• 한국환경과학회지
• /
• 제23권6호
• /
• pp.1037-1047
• /
• 2014

A highly sensitive analytical method based on stir bar sorptive extraction (SBSE) technique and gas chromatography/tandem mass spectrometry (GC/MS-MS) has been developed, allowing the simultaneous multi-analyte determination of seven UV filters in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 40 mL of water sample at pH 3 and stirred at 1,100 rpm for 120 min. Other SBSE parameters (salt effect and presence of organic solvent) were optimised. The method shows good linearity (coefficients > 0.990) and reproducibility (RSD < 12.9%). The extraction efficiencies were above 84% for all the compounds. The limits of detections (LOD) and limits of quantification (LOQ) were 2.1~8.6 ng/L and 6.8~27.5 ng/L, respectively. The developed method offers the ability to detect 8 UV filters at ultra-low concentration levels with only 40 mL of sample volume. Matrix effects in tap water, river water, wastewater treatment plant (WWTP) final effluent water and seawater were investigated and it was shown that the method is suitable for the analysis of trace level of 7 UV filters except of benzophenone (BP). The method developed in the present study has the advantage of being rapid, simple, high-sensitive and both user and environmentally friendly.

• 대한유전성대사질환학회지
• /
• 제17권2호
• /
• pp.39-47
• /
• 2017

Purpose: A sensitive gas chromatography mass spectrometry (GC-MS) method was developed for screening of fatty acid oxidation disorders. Methods: The assay utilized a simple protein precipitation with sulfosalicylic acid followed by tert-butyl dimethylsilyl (TBDMS) derivatization of hydroxyl functional group by N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide (MTBSTFA). Results: Calibration curves of spiked pooled plasma showed a linear relationship in the range of 0.01 ng -2 mg with correlation coefficient value greater than 0.98. Limits of detection (LOD) and limits of quantification (LOQ) were found in the range of 0.9-8.8 ng and 9-88 ng, respectively. Conclusion: The new developed method might be useful for a rapid, sensitive screening of inherited fatty acid oxidation disorders. In addition, the method expected to be one of the alternative method for screening newborns of metabolic disorders in the laboratories where expensive MS/MS is unavailable.

• 한국대기환경학회지
• /
• 제18권2호
• /
• pp.127-137
• /
• 2002

Phenolic compounds in air are toxic even at their low concentrations. We had evaluated a total of five phenolic compounds (Phenol, o-Cresol, m-Cresol, 2-Nitrophenol and 4-Chloro-3-methylphenol) in artificial air using a combination of ATD/GC/MS. To compare the adsorption efficiency of these phenolic compounds, three adsorbents (Tenax TA, Carbotrap and Carbopack B) were tested. Tenax TA adsorbent was most effective of all the adsorbents used for the efficiency test. Five phenolic compounds were found to be very stable on adsorbent tubes for 4 days at room temperature. Detection limit of five phenolic compounds ranged from 0.05 to 0.08 ppb (when assumed to collect 10 L air). The calibration curve was linear over the range of 22∼ 164 ng. The reproducibility was less than 4%. Sampling of duplicate pairs (DPs) was made to demonstrate duplicate precision and sampling efficiency.

• Journal of Microbiology and Biotechnology
• /
• 제16권7호
• /
• pp.1139-1143
• /
• 2006

Various techniques and strategies have been developed for the identification of intracellular metabolic conditions, and among them, isotope balance-based flux analysis with gas chromatography/mass spectrometry (GC/ MS) has recently become popular. Even though isotope balance-based flux analysis allows a more accurate estimation of intracellular fluxes, its application has been restricted to relatively small metabolic systems because of the limited number of measurable metabolites. In this paper, a strategy for incorporating isotope balance-based flux data obtained for a small network into metabolic flux analysis was examined as a feasible alternative allowing more accurate quantification of intracellular flux distribution in a large metabolic system. To impose GC/MS based data into a large metabolic network and obtain optimum flux distribution profile, data reconciliation procedure was applied. As a result, metabolic flux values of 308 intracellular reactions could be estimated from 29 GC/ MS based fluxes with higher accuracy.

• 한국식품위생안전성학회지
• /
• 제10권4호
• /
• pp.239-247
• /
• 1995

Analytical method for saccharin in foods was developed using gas chromatography/mass spectrometry(GC/MS). Methylation with diazomethane, acetylation with MBTFA, and silylation with MSTFA and MTBSTFA were compared. Methylation of saccharin produced N-methylated saccharin as the major product and O-methylated saccharin as the minor one. Silylation of saccharin with MSTFA and MTBSTFA reasulted in the formation of the correponding O-silylated products, respectively. The derivatization of saccharin was optimized with MSTFA. The ions at m/z 240, 255, and 166 were monitored to characterize saccharin.

• 분석과학
• /
• 제7권1호
• /
• pp.41-52
• /
• 1994

아미노산 중 alanine, threonine, isoleucine, leucine, aspartic acid, methionine, glutamic acid, tyrosine을 대상으로 열처리, 산처리, UV 광선 조사, 효소(trypsin)의 영향을 살펴보고 6N-HCl, $105^{\circ}C$로 가열했을 때 이성화하는 정도를 측정하였다. 또한 Mass Spectrometer를 이용할 때 각 아미노산의 fragment되는 과정을 조사하여 GC에서 서로 겹칠 때 분석하는 법을 개발하였다. HPLC에서 cyclodextrin bonded phase를 이용해서 dansyl amino acid의 분리를 시도하였다.

