• Mass Spectrometry Letters
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• 제13권4호
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• pp.158-165
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• 2022

Many therapeutic class drugs such as beta-blocker, corticosteroids, NSAIDs, etc are prohibited substances in the horse racing industry. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology makes it possible to isolate drugs from interference, enables various drug analyses in complex biological samples due to its sensitive sensitivity, and has been successfully applied to doping control. In this paper, we describe a rapid and sensitive method based on solid-phase extraction (SPE) using solid phase cartridge and LC-MS/MS to screen for different class's 35 drug targets in equine plasma. Plasma samples were pretreated by SPE with the NEXUS cartridge consisted non-polar carbon resin and minimum buffer solvent. Chromatographic separation of the analytes was performed on ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 ㎛). The elution gradient was conducted with 5 mM ammonium formate (pH 3.0) in distilled water and 0.1% formic acid in acetonitrile at a flow rate of 0.25 mL/min. The selected reaction monitoring (SRM) mode was used for drug screening with multiple transitions in the positive ionization mode. The specificity, limit of detection, recovery, and stability was evaluated for validation. The method was found to be sensitive and reproducible for drug screening. The method was applied to plasma sample analysis for the proficiency test from the Association of Racing Chemist.

• Journal of Microbiology and Biotechnology
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• 제21권12호
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• pp.1306-1311
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• 2011

Recombinant Rhodopseudomonas palustris, harboring the carotenoid-metabolizing gene crtI (CrtIBS), and whose color changes from greenish yellow to red in response to inorganic As(III), was cultured in transparent microplate wells illuminated with a light emitting diode (LED) array. The cells were seen to grow better under near-infrared light, when compared with cells illuminated with blue or green LEDs. The absorbance ratio of 525 to 425 nm after cultivation for 24 h, which reflects red carotenoid accumulation, increased with an increase in As(III) concentrations. The detection limit of cultures illