• 대한화학회지
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• 제58권3호
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• pp.283-288
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• 2014

A column solid phase extraction procedure based on modified polyurethane foam (PUF) by a newly synthesized Schiff base ionophore, named 2,2'-{iminobis[propane-3,1-diylnitrilo(1E)prop-1-yl-1-ylidene]}diphenol, was developed for preconcentration step of trace amounts determination of copper ions in water samples by atomic absorption flame spectroscopy. The influence of parameters on the adsorption process such as sample pH, amount of modified PUF packed in the column, type and volume of stripping reagent and its flow rate were investigated and optimized. Under optimum experimental conditions, the calibration graph was linear in a relatively wide range ($0.005-210{\mu}g/ml$) with a limit of detection $0.002{\mu}g/ml$ of copper. The proposed method allows achieving to a concentration factor of >133. The capacity of a column (1.6 cm i.d.) packed by 6 g of PUF modified by 12 mg of the Schiff base was found to be $247.7({\pm}2.1){\mu}g$ of copper. It was found that the adsorption process was highly selective towards copper ions with respect to some associated metal ions. The presented procedure was successfully applied for determination of copper in some water samples.

• 한국수산과학회지
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• 제39권6호
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• pp.441-446
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• 2006

Volatile flavor compounds in meat of the blue crab Portunus trituberculatus were compared using vacuum simultaneous steam distillation-solvent extraction (V-SDE) and solid phase microextraction (SPME)/ gas chromatography (GC)/ mass selective detection (MSD) methods. A total of 100 volatile flavor compounds were identified by both methods: 77 by V-SDE and 59 by SPME. These compounds were composed of 17 aldehydes, 12 ketones, 19 alcohols, 5 esters, 4 sulfur-containing compounds, 6 nitrogen-containing compounds, 23 aromatic compounds, 6 hydrocarbons, 2 terpenes, and 6 miscellaneous compounds. Although more compounds were detected using V-SDE than using SPME, the levels of all groups detected, except esters, were higher using SPME than using V-SDE. In addition to trimethylamine, aldehydes, and aromatic compounds, the S- and N-containing compounds with low thresholds are thought to have positive roles for flavors in the meat of the blue crab.

• 대한화학회지
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• 제52권2호
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• pp.133-139
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• 2008

고상추출 매질로 bis-(2-ethylhexyl)phthalate를 포함하는 polyvinyl chloride막을 사용하여 카드뮴의 잔유양 을 측정하기 위한 새로운 민감하고 선택적인 분광광도법을 연구하였다. Bis-(2-ethylhexyl)phthalate는 가소제로 사용되 었다. 수용액에서 Cd(II)은 색을 가진 Cd(II) - I- - MG 착체(여기서 MG는 malachite green이다). 형으로 있는 막에 의해 트랩되었고, 카드뮴 착체는 막에 농축되었다. 그린색의 막의 흡수는 분광광도법을 사용하여 629 nm에서 측정되었 다. 카드뮴 농도는 Cd(II) 농도와 25분 동안 착색후 막의 흡수 사이에 관계로 나타내는 검정곡선으로부터 계산하였다. 검정곡선은 시험용액에서 10-760 μgL-1 cadmium 범위에서 선형이었다. 3Sbl criterion의 검출한계는 1.8199 μgL-1 상 대 표준편차(RSD)는 4% (n=5).보다 적다. 제안된 방법은 Tadjan강(Sari-Iran), 에 있는 카드뮴의 잔량을 성공적으로 측 정하였다. 28.7 μgL-1의 평균 값을 얻었다.

• 한국미생물·생명공학회지
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• 제19권2호
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• pp.135-139
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• 1991

Tridecanedioic acid (DC-13), starting material of the valuable musk ethylene brassylate, was obtained from n-tridecane by the Candida tropicalis mutant. The mutants were first obtained from primary screening step using the selective medium and then solid phase extraction sampling method was used for the selective isolation of organic acids from the cultured media of mutants. The resulting acids were directly converted to volatile tert-butyldimethyl silyl delivatives, which were then analyzed by gas chromatography. The efficient GC profiling method was used for the rapid identification of the mutant producing DC-13 in large quantity, and for the optimization of the culture conditions of mutant. The optimal culture conditions were found as follows: pH 8.0, 30$^{\circ}C$, 250rpm, 48hour of culture and $(NH_4)_2HPO_4$ as nitrogen source.

• Bulletin of the Korean Chemical Society
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• 제28권3호
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• pp.373-378
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• 2007

A micro organism Agrobacterium tumifacient as an immobilized cell on a solid support was presented as a new biosorbent in a simple and sensitive spectrophotometry determination of Ni(II) in various samples using 4-hydroxy benzaldehyde-4-bromophenyl hydrazone as a color developing agent (λmax 497 nm) at pH 4.0 ± 0.2. Beer's law was obeyed over the range of 0.01-0.1 μg L-1. The molar absorptivity and Sandell's sensitivity were 1.285 × 105 L mol-1cm-1 and 0.007245 μg cm-2 respectively. Under these conditions, the preconcentration factor obtained was 82, and the detection limit achieved was 0.05 μg L-1. The detailed study of various interfering ions made the method more sensitive and selective. The recovery of Ni(II) from various samples range from 97.75 to 99.35%. The present method was successfully applied for the determination of Ni(II) in spiked, natural water and alloy samples. The proposed method was compared with reported methods in terms of Student's ‘t'-test and Variance ratio ‘f'-test which indicates that there is no significant difference between proposed and literature method at 95% confidence level.

• 한국식품영양과학회지
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• 제31권1호
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• pp.26-31
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• 2002

Pinus densiflora(2엽송) 1년생을 채취하여 가지, 잎, 새순 부분으로 구분하고, 시료병에 넣어 밀봉한 뒤, solide phase microextraction (SPME)과 dynamic headspace analysis(DHA)를 이용하여 휘발성 성분을 분리, 동정하였다. SPME와 DHA의 결과를 terpenes의 구성 성분에 따라 monoterpenes과 sesquiterpenes, oxygenated terpenes으로 나누어 조성비를 살펴보면, monoterpenes의 조성은 잎의 경우 각각 66.7%와 14.3%, 새순은 90.6%와 0.7%, 가지에서는 90.6%와 1.2%로 나타났다. Sesquiterpenes의 함량은 SPMe의 결과에서만, 잎이 25.8%, 가지 4.4%, 새순 1.5%로 나타났다. 산소를 함유하고 있는 terpenes의 함량은 새순 부위가 4.7%, 79.0%로 나타났으며, 가지 부위는 3.7%와 70.4%, 잎에서 1.0%와 50.7%를 각각 차지하였다. SPME의 결과는 이전의 용매추출을 통한 결과와 다소 비슷한 양상을 보였으며, DHA의 결과는 10$0^{\circ}C$이상의 고비점 화합물들이 나타나지 않은 반면, 5$0^{\circ}C$이하의 저비점 화합물이 15개 분리되었다.

• Mass Spectrometry Letters
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• 제4권1호
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• pp.18-20
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• 2013

Headspace solid phase micro-extraction gas chromatography/flame ionization detection (HS-SPME-GC/FID) method was compared with headspace gas chromatography/mass selective detection (HS-GC/MS). Organic solvent-spiked urine as well as urine samples from workspace was analyzed under optimal condition of each method. Detection limit of each compound by HS-SPME-GC/FID was $3.4-9.5{\mu}g/L$, which enabled trace analysis of organic solvents in urine. Linear range of each organic solvent was $10-400{\mu}g/L$, with fair correlation coefficient between 0.992 and 0.999. The detection sensitivity was 4 times better than HS-GC/MS in selected ion monitoring (SIM) mode. Accuracy and precision was confirmed using commercial reference material, with accuracy around 90% and precision less than 4.6% of coefficient of variance. Among 48 urine samples from workplace, toluene was detected from 45 samples in the range of $20-324{\mu}g/L$, but no other solvents were found. As a method for trace analysis, SPME HS GC/FID showed high sensitivity for biological monitoring of organic solvent in urine.

• Environmental Engineering Research
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• 제12권3호
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• pp.93-100
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• 2007

I improved an analytical method for determining trace amounts of eleven phenolic endocrine-disrupting chemicals (11 phenolic EOCs) in human urine. The 11 phenolic EOCs were subjected to hydrolysis and then to solid phase extraction with a XAD-4 column. Alkylphenols, chlorophenols, and bisphenol A in XAD-4 column were eluted with acetonitrile, and the eluate was concentrated under a nitrogen stream, and then tert-butyldimethylsilylation. Separation and determination were done by gas chromatography, using mass spectrometry operating in the selective ion monitoring mode for quantitation. For tert-butyldimethylsily (TBDMS) derivatization the recoveries were $91.2{\sim}125.9%$, the limits of quantitation (LOQ) for the 11 phenolic EOCs in the nanogram-per-milliliter range ($0.025{\sim}1.000\;ng/mL$) were thus achieved by using 1 mL of urine, and the SIM responses were linear with the correlation coefficient varying by $0.9300{\sim}0.9943$. Based on the results for urine samples from unexposed individuals, 4-tert-octylphenol and pentachlorophenol were detected in hydrolysed urine sample. Other alkylphenols, chlorophenols and bisphenol A were not detected.

• Mass Spectrometry Letters
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• 제3권3호
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• pp.78-81
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• 2012

The hydrophobic hydrocarbon chain and the polar sulfate group confer surfactant properties and enable them to be used as anionic surfactants. Anionic surfactants (AS) are known for their adverse impact on environment, particularly on aquatic ecosystem. In the present study a fast, sensitive and selective method for the determination and subsequent quantification of six anionic surfactants was developed using hydrophilic interactive liquid chromatography (HILIC) coupled to a electrospray ionization (ESI) mass spectrometer (MS), in the concentration range 15-20 ${\mu}g/L$. The capability of the method was established using regression analysis and ANOVA. The method performance was evaluated by analyzing real time surface water spiked with 1-dodecyl hydrogen sulfate at 15 ${\mu}g/L$. Combined efficiency of solid phase extraction and MS detection established recovery of 89% in presence of natural matrix. These results point out that HILIC coupled to multistage MS procedures can be a powerful technique for environmental applications concerning the screening of polar contaminants.

• 분석과학
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• 제28권1호
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• pp.17-25
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• 2015

A rapid, sensitive and specific method was developed and validated using electrospray ionization (ESI) tandem mass spectrometry (LC-MS/MS) for determination of misoprostol acid in human plasma. Misoprostol $acid-d_5$ was used as in internal standard (IS). The analyte and IS were extracted by simple one step solid phase extraction (SPE). Linearity in plasma was obtained over the concentration range 10~3000 pg/mL and lower limit of quantification (LLOQ) was identifiable and reproducible at 10 pg/mL. The intra- and inter-day precision values were below 9% and the accuracy was ranged from 93.81% to 102.02% at all four quality control samples. The method was has been successfully applied for routine assay to support pharmacokinetic study of misoprostol acid in human plasma after an oral administration of 0.4 mg misoprostol.