• Bulletin of the Korean Chemical Society
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• 제28권1호
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• pp.59-62
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• 2007

A quantitative analysis method of halogen elements in volatile organohalogen compounds was established by the Wickbold combustion pretreatment in an enclosed system and ion chromatography. The sample pretreatment parameters of Wickbold combustion were experimentally optimized, and using the determined optimal pretreatment parameters, the reproducibility was estimated by ion chromatography. As a comparison for real samples, NIST certified reference materials (CRMs) were analyzed for the recovery efficiency and reproducibility.

• Mass Spectrometry Letters
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• 제5권1호
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• pp.24-29
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• 2014

An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.

• 대한화학회지
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• 제30권3호
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• pp.312-319
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• 1986

알킬 처리된 실리카(ODS)칼럼을 정지상으로하여 역상에서의 이온-쌍 크로마토그래피 법으로 방향족 카르복시산들의 크기 인자를 조사하고 분리하는데 반대 이온으로 브롬화 도데실트리메틸암모늄(DTAB)을 사용하였다. 시료의 크기 인자는 반대 이온의 농도, 메탄올의 농도, 전해질의 종류 및 농도, 시료 분자에 붙어 있는 다른 작용기의 종류 및 위치등에 따라 영향을 받았다. 최적 조건하에서 몇 가지 혼합 시료를 분리할 수 있었다.

• Bulletin of the Korean Chemical Society
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• 제24권12호
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• pp.1805-1808
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• 2003

The simultaneous determination of As(III), As(V), and DMA has been performed by ion chromatography (IC) coupled with inductively coupled plasma-mass spectrometry (ICP-MS). The separation of the three arsenic species was achieved by an anionic separator column (AS 7) with an isocratic elution system. The separated species were directly detected by ICP-MS as an element-selective detection method. The IC-ICP-MS technique was applied for the determination of arsenic species in a NIST SRM 1643d water sample. An As(III) only was detected in the sample. The detection limits of As(III), As(V) and DMA were 0.31, 0.45, and 2.09 ng/mL, respectively. It was also applied for the determination of arsenic species in a human urine obtained by a volunteer, and three arsenic species were identified. The determination of total As in human urines that were obtained from 25 volunteers at the different age was also carried out by ICP-MS.

• Bulletin of the Korean Chemical Society
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• 제24권9호
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• pp.1324-1328
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• 2003

The simultaneous determination of anions ($SO_4 ^{2-},\;Cl^-,\;and\;NO_3^-$) and cations ($Na^+,\;NH^{4+},\;K^+,\;Mg^{2+},\;and\;Ca^{2+}$) in natural water obtained by Nakdong River waters system in Korea were performed by ion-exclusion/cationexchange chromatography with conductimetric detection. The stationary phase was a polymethacrylate-based weakly acidic cation-exchange resin column in the $H^+$-form and a weak-acid eluent. When using only a 1.4 mM sulfosalicylic acid/6 mM 18-crown-6 ether as an eluent, good resolution of both anions and cations, minimum time required for the separation, and satisfactory detection sensitivity were obtained in a reasonable time. The method was successfully applied to the simultaneous determination of anions and cations in natural waters.

• 분석과학
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• 제25권6호
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• pp.350-363
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• 2012

이온크로마토그래피(IC) 시스템을 이용하여 눈 시료의 이온성분을 측정하기 위해 IC 시스템의 성능평가, 시료 병의 세척법, 필터 적용에 따른 문제점을 조사하였다. 이를 바탕으로 이온성분 측정자료의 불확도 산출법을 연구하였다. 본 연구의 IC 시스템 검출한계는 양이온의 경우 0.01~0.26 ${\mu}g/L$, 음이온 성분들은 0.02~0.26 ${\mu}g/L$로 나타났다. 그리고 양이온과 음이온의 재현성을 나타내는 변동계수는 각각 0.4-17.4%, 0.1-27.6%로 조사되었다. BCR$^{(R)}$-408을 이용한 측정자료의 정확도 조사 결과 양이온과 음이온의 상대오차는 각각 4.5-12.0%, 1.3-5.6%로 나타났다. 시료 병에 대한 실험실 바탕시험 결과 유기음이온을 포함한 일부 성분들($CH_3CO_2{^-}$, $HCO_2{^-}$, $NH_4{^+}$)의 경우 다른 성분들에 비해 오염 가능성이 높은 것으로 조사되었다. $NO_3{^-}$ 성분의 바탕시험 결과는 시료 병 세척과정에 사용된 $HNO_3$의 잔류에 따른 오염영향으로 나타났다. 그리고 눈 시료 용융액의 불용성 입자를 제거하기 위해 필터를 사용할 경우 일부 이온 성분들은 필터로부터 직접 용출되는 것으로 조사되었다. 따라서 사용 전에 증류수(~ 6 mL)로 세척하는 것이 필요하고 지역별로 눈 시료의 농도 특성을 고려하여 선별적으로 필터를 적용해야 한다. 마지막으로 그린란드 북서부 내륙의 NEEM 캠프의 풍상 지역에서 채취한 눈 시료의 이온성분 측정 자료의 불확도를 산출하기 위해 이온 성분 가운데 $F^-$ 측정 자료에 대해 불확도를 결정하였다.

