• 대한화학회지
• /
• 제31권1호
• /
• pp.45-54
• /
• 1987

Calcon carboxylic acid[2-hydroxy-1-(2-hydroxy-4-sulfo-1-naphthylazo)-3-naphthoic acid;CCA)]를 이온교환시킨 Dowex 1-X8수지(CCA-Dowex 1-X8)와 2-methyl-8-hydroxyquinoline(MHQ)을 침윤시킨 Amberlite XAD-4 수지(MHQ-XAD-4)를 여러가지 매질중에 있는 철(Ⅲ)이온의 분리-농축에 사용하였다. 이들 수지의 안정성을 검토하고 철(Ⅲ)이온에 대한 흡착능을 측정하였다. 매트릭수의 주성분인 Al(Ⅲ), Ca(Ⅱ), 및 Fe(Ⅲ)들의 수지에 대한 흡착성을 pH를 변화시키며 조사하여 최적 pH범위를 결정하였다. 용리법으로 알루미늄호일과 초정약수중 미량의 철분을 매트릭스 이온으로부터 분리-농축하였다. 농축된 Fe(Ⅲ)는 소량의 강산으로 용리시켜 불꽃 원자흡광광도법으로 정량하였다. 초정약수중의 Fe(Ⅱ)와 Fe(Ⅲ) 이온들은 SP-Sephadex C-25컬럼으로 농축하고, ferrozine용액과 1% ascorbic acid-ferrozine용액으로 단계적 용리법에 의해 용리시킴으로써 각각을 분리할 수 있었다. 분리된 각 이온들은 Fe(Ⅲ)-ferrozine착물의 분석 파장인 562nm에서 분광 광도법으로 정량하였다.

• 콘크리트학회지
• /
• 제9권2호
• /
• pp.99-108
• /
• 1997

철근콘크리트 기둥의 2계거동 해석을 위한 기존의 연구는 대부분 대칭단면에 1축 휨과 축력이 동시에 작용하는 경우에 한정되어 왔다. 그러나 일반적으로 기둥은 2축 휨과 축력을 동시에 받으며 이때 기둥의 거동을 보다 정확하게 예측하기 위해서는 휨모멘트간의 상호 연관성을 고려하여야 한다. 본 연구에서는 이와 같은 휨모멘크간의 상호 연관성을 고려한 보다 일반적인 기둥의 강성행렬을 유도하였으며, 이를 이용하여 2축 휨을 받는 철근콘크리트 기둥의 2계거동 해석방법을 제안하였다. 제안된 해석방법을 이용하여 2축 휨과 축력을 동시에 받는 정사각형과 직사각형 기둥에 대하여 2계거동 해석을 수행하였다. 그리고 다양한 하중조건에 대한 기둥의 극한강도를 평가하고, ACI 설계규준의 모멘트 확대계수법에 의해 계산된 기둥의 극한강도와 해석결과를 비교하였다. 이러한 결과에 의하면 직사각형 기두에서 모멘트 확대계수법에 의한 기둥의 극한강도가 해석결과보다 큰 경우도 있었다. 따라서 직사각형 단면 기둥에 2축 휨과 축력이 동시에 작용하는 경우에는 모멘트 확대계수법을 이용하여 기둥의 극한강도를 평가하면 실제 기둥의 극한강도가 크게 평가될 수 있다는 것을 알 수 있다.

• Bulletin of the Korean Chemical Society
• /
• 제32권10호
• /
• pp.3597-3602
• /
• 2011

A simple and rapid analytical method was developed for the determination of eight isoquinoline alkaloids in Corydalis species. Eight isoquinoline alkaloids, including 2 aporphine alkaloids (isocorydine and glaucine) and 6 protoberberine alkaloids (coptisine, palmatine, berberine, canadine, corydaline, and tetrahydrocoptisine) were used as chemical markers which have a various biological activity and determined for quality control of Corydalis (C.) species (C. ternata, C. yanhusuo, and C. decumbens). To evaluate the quality of these herbal medicines, LC chromatographic separation of alkaloids were preferentially investigated on reversed-phase C18 column with pH variation and composition of mobile phase. In addition, the separation of these alkaloids in herbal extracts was found to be significantly affected on mobile phase composition using gradient elution. Especially for C. yanhusuo extract, berberine was seriously interfered with other alkaloid extracted from sample matrix when mobile phase composition was not optimized. As results, these compounds were successfully separated within 28 min using 10 mM ammonium acetate containing 0.2% triethylamine (adjusted at pH 5.0) as a mobile phase with gradient elution. On the basis of optimized HPLC conditions, 23 different Corydalis species samples were analyzed for the determination of alkaloid levels. In addition, principal component analysis (PCA) combined with the chromatographic data could be successfully classified the different geographic origin samples.

