위해 다공성 키토산 막에 반응성 염료인 Cibacron Blue 3GA를 고정화시켰으며, BSA 단백질 및 lysozyme 효소의 흡착실험을 수행하여 친화 키토산 막 및 키틴 막의 단백질 결합용량을 측정하였다. 친화 키토산 막의 BSA 단백질 결합용량은 약 22 mg/mL이었으며, 친화 키틴 막의 lysozyme 효소 결합용량은 약 26 mg/mL로서 이는 키토산 또는 키틴을 기반으로 하여 제조된 hydrogel bead의 단백질 결합용량보다 수~수십 배 큰 값으로서, 향후 막여과 크로마토그래피용 친화 막으로의 효과적인 활용이 기대된다.

한외여과막의 분획분자량을 결정하기 위하여 dead-end형 셀내에 평막을 설치하고 분자량 분포가 수천 내지 수백만의 혼합 dextran 수용액으로 투과 실험하였다. 원료 용액과 투과액을 GPC로 분석하여 각 분자량에 대한 배제율을 구하고 90% 배제율에 해당하는 dextran분자량을 분획분자량를 결정하였다. 투과압력을 0.5에서 2.0 bar까지 증가시킬 경우, Millipore사의 PBTK막은 63,000 내지 68,000 daltons로 10% 이내에서 변화하였지만 Millipore사의 PBQK 막 또는 (주)새한의 UE1812막의 분획분자량은 각각 3.5 및 4.3 배 증가하였다. 또한 투과액을 원료용액의 10내지 40%까지 분리막을 증가시키면서 배제율을 측정한 결과, PBTK의 분획분자량은 25% 증가하였다.

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 C18:2Ω6 (46.2 %) and C18:1Ω9 (25.4 %) as main components, and considerable amounts of PUFAs with NMiDB radical such as δ5. 9. 12-C18:3 (16.0 %), δ5. 9-C18:2 (2.3 %) and δ5. 11. 14-C20:3 (0.8 %).

To investigate the optimum condition of 3-monochloro-l,2-propanediol(MCPD) analysis, gas chromatography with electron capture detector was-used. Determination of MCPD derivatized with phenylboric acid was more effective than that of underivatized MCPD. In derivatization of MCPD with phenyl boric acid, there were no significantly different between boiling for 2min at 90℃ and vortexing for Smin at room temperature. Extrelut column was suitable for extraction of MCPD diluted in 20% NaCl solution and recovery rates were higher than direct extraction of MCPD with ethyl acetate. But, the method of direct extraction of MCPD with ethyl acetate was useful for rapid and qualitative analysis. The sample extracted in soysauce(ganjang) was derivatized with phenylboric acid and analyzed by gas chromatography-mass selective detector. That was confirmed as MCPD-phenylboronate.

Analytical method for preservatives in food was developed using gas chromatography/mass spectrometry (GC/MS). Propionic acid, sorbic acid, benzoic acid, ethyl salicylate, ethyl p-hydroxy benzoate, iso-propyl p-hydro benzoate, n-propyl p-hydroxy benzoate, iso-butyl phydroxy benzoate, n-butyl p-hydroxy benzoate, p-hydroxy benzoic acid and dehydro acetic acid were extracted from cooling beverage with diethyl ether. The polar hydroxyl and carboryl groups of food preservatives were derivatized with N-methyl-N-tent-butyldimethylsilyl-trifluoroacetamide (MTBSTFA) to form the corresponding tert-butyldimethyl-silylated derivatives, and submitted to GC/MS analysis. The mass spectra of the derivatives were investigated for the selection of monitoring ions for multi-residue analysis of 11 preservatives by GC/MS. The macro program was also developed for the qualitative analysis of these preservatives in food.

난포액내 함유되어 있는 단백질성분 중에서 sucrose 층으로부터 정자의 swim-up 이동을 자 극하는 성분을 분리하기 위하여 paper chromatography (PC) 및 reverse phase column (RPC) 과 superose column (SC)를 이용한 액체 chromatography의 분리효과를 조사하였던 바 결과는 다음과 같다. 1. Chromatography용 paper로 분리한 각 band 의 성분은 첨가농도가 증가할수록

HPLC에 의한 주요 aflatoxins(afatoxin B₁, B₂, G₁ 및 G₂)의 동시 분석에서 postcolumn 유도체화법을 시도하였다. Electrochemical cell(Kobra-cell)을 사용한 postcolumn 유도체화법은 기존의 precolumn 유도체화법보다 분석시간을 단축하였으며(약 1/2 단축), 더 안전하고, 향상된 분석능을 보였다. Aflatoxin B₁과 G₁의 경우 10~100 ppb에서, 그리고 B₂와 G₂의 경우 3~30 ppb에서 직선성을 나타내었다. Aflatoxin B₁과 G₁은 각각 88.9% 및 100.5%로 양호환 회수육을 보였다. Aflatoxin B₂와 G₂의 경우 분리도는 우수하였으나 회수율에 있어서 변이가 크게 나타났다.