• 대한화학회지
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• 제29권4호
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• pp.365-371
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• 1985

이온쌍크로마토그래피에 의한 유기 및 무기음이온을 분리하는데 반대이온으로서 양이온 염료인 메틸렌 부루$(MTB^+)$를 사용하여 흡수가 되지 않는 음이온 시료를 간접적으로 분광광도 검출기로서 가시영역인 665nm에서 검출할 수 있었으며 혼합시료의 분리를 시도한 결과 좋은 분리도와 높은 감도를 보여주었다. 또한 여러 실험조건에서 분리인자를 측정하여 머무름 기구를 조사하였다. 본 연구에서 머무름 기구는 $MTB^+$가 고정상에 일차층(primary layer)을 형성하고 반면 음이온 시료 또는 이동상에 존재하는 다른 음이온들이 경쟁적으로 이차층(secondary layer)을 형성하는 ion-interaction model임을 확인하였다.

• Bulletin of the Korean Chemical Society
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• 제15권9호
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• pp.786-791
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• 1994

A simple and rapid sample pretreatment process necessary for determination of metal oxides in water was proposed. Samples were injected into the continuous-flow tube installed inside the microwave oven and the treated samples were cooled before entered to the Ion Chromatography (IC) or Inductively Coupled Plasma (ICP). By coupling this microwave digestion system with IC or ICP, a fully automatic analytical procedures may be easily established. In this study, two different types of digestion methods were considered; the open tubing method (OTM) and the restraint tubing method (RTM). The RTM was proved to be 3 times faster in digestion period and 10 times higher in detection range than the OTM. Validation of proposed sample digestion system was carried out by using an ICP. The results showed that both of continuous-flow methods, the OTM and the RTM were comparable in accuracies with the conventional batch-type vessel digestion method.

• Journal of Animal Science and Technology
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• 제47권6호
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• pp.1025-1032
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• 2005

난백 단백질 중 ovotransferrin을 gel chromato- graphy와 heparin affinity chromatography를 통하여 분리 하였다. 1차 gel filtration의 경우에 샘플인젝션 후 65-70min(fraction No. 14) 이후에는 ovalbumin이 ovotransferrin과 혼입되어 분리되고 오히려 ovalbumin의 농도가 더 높은 분포를 보였다. 고순도의 ovotransferrin을 분리하기 위하여 다시 fraction No. 12-14을 농축한 뒤 gel filtration을 실시한 결과 ovotransferrin이 완전히 분리되지 않았는데 이는 gel filtration만의 반복을 통해서 순수한 ovotransferrin을 얻는 것이 비효과적임을 의미하는 것으로 판단된다. Ovotransferrin을 heparin affinity chromatography을 이용하여 분리한 경우 칼럼에 Fe2+를 고정시킨 후 50mM EDTA를 흘려 주었는데 ovalbumin이 5-10분경에 용출이 되었고 10-15분경에 ovalbumin과 ovotransferrin이 같이 용출되었다. 그 후에 50mM Phosphate buffer (pH 7.2, 0.15M salt)를 흘려주었는데 여전히 ovalbumin의 밴드가 보여 순수하지 않음을 확인하였다. Fe3+를 컬럼에 고정시킨 후 50mM EDTA를 흘려주었을 때 ovalbumin이 10-15분경에 용출이 되었고 15-20분경에 ovalbumin과 ovotransferrin이 같이 용출되었지만 50mM Phosphate buffer (pH 7.2, 0.15M salt free)를 흘려주었을 때 156-165분경에 ovalbumin이 혼입되지 않은 매우 순수한 ovotransferrin이 용출되는 것을 확인하였다. 위의 결과를 종합해볼 때 gel chromatography를 반복적으로 실시한 경우 보다는 heparin affinity chromatography를 이용하여 분리하고 컬럼에 Fe2+를 고정시킨 경우보다 Fe3+를 고정시켰을 때 더욱 순수한 ovotransferrin을 분리해낼 수 있었다.

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