• 한국해양바이오학회지
• /
• 제15권2호
• /
• pp.96-102
• /
• 2023

Salicornia herbacea, a noted halophyte, has been widely researched for its diverse physiological activities. The continuous exploration of its compounds is essential. This study employed gas chromatography (GC) coupled with mass spectrometry (MS) for qualitative analysis. This involved pretreatment including trimethylsilyl (TMS) derivatization of the S. herbacea extract, facilitating its GC analysis. Five compounds, including various fatty acids and β-sitosterol, were identified by direct analysis of the methanol extract of S. herbacea without pretreatment by GC-MS. Conversely, the analysis of the TMS-derivatized extract revealed 28 distinct peaks. Quantitative analysis further indicated that the predominant compounds in the S. herbacea extract were sugars and sugar derivatives, notably glucose, fructose, and glucitol. The collective concentration of these sugars and its derivatives amounted to 116.45 mg/g, representing 11.6% of the dry weight of the raw S. herbacea. Following sugars and their derivatives, fatty acids constituted the next most abundant group of compounds. However, the presence of amino acids and organic acids was relatively low.

• 분석과학
• /
• 제20권2호
• /
• pp.91-108
• /
• 2007

토양 중 PCBs 분석방법을 검토하기 위해 우리나라 토양오염공정시험방법 및 선진국의 분석방법을 비교 검토하고 결과를 근거로, 추출 및 전처리방법, 칼럼정제방법, 분석용 칼럼 조건, 기기분석 조건 및 정량방법을 검토하였다. 또한 검토된 방법에 따라 토양 중 PCBs 세부분석지침(안)을 제시하고, 제시된 세부분석지침(안)에 의해 PCBs 제품으로 오염시킨 토양 5건 시료와 토지이용도별 및 오염원별 23건의 시료를 전처리하여 분석하였다. 기체크로마토그래피/전자포획검출법(GC/ECD)에 의한 토지이용도별 및 오염원별 PCBs 분석결과는 모든 시료에서 피크패턴(GC/ECD)을 확인 할 수 없었으나, 기체크로마토그래피/질량분석법(GC/MS)에 의한 개별이성체 정량결과는 $0.002{\sim}0.487{\mu}g/kg$ 범위로 검출되었다.

• 분석과학
• /
• 제21권6호
• /
• pp.495-501
• /
• 2008

GC-MS 의 기존 인터페이스와 새로운 인터페이스의 차이점과 유용성을 판단하기 위하여 Agilent 5973 GC-MS의 capillary direct interface를 떼어내고 GC와 질량분석기 사이에 실리콘 membrane을 장착하여 membrane interface GC-MS의 분석 유용성을 조사하였다. 최대 $4.7m{\ell}/min$ 까지 헬륨 운반기체유량을 올릴 때 질량분석기의 진공도는 거의 영향을 받지 않으며, 피이크끌림 현상이 줄어들고 머무른시간이 줄어드는 빠른 분석을 보였다. Membrane 의 두께를 $127{\mu}m$에서 $75{\mu}m$으로 줄일 때 분리능이 향상 되며, membrane interface의 온도를 올릴 때 분리능과 감도가 향상되었다. 그러나 membrane interface GCMS는 질량/전하 비 73, 147에서 바탕이온이 발생하는 것과 기존의 capillary direct insertion interface보다 낮은 감도와 peak tailing에 의한 낮은 분리능의 문제점을 갖는다.

• Preventive Nutrition and Food Science
• /
• 제7권1호
• /
• pp.5-11
• /
• 2002

The comparison of the volatile flavor components from Korean and Japanese Satsuma mandarin (C. unshiu Marcov. forma Miyagawa-wase) peel oils, isolated by cold-pressing, was performed by gas chromatography, mass-spectrometry and gas chromatography-olfactometry (GC-O). Eighty-five volatile components were identified in each oil by GC and GC-MS. Forty-three components were detected in each oil by GC-O. The total amount of monoterpene hydrocarbons was 95.88% (Korean mandarin) and 95.29% (Japanese mandarin). Limonene, ${\gamma}$-terpinene, myrcene and $\alpha$-pinene were the main components of the cold-pressed oils from the both samples. The volatile composition of the Japanese mandarin was characterized by a higher content of sesquiterpene hydrocarbons, especially bicyclogermacrene, $\alpha$-humullene and valencene. The volatile composition of two samples can easily be distinguished by the percentages of aldehydes, ketones and esters, which were found at higher levels in the Japanese mandarin. The sweet and fruity flavor was stronger in the Korean mandarin oil while herbaceous flavor was stronger in Japanese sample. From GC-O data it is suggested that the sweet and fruity flavor of the Korean mandarin resulted from terpinolene and linalool, and the herbaceous note of the Japanese mandarin from $\alpha$-humullene, nepal, ι-carvone and perill aldehyde.