Polysulfone 재질의 다공성 평판막 및 실관막에 키토산 피막층을 형성시킨 후 반응성 염료인 Cibacron Blue 3GA를 고정화시켜 human serum albumin(HSA)의 결합용량이 최대 70 μg/cm2인 단백질 친화성 막을 제조하였다. 친화성 평판막 모듈을 대상으로 HSA에 대한 용출 크로마토그래피 실험을 수행하여 eluent 용액의 최적 환경조건을 결정하였는바, 1M KCl이 첨가된 농도 0.06 M, pH 10의 universal buffer를 eluent로 사용했을 때 리간드와 결합된 단백질의 용출이 가장 우수하였다. 친화성 평판막 및 실관막 모듈을 대상으로 HSA의 전열 크로마토그래피 실험을 수행하여 단백질에 대한 동적 결합용량을 측정하였다. 이 결과 동적 결합용량은 평판막 모듈의 경우에는 loading 용액의 유량과 HSA의 농도가 증가함에 따라 평형 결합용량 값으로부터 크게 감소하였으나, 실관막 모듈의 경우에는 loading 용액의 유량과 HSA의 농도에 관계없이 항상 평형 결합용량 수준을 유지하였는바, 따라서 실관막 모듈이 평판막 모듈보다 단백질 친화성 크로마토그래피 분리관으로서 더 효과적이었다

The prevention of oxidative degradation in fats and oils is largely controlled by the use of synthetic phenolic antioxidants. Antioxidants, BHA: 2-&3-tert-butyl-4-hydroxyanisol, BHT: 3,5-di-tert-butyl-4-hydroxytoluene, TBHQ: tert-butylhydroquinone, PG: propyl gallate, PTG: pentyl gallate, OG: octyl gallate, were extracted from fatty foods with hexane and from hexane layer to presaturated acetonitrile with hexane. The polar phenolic hydroxyl groups of antioxidants were silylated with MSTFA and injected to Gas Chromatography/Mass Spectrometry. The calibration plots were linear in the investigated range, 0.1-10.0 ug/g. The limit of detection for 6 phenolic antioxidants was 0.1 ug/g. Recoveries and reproducibilities from samples fortified at 1.0 ug/g were in the range of 70-90% and 0.5-13%, respectively. The simultaneous determination of phenolic antioxidants in fatty foods using GC/MS-SIM mode and macro program was described.

Triacylglycerols of the seeds of Ginkgo biloba have been resolved by high-performace liquid chromatography(HPLC in the silver-ion and reverse-phase modes. The fatty acids were identified by a combination of capillary gas chromatography and gas-chromatography /mass spectrometry as the methyl and /or picolinyl ester. The main components are C18:2Ω6(39.0mol%), C18:1Ω7(asclepic acid 21.5mol%), and C18:1Ω9(oleic acid, 13.8mol%). Considerable amounts of unusual acid such as C20:3δ5,11,14 (5.7mol%), C18:2δ5,9(2.8mol%), and C18:3δ5,9,12(1.6mol%), were checked. In addition, an anteiso-branched fatty acid, 14-methylhexadecanoic acid, was also present as a minor component(0.9 mol%). The triacylglycerols were separated into 17 fractions by reverse-phase HPLC, and the fractionation was achieved according to the partition numnber(PN) in which a δ5-non methylene interrupted double bond(5-NMDB) showed different behaviour from a methylene interrupted double bond in a molecule with a given cahinlength. Silver-ion HPLC exhibited excellent resolution in which fractions(23 fractions) were resolved on the basis of the number and configuration of double bonds. In this instance, the strength of interaction of a δ5-NMDB system with silver ions seemed to be weaker than a methylene interrupted double bond system. The principal triacylglycerol species are as follows ; (C18:2Ω6)2/C18:1Ω7, C18:1Ω9/C18:1Ω7/C18:2Ω6, (C18:1Ω7)2/C18:2Ω6, C16:1Ω7/C18:1Ω9/C20:3δ5,11,14, C16:1Ω7/C18:1Ω7/C20:3δ5,11,14, C18:1Ω9/C18:1Ω7/C18:2Ω6, C18:1Ω9/C18:2δ5,5/C20:3δ5,11,14, (C18:1Ω7)2/C18:2Ω6 and (C18:1Ω9)2/C18:2Ω6, while simple triacylglycerols without C18:2Ω6)3 were not present. Stereospecific analysis showed that fatty acids with δ5-NMDB system and saturated chains were predominantly located at the site of sn-3 carbon of glycerol backbones. It is evident that there is asymmetry in the distribution of fatty acids in the TG molecules of Ginkgo nut oils.

Sulfonamides, a therapeutically important group of antimicrobial drugs, are widely used to treat and prevent the acute systemic and skin infections in dairy cattle. They also pose an economic hazard through inhibition of growth of dairy starter cultures. This study was carried out to compare four screening methods for detection of sulfamethazine in milk and determine the positive milk sample by HPLC method. Sulfamethazine was used to spike at five levels of sulfamethazine. The Lac-Tek test and CharmII test were also consistent better than TTCII test and Delvo SP test in sulfamethazine detection. Analysis probabilities of obtaining a positive response with TTCII test and Delvo SP test assay at 50 ppb sulfamethazine level in milk samples were only 14%, 42% each. Whereas using the Lac-Tek test and CharmII test would have resulted in 100% identification of the five levels. Determination of sufamethazine using the HPLC method in the spiked milk were 10.64, 19.30, 30.76, 38.83 and 50.23 ppb, respectively.