• Bulletin of the Korean Chemical Society
• /
• 제34권6호
• /
• pp.1745-1750
• /
• 2013

A novel green aqueous mobile phase modified with room temperature ionic liquids (RTILs) was employed in the absence of volatile organic solvents or ion-pairing reagents to analyze thiamine, a very polar compound, by reverse phase high performance liquid chromatography (RP-HPLC). Due to its strongly hydrophilic nature, thiamine was eluted near the column dead time ($t_0$) using a mobile phase without adding RTILs or ion-pairing reagents, even if a 100% aqueous mobile phase, which has weak elution power under reverse phase conditions, was used. Thus, 1-ethyl-3-methyl-imidazolium hexafluorophosphate ([EMIM][$PF_6$]), which has the strongest chaotropic effect, was selected as a mobile phase additive to improve retention and avoid baseline disturbances at $t_0$. Various mobile phase parameters such as cation moiety, chaotropic anion moiety, pH and concentration of RTILs were optimized to determine thiamine at the proper retention time. Method validation was performed to assess linearity, intra- and inter-day accuracy and precision, recovery and repeatability; all results were found to be satisfactory. The developed method was also compared to the current official United States Pharmacopoeia (USP) and Korean Pharmacopoeia (KP) methods using an organic mobile phase containing an ionpairing reagent by means of evaluating various chromatographic parameters such as the capacity factor, theoretical plate number, peak asymmetry and tailing factor. The results indicated that the proposed method exhibited better efficiency of thiamine analysis than the official methods, and it was successfully applied to quantify thiamine in pharmaceutical preparations.

• 분석과학
• /
• 제9권3호
• /
• pp.292-301
• /
• 1996

산화환원반응 탐침제로, poly ether 꼬리가 결합된 Cobalt(II)bipyridine 착물을 합성 하였고, 이들 화합물의 느린 확산계수와 불균일 전자이동을 설명하였다. $Co(bpy(ppgm)_2)_{3^-}(ClO_4)_2$에 전해질 $LiClO_4$가 혼합된 neat 상태의 산화반응에 대한 확산계수는 $1.5{\times}10^{-15}cm^2/s$ 였다. 이 화합물들의 불균일 전자이동 속도상수들은 확산계수와 관련이 있었다. 확산계수의 감소에 따라 속도상수(k)의 감소가 일어났다. 강한 이온쌍을 형성하는 $ClO{_4}^-$의 화합물은 약한 이온 쌍을 형성하는 $CF_3COO^-$ 화합물보다 확산계수가 훨씬 작았다.

• Preventive Nutrition and Food Science
• /
• 제4권3호
• /
• pp.171-174
• /
• 1999

For monitoring lipid oxidation development in cooked ground pork during refrigerationm, malonaldehydethiobarbituric acid(MA-TBA) contents were measured using high performance liquid chromatography(HPLC). As the oxidation proceeded during refergeration, TBA-reaction substances(TBARS) absorbances increased and the corresponding HPLC peak areas also increased proportationately. The correlation coefficient between the HPLC peak areas and MA-TBA absorbance were 0.9979. The treatemtn of cetrimide, an ion pairing agent, gave a complete resolution of the MA-TBA complex and the butanol extraction of the complex increased its recovery by 37.8%. Both cetrimide treatment and butanol extraction are essential steps for analyzing MA-TBA complex in ground pork wiht HPLC. A reliable and specific measurement of NA-TBA in ground pork was successfully performed using HPLC.