• Bulletin of the Korean Chemical Society
• /
• 제28권5호
• /
• pp.737-744
• /
• 2007

An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of acrylamide in potato chips, starch-rich foodstuff cooked at high temperature. Sample was spiked with 13C3-acrylamide and then extracted with water. The extract was further cleaned up with an Oasis HLB solid-phase extraction (SPE) cartridge and an Oasis mixed-phase cation exchange (MCX) SPE cartridge. The extract was analyzed by using LC/ESI/Tandem MS in positive ion mode. LC with a medium reversed-phase (C4) column was optimized to obtain adequate chromatographic retention and separation of acrylamide. MS was operated to selectively monitor [M+H]+ ions of the analyte and its isotope analogue at m/z 72 and m/z 75, respectively. Sample was also analyzed by the LC/MS with selectively monitoring the collisionally induced dissociation channels of m/z 72 → m/z 55 and m/z 75 → 58. Compared to the LC/MS chromatograms, the LC/MS/MS chromatograms showed substantially reduced background chemical noises coming from solvent clusters formed during ESI spray processes and interferences from sample matrix. Repeatability and reproducibility studies showed that the LC/MS/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0% while the LC/MS results are influenced by chemical interferences.

• 한국음향학회지
• /
• 제20권1호
• /
• pp.13-20
• /
• 2001

음향 에코우제거기나 소음제어와 같은 임펄스 응답이 긴 디지털 필터를 이용하여 필터링을 할 경우 수렴속도가 느리고 계산시간이 많이 걸린다. 이러한 기존의 필터링에서 생기는 계산시간이나 수렴속도 문제를 개선하기 위해서 서브밴드 필터링과 멀티레이트 신호처리 기술이 개발되었다. 모든 시스템의 전달함수는 interpolator와 임펄스 응답사이에 임의 수만큼의 0이 들어있는 sparse 임펄스 응답을 갖는 서브필터를 직렬로 연결한 구조로 표현할 수 있다. 이 경우에 interpolator는 Hadamard 행렬로 표현되고 저역통과필터 특성을 갖는 원형필터를 균일하게 이동시킨 것과 같다. 그래서 입력신호를 Hadamard 변환을 이용하여 각 서브대역으로 분할하고 decimation을 하여 샘플링 레이트를 줄이는 멀티레이트기술이 음향 함수 모델링이나 잡음제거에 응용할 수 있다. 본 논문에서는 decimation으로 생기는 에리어싱을 제거하고 수렴속도를 향상시키기 위해서 입력 신호를 트리구조를 갖는 필터뱅크를 이용하여 비균일한 서브대역으로 분할, 그리고 decimation을 하여 샘플링레이트를 변환하고 각 서브대역에서 계수를 갱신한 후 이 계수를 전대역으로 Hadamard 변환을 이용하여 변환하는 비균일한 대역폭을 갖는 delayless 필터 구조를 제안하고 이 구조를 컴퓨터 시뮬레이션을 통하여 성능을 검증한다.

• Bulletin of the Korean Chemical Society
• /
• 제25권1호
• /
• pp.109-114
• /
• 2004

A sensitive method for quantitation of glimepiride in human plasma has been established using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Glipizide was used as an internal standard. Glimepiride and internal standard in plasma sample was extracted using diethyl etherethyl acetate (1 : 1). A centrifuged upper layer was then evaporated and reconstituted with the mobile phase of acetonitrile-5 mM ammonium acetate (60:40, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS in the multiple reaction monitoring (MRM) mode, glimepiride and glipizide were detected without severe interference from human plasma matrix. Glimepiride produced a protonated precursor ion ([M+H]$^+$) at m/z 491 and a corresponding product ion at m/z 352. And the internal standard produced a protonated precursor ion ([M+H]]$^+$) at m/z 446 and a corresponding product ion at m/z 321. Detection of glimepiride in human plasma by the LC-ESI/MS/MS method was accurate and precise with a quantitation limit of 0.1 ng/mL. The validation, reproducibility, stability, and recovery of the method were evaluated. The method has been successfully applied to pharmacokinetic studies of glimepiride in human plasma.

