• 분석과학
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• 제33권6호
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• pp.274-284
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• 2020

액체시료 중 89Sr와 90Sr을 자동핵종분리장치를 이용하여 Sr-resin으로 분리-정제하고, 액체섬광계수기(LSC)로 동시 분석하는 방법을 연구하였다. 액체시료 0.5 kg 중 방사성스트론튬을 탄산염 형태로 농축하고, Sr-resin 2 mL (Bed volume)으로 분리하였다. 유량이 최대 1 mL min-1까지 가능한 중력법과, 유량 2 mL min-1, 4 mL min-1 조건에서, Sr과 방해이온들의 거동을 평가하였다. LSC를 이용해 섬광용액을 혼합하지 않은 Cerenkov mode와, 섬광용액을 혼합한 Scintillation mode에서 측정한 결과를 이용해 정제된 89Sr와 90Sr의 방사능을 동시에 분석하였다. 표준선원을 이용해 90Sr/89Sr의 방사능 비가 1:1, 1:2, 1:5 되도록 탈염수를 이용해 모의시료를 준비하였고, 89Sr 방사능은 0.5~10 Bq kg-1, 90Sr 방사능은 0.5~50 Bq kg-1의 범위이다. Sr의 회수율은 68~94 %이고, 89Sr의 상대편의는 -5~20 %, 90Sr 방사능의 상대편의는 -10~10 %로 나타났다.

• 분석과학
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• 제23권5호
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• pp.457-464
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• 2010

먹는물(정수) 중에 잔류하는 버지니아마이신을 비롯한 macrolide 계열 의약물질 3종과 시메티딘을 동시에 정량 및 정성 분석하는 방법을 확립하였다. HLB 카트리지를 사용하여 분석물질을 추출/정제 및 농축한 후, HPLC/ESI-MS/MS를 이용하여 4종의 물질들을 효과적으로 분리하고 감도 좋게 검출할 수 있었다. 정량분석을 위해서 0.01~2.0 ng/mL 범위에서 $r^2$=0.995이상의 높은 직선성을 나타내는 검량선을 얻었으며, 시메티딘(37.7~48.1%)을 제외한 macrolide 계열 3종 의약물질은 64.7~118.1% 범위의 양호한 회수율을 나타내었다. 바탕 정수에 소량 첨가하여 얻은 분석방법의 검출한계와 정량한계는 각각 1.6~74.8 pg/mL 와 5.5~249.7 pg/mL 범위의 높은 감도를 나타내었다.

• 분석과학
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• 제12권4호
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• pp.265-272
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• 1999

에스트로겐처럼 행동하여 호르몬 수용체와 결합하거나 세포의 신호전달 과정에 영향을 미침으로서 내분비계를 교란시킬 수 있는 환경 에스트로겐 19종 (phytoestrogen: 12종, mycoestrogen: 5종, synthetic estrogen: 2종)의 동시 프로필 분석을 시도하였다. Gas Chromatography/Mass Spectrometry (GC/MS)의 selected ion monitoring (SIM) 방법을 기본으로 하였으며, 액체-고체 추출, 효소 기수분해, 액체-액체 추출 그리고 trimethylsilyl (TMS)-ether 형태의 유도체화를 거치는 비교적 간편한 전처리 방법으로 47.6~99.5%의 회수율과 0.66~9.33%, 1.66~16.14%의 within-a-day 및 day-to-day 분석의 RSD 값을 얻었다. 이 방법을 적용하여 정상 성인 여성과 남성의 뇨 시료에 존재하는 대상 물질들의 농도범위를 결정함으로서 환경 에스트로겐의 영향을 평가하는데 기준이 될 수 있는 한국인 정상인 참고치를 설정하였다.

• 생약학회지
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• 제45권4호
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• pp.338-345
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• 2014

HPL-4 is a new herbal formulation developed for the treatment of osteoarthritis. In this study, we took HPL-4 to develop a method for simultaneous determination of nine marker compounds (protocatechuic acid, chlorogenic acid, liriodendrin, nodakenin, ${\beta}$-$\small{D}$-(3-O-sinapoyl)frucofuranosyl-${\alpha}$-$\small{D}$-(6-O-sinapoyl)glucopyranoside, quercitrin, 6-gingerol, decursin and decursinol angelate) present in the formulation. The analytes were separated by UPLC system consisting of diode array detector at 205 nm and RP-amide column, and solvent system of $ACN/0.1%H_3PO_4$. Analytical method was validated to evaluate its linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy. All standards showed good linearity ($R^2$ >0.99) in the rage of $0.25-400.0{\mu}g/mL$. The LOD and LOQ were within the range of 0.021-0.148 and $0.070-0.448{\mu}g/mL$, respectively. Intra- and inter-day precision was less than RSD 4.0% and the accuracy was range from 92.00-104.81% with RSD<4.2%. The results suggest that the developed UPLC method is precise, accurate and effective, and could be applied for quality control of HPL-4 formulation.