• Bulletin of the Korean Chemical Society
• /
• 제29권1호
• /
• pp.117-121
• /
• 2008

Pseudo-first-order rate constants (kobsd) have been measured spectrophotometrically for nucleophilic substitution reactions of 5-nitro-8-quinolyl benzoate (5) with alkali metal ethoxides, EtO?M+ (M+ = Li+, Na+ and K+) in anhydrous ethanol (EtOH) at 25.0 0.1 C. The plots of kobsd vs. [EtO?M+] exhibit upward curvatures, while the corresponding plots for the reactions of 5 with EtO?Na+ and EtO?K+ in the presence of complexing agents, 15-crown-5-ether and 18-crown-6-ether are linear with rate retardation. The reactions of 5 with EtO?Na+ and EtO?Li+ result in significant rate enhancements on additions of Na+ClO4, indicating that the M+ ions behave as a catalyst. The dissociated EtO and ion-paired EtOM+ have been proposed to react with 5. The second-order rate constants for the reactions with EtO (kEtO) and EtOM+ (kEtOM+) have been calculated from ion-pairing treatments. The kEtO and kEtOM+ values decrease in the order kEtONa+ > kEtOK+ > kEtOLi+ > kEtO, indicating that ion-paired EtOM+ species are more reactive than the dissociated EtO ion, and Na+ ion exhibits the largest catalytic effect. The M+ ions in this study form stronger complex with the transition state than with the ground state. Coordination of the M+ ions with the O and N atoms in the leaving group of 5 has been suggested to be responsible for the catalytic effect shown by the alkali metal ions in this study.

• Carbon letters
• /
• 제10권4호
• /
• pp.305-313
• /
• 2009

In this study, the adsorption of toxic pollutants onto cetyltrimethylammonium kaolin (CTAB-Kaolin) is investigated. The organo-kaolin is synthesized by exchanging cetyltrimethylammonium cations (CTAB) with inorganic ions on the surface of kaolin. The chemical analysis, the structural and textural properties of kaolin and CTAB-kaolin were investigated using elemental analysis, FTIR, SEM and adsorption of nitrogen at $-196^{\circ}C$. The kinetic adsorption and adsorption capacity of the organo-kaolin towards o-xylene, phenol and Cu(II) ion from aqueous solution was investigated. The kinetic adsorption data of o-xylene, phenol and Cu(II) are in agreement with a second order model. The equilibrium adsorption data were found to fit Langmuir equation. The uptake of o-xylene and phenol from their aqueous solution by kaolin, CTAB-kaolin and activated carbon proceed via physisorption. The removal of Cu(II) ion from water depends on the surface properties of the adsorbent. Onto kaolin, the Cu(II) ions are adsorbed through cation exchange with $Na^+$. For CTAB-kaolin, Cu(II) ions are mainly adsorbed via electrostatic attraction with the counter ions in the electric double layer ($Br^-$), via ion pairing, Cu(II) ions removal by the activated carbon is probably related to the carbon-oxygen groups particularly those of acid type. The adsorption capacities of CTAB-kaolin for the investigated adsorbates are considerably higher compared with those of unmodified kaolin. However, the adsorption capacities of the activated carbons are by far higher than those determined for CTAB-kaolin.

• 대한화학회지
• /
• 제42권4호
• /
• pp.416-421
• /
• 1998

귀금속-티아크라운에테르 착물들의 역상 이온쌍 고성능 액체크로마토그래피(RPIP-HPLC)용리 거동에서 이온쌍 시약의 농도와 리간드 종류 효과를 연구하였다. 귀금속 이온 분석의 선택성은 사용한 티아크라운에테르의 고리를 구성하는 원자들의 수가 작을수록 좋았고, 귀금속-티아크라운에테르 착물의 용리 메카니즘은 이동상 중 이온쌍 시약인 도데실술폰산나트륨염(SDS)의 농도가 10 mM 이하일 경우 이온쌍 형성 메카니즘으로, 10 mM 이상일 경우 미쎌 형성 메카니즘으로 설명되었다. 결론적으로 몇 가지 귀금속-티아크라운에테르 착물들을 최적 조건에서 성공적으로 분리하였고, 흑백사진 정착액 중 Ag(Ⅰ) 이온 분리와 정량에 유용함을 증명하였다.