• 한국식품과학회지
• /
• 제11권4호
• /
• pp.249-257
• /
• 1979

전보에서 저자들을 물리적 견고성이 우수한 포도당 이성화 효소를 세포 고정화 시킨 제품을 얻었다.(한국 식품 과학 회지, 11(No. 3), 192(1979). 이 효소 제품을 사용하여 실험실 조건에서 회분식 반응조와 충진식 반응조를 운영하여 효소의 반응 특성과 생산성, 활성 감소 현상을 비교 하였다. 본 고정화 효소의 비활성 역가는 회분식 반응조와 충진식 반응조에서 1 g당 각각 48 및 114 units였으며 연속적인 공정에서 더 높은 생산성과 이성화율을 보였다. 효소의 생산성은 체장 시간, 기질의 농도, 효소 부하율(附荷率) 및 반응조의 외형에 영향을 받았으며 충진 밀도가 450 g/l일 때 실제 공간율은 0.36이었으며 비교적 좋은 충진 현상을 보였다. 연속 공정중 효소의 활성 감퇴 현상을 고찰하기 위하여 2.5 M 포도당 용액을 체장 시간이 5.3시간이 되도록 약 220시간 동안 반응시켜 본 결과, 효소 활성 감퇴 곡선은 일차 반응을 따르며 활성 반감기는 115일로 연속 공정에 이용 가능함을 알았다. 이 고정화 효소 제품은 물리적 안정성이 높은 반면 물질 전달 계수가 반응 속도에 큰 영향을 미치는 것으로 나타났다.

• Journal of Pharmaceutical Investigation
• /
• 제34권6호
• /
• pp.513-519
• /
• 2004

A sensitive method for quantification of pinaverium bromide in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS/MS). Glimepiride was used as internal standard. Pinaverium bromide and internal standard in plasma sample were extracted using tert-butylmethylether(TBME). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of acetonitrile-5 mM ammonium formate (80/20, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS with multiple reaction monitoring (MRM) mode, pinaverium and glimepirde were detected without severe interference from human plasma matrix. Pinaverium produced a protonated precursor ion $([M+H]^+)$ at m/z 510.3 and a corresponding product ion at m/z 228.9. Internal standard produced a protonated precursor ion $([M+H]^+)$ at m/z 491.5 and a corresponding product ion at m/z 352.0. Detection of pinaverium bromide in human plasma was accurate and precise, with limit of quantitation at 0.5 ng/ml. The method has been successfully applied to bioavailability study of pinaverium bromide tablet in Korean healthy male volunteers. Pharmacokinetic parameters such as $AUC_t,\;C_{max},\;T_{max},\;K_{el}\;and\;t_{1/2}$ were calculated.

• 한국환경농학회지
• /
• 제34권3호
• /
• pp.230-237
• /
• 2015

BACKGROUND: To identify the sources of inaccuracy in LC/MS/MS methods used in the routine quantitation of small molecules are described and discussed. METHODS AND RESULTS: Various UPLC coupled to triple quadrupole mass spectrometer and time of flight (TOF) were used to identify the potential sources of inaccuracy and inducing the pitfalls of qualification and quntitation during the veterinary drug residue analysis. Some of stable isotope labelled veterinary drugs, which were used as internal standards, presented "cross-talk", regardless of manufactures of mass spectrometer and types of spectrometer. Group of sulfonamides also presented inaccuracy qualification and quantitation due to the multi-residue analytical method with the same fragment ions at the close retention times. CONCLUSION: The phenomena of "cross-talk" occurring between subsequently monitored transition from stable isotope labelled and isotope non-labelled authentic chemical were identified. To prevent errors and achieve more accurate data during the analysis of small molecules by LC/MS/MS SRM method, Followings should be taken care of and kept checking; purity and concentration of stable isotope as an internal standard, prevention of carry-over during the separation in column, minimizing the ion suppression by matrix effect, identification of retention time, precursor ion and product ion, and full knowledge of data processing including smoothing and peak integration.

• Mass Spectrometry Letters
• /
• 제9권1호
• /
• pp.30-36
• /
• 2018

A quantitation method for free amino acids in human serum was developed using a stepwise-dilution method and a bimodal cation exchange (CEX)/hydrophilic interaction liquid chromatography (HILIC)-tandem mass spectrometry system equipped with an electrospray ionization source (ESI/MS/MS). This method, which was validated using quality control samples, was optimized for enhanced selectivity and sensitivity. Dithiothreitol (DTT) was used as a reducing agent to prevent the oxidation of a serum sample ($50{\mu}L$), which was then subjected to stepwise dilution using 3, 30, and 90 volumes of acetonitrile containing 0.1% formic acid. Chromatographic separation was performed on an Imtakt Intrada Amino Acid column ($50mm{\times}3mm$, $3{\mu}m$) in mixed mode packed with CEX and HILIC ligands embedded in the stationary phase. Underivatized free amino acids were eluted and separated within 10 min. As a result of the validation, the precision and accuracy for the inter- and intraday assays were determined as 2.11-11.51% and 92.82-109.40%, respectively. The lowest limit of quantification (LLOQ) was $0.5-4.0{\mu}g/mL$ and the matrix effect was 80.22-115.93%. The proposed method was successfully applied to the quantitative analysis of free amino acids in human serum.