• 분석과학
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• 제21권3호
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• pp.167-173
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• 2008

PCB (poly chlorinated biphenyl)의 재생성문제를 해결하기 위해 PCB가 재생성되지 않는 $220^{\circ}C$ 이내의 온도에서 PCB를 90% 이상 효과적으로 분해할 수 있는 저온활성이 우수한 촉매에 대해 연구 하였다. 기존의 백필터에 저온활성이 우수한 PCB 제거용 촉매를 코팅하여 분진 및 PCB를 동시에 제거 가능한 백필터 여과재를 얻고자 하였다. 촉매 반응 후 벤젠고리가 분해되어 PCB가 재생성될 수 없음을 확인하였다. 그리고 spray법에 의한 촉매코팅이 함침법에 의한 코팅보다 효과적이었으며, Pt-Co 촉매를 사용하였을 때가 PCB 제거율이 가장 높았다. 본 연구를 잘 활용한다면 기존의 소각로에서 사용되던 기존 백필터를 촉매 여과재로 교체만 하여도 분진과 PCB를 동시에 효율적으로 제거할 수 있을 것으로 판단된다.

• Advances in nano research
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• 제16권1호
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• pp.27-40
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• 2024

This work is the first of its kind to integrate Mindlin's theory with analytical methods in order to produce an exact solution to a specific vibration issue as well as a bending problem involving a nanoplate that is supported by a viscoelastic foundation. The plate is exposed to the simultaneous effects of a compressive load in the plate plane and a force operating perpendicular to the plane of the nanoplate. In addition, the flexoelecity effect is included into the plate. The strain gradient component is taken into consideration while calculating the plate equilibrium equation using the nonlocal theory and Hamilton's principle. The free vibration and static responses of the nanoplate seem to be both real and imaginary components because of the appearance of the viscoelastic drag coefficient of the viscoelastic foundation. This study also shows that when analyzing the mechanical response for nanostructure, taking into account the flexoelectricity effect and the influence of the nonlocal parameter, the results will be completely different from the case in which this parameter is ignored. This indicates that it is vital to take into consideration the effects of nonlocal parameters on the nanosheet structure while also taking into consideration the effect of flexoelectricity.

• 한국환경보건학회지
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• 제36권6호
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• pp.510-517
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• 2010

Phthalates, such as di (2-ethylhexyl) phthalate (DEHP), dibutyl phthalate (DBP) have been proved to be teratogenics and endocrine disruptors, metabolized rapidly and excreted in the urine. In this study, a simultaneous analytical method for 10 phthalate metabolites, MnBP, MiBP, MBzP, MCHP, MEHP, MEHHP, MEOHP, MnOP, MiNP and MiDP, in human urines, based on switching system with on-line pretreatment column using HPLC-MS/MS has been developed. This method was validated according to the guideline of bioanalytical method validation of National Institute of Toxicological Research. Limits of detection range between 0.2 and 0.9 ng/ml for 10 phthalate metabolites. The calibration curves showed linearity in the range 0.997~0.999, and the results of the intra- and inter-day validations were in the range from 0.4 to 14.7% RSD and from 0.3 to 9.4% RSD, respectively. Recoveries of phthalate metabolites varied from 87.0 to 116.1%. This analytical method showed high accuracy and stable precision for all metabolites, and seems to be suitable for biomonitoring of phthalates in human urine.

• Asian Journal of Atmospheric Environment
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• 제11권4호
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• pp.283-299
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• 2017

An analytical method using high-performance liquid chromatography (HPLC) with fluorescence (FL) detection was developed for simultaneously analyzing 10 polycyclic aromatic hydrocarbons (PAHs) and 18 nitro-derivatives of PAHs (NPAHs). The two-dimensional HPLC system consists of an on-line clean-up and reduction for NPAHs in the 1st dimension, and separation of the PAHs and the reduced NPAHs and their FL detection in the 2nd dimension after column-switching. To identify an ideal clean-up column for removing sample matrix that may interfere with detection of the analytes, the characteristics of 8 reversed-phase columns were evaluated. The nitrophenylethyl (NPE)-bonded silica column was selected because of its shorter elution band and larger retention factors of the analytes due to strong dipole-dipole interactions. The amino-substituted PAHs (reduced NPAHs), PAHs and deuterated internal standards were separated on polymeric octadecyl-bonded silica (ODS) columns and by dual-channel detection within 120 min including clean-up and reduction steps. The limits of detection were 0.1-9.2 pg per injection for PAHs and 0.1-140 pg per injection for NPAHs. For validation, the method was applied to analyze crude extracts of fine particulate matter ($PM_{2.5}$) samples and achieved good analytical precision and accuracy. Moreover, the standard reference material (SRM1649b, urban dust) was analyzed by this method and the observed concentrations of PAHs and NPAHs were similar to those in previous reports. Thus, the method developed here-in has the potential to become a standard HPLC-based method, especially for NPAHs.

• 분석과학
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• 제35권2호
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• pp.69-81
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• 2022

The method of measuring and classifying the energy category of neutrons directly using raw data acquired through a CZT detector is not satisfactory, in terms of accuracy and efficiency, because of its poor energy resolution and low measurement efficiency. Moreover, this method of measuring and analyzing the characteristics of low-energy or low-activity gamma-ray sources might be not accurate and efficient in the case of neutrons because of various factors, such as the noise of the CZT detector itself and the influence of environmental radiation. We have therefore developed an efficient method of analyzing radiation characteristics using a neutron and gamma-ray analysis algorithm for the rapid and clear identification of the type, energy, and radioactivity of gamma-ray sources as well as the detection and classification of the energy category (fast or thermal neutrons) of neutron sources, employing raw data acquired through a CZT detector. The neutron analysis algorithm is based on the fact that in the energy-spectrum channel of 558.6 keV emitted in the nuclear reaction ¹¹³Cd + ¹n → ¹¹⁴Cd + in the CZT detector, there is a notable difference in detection information between a CZT detector without a PE modulator and a CZT detector with a PE modulator, but there is no significant difference between the two detectors in other energy-spectrum channels. In addition, the gamma-ray analysis algorithm uses the difference in the detection information of the CZT detector between the unique characteristic energy-spectrum channel of a gamma-ray source and other channels. This efficient method of analyzing radiation characteristics is expected to be useful for the rapid radiation detection and accurate information collection on radiation sources, which are required to minimize radiation damage and manage accidents in national disaster situations, such as large-scale radioactivity leak accidents at nuclear power plants or nuclear material handling facilities.

• Journal of Pharmaceutical Investigation
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• 제37권3호
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• pp.179-186
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• 2007

A simple, sensitive and selective liquid chromatographic/tandem mass spectrometric method (LC-MS/MS) was developed and validated for doxifluridine and 5-fluorouracil (5-FU) quantification in dog heparinized plasma. Sample preparation was based on liquid-liquid extraction using a mixture of isopropanol/ethyl acetate (1/9 v/v) to extract doxifluridine, 5-FU and 5-chlorouracil (5-CU, an internal standard) from plasma. Chromatography was performed on a C-18 analytical column and the retention times were 2.7, 1.5 and 1.7 min for doxifluridine, 5-FU and 5-CU, respectively with shorter analysis time within 5 min than previously reported methods. The ionization was optimized using ESI negative mode and selectivity was achieved by tandem mass spectrometric analysis by multiple reaction monitoring (MRM) using the transformations of m/z 244.8>107.6, 129.0>42.0 and 144.9>42.1 for doxifluridine, 5-FU and 5-CU, respectively. The achieved low limit of quantification was 20.0 ng/mL and the assay exhibited linear range of 20-2000 ng/mL ($R^2>0.99957$ for doxifluridine and $R^2>0.99857$ for 5-FU), using $100{\mu}L$ of plasma. Accuracy and precision of quality control samples for both doxifluridine and 5-FU met KFDA and FDA Guidance criteria of 15% for accuracy with coefficients of variation less than 15%. This method demonstrated adequate sensitivity, specificity, accuracy, precision and stability to support the simultaneous analysis of doxifluridine and 5-FU in dog plasma samples in pharmacokinetic and bioequivalence studies.