• 한국광학회지
• /
• 제12권3호
• /
• pp.205-211
• /
• 2001

본 논문에서는 최근 주목받고 있는 장파장 EDFA(Erbium-Doped Fiber Amplifer)에서의 성능 분석, 특히 전력변환률(Power Conversion Efficiency)의 예측을 위한 밀도반전이 고정된 상태에서의 black box 모델을 유도하고 이득이 평탄화된 장파장 EDFA의 요구되는 펌프파워측면에서 수치해석과 실험을 통하여 유도된 모델의 유용성을 증명하였다. 모델을 통한 펌프파워의 예측치는 실험오차 범위내에서 1.9%이내의 정확성을 보였다. 밀도반전이 고정된 상태에서의 black box 모델은 일반적으로 980nm, 1480m, 펌핑의 경우 모두 적용이 가능하며 EDF의 3가지 이상의 길이에 대하여 입력 펌프파워와 입력/출력 신호파워의 관계를 측정하여 밀도반전이 일정한 상태에서 다른 동작점의 성능을 예측할 수 있었다. 또한 단파장 EDFA에서는 손실의 효과가 크게 나타나지 않아 해석적인 해와 일치하는 결과가 알려져 있었으나 이에 비해 장파장 EDFA에서는 여러 가지 손실의 효과가 더욱 크게 작용하게 되며 특히 paired ion의 효과로 인한 손실로써 비선형적인 관계식이 유도됨을 보였다.

• 분석과학
• /
• 제12권3호
• /
• pp.203-208
• /
• 1999

살리실산 및 그 유도체들의 이온쌍 고성능 액체크로마토그래피 용리거동을 이동상 중 이온쌍 시약(tetrabutylammonium chloride, TBACl)의 농도를 변화시키면서 용량인자, k'를 측정함으로서 고찰하였다. 이동상의 pH 및 TBACl의 농도가 증가함에 따라 시료들의 k'는 증가하였다. 살리실산 정량의 최적 이동상 조건은 pH 7.2에서 20 mM TBACl을 함유한 메탄올 용액($MeOH:H_2O$ 30:70), p-아미노살리실산(PAS)은 40 mM TBACl을 함유한 메탄올 용액($MeOH:H_2O$ 20:80) 이었다. 머무름 거동의 관찰로부터 발견한 최적 조건에서 몇 가지 유도체들을 분리하였으며 아울러 아스피린과 결핵 치료제 중 살리실산 유도체들의 함량을 조사하였다.

• Preventive Nutrition and Food Science
• /
• 제4권3호
• /
• pp.167-170
• /
• 1999

Various concentrations of malonaldehyde (MA) produced upon hydrolysis of 1, 1, 3,3-tetraethoxypropane (TEP) were reacted with 2-thiobarbituric acid (TBA)and th e contents of MA-TBA complex were measured both with spectrophotometer and high performance liquid chromatography (HPLC). As the concentrations of MA-TBA increased, their absorbances and the corresponding HPLC peak areas increased. The correlation coefficient between absorbances and HPLC peak areas of MA-TBA peaks from the other compounds and butanol extraction of the complex increased its recovery its recovery by 29.4% . Measurement of the content of MA-TBA complex for monitoring the development of lipid oxidation was proven to be successful with the use of high performance liquid chromatography.

• Bulletin of the Korean Chemical Society
• /
• 제13권3호
• /
• pp.240-245
• /
• 1992

The effect of the addition of sodium dodecyl sulfate (SDS) to a buffered mobile phase (pH 3.4) on the retention of nucleotides, nucleosides and bases was investigated with a polyvinyl alcohol (PVA) column. Depending on the concentration of SDS, two different trends in the retention of nucleosides and bases containing an $NH_2$ group were observed. If the concentration of SDS was less than 5.5 mM, the retention of compounds containing an $NH_2$ group increased as the concentration of SDS in the mobile phase increased. In contrast, if the concentration was greater than 5.5 mM, the retention of compounds containing an $NH_2$ group decreased. Thus, the SDS acted as an ion-pairing reagent at lower concentration but formed micelles at higher concentrations. The retention behavior of the nucleosides and bases in the presence of a micellar concentration of SDS in the mobile phase on the PVA column was compared to the retention behavior on other types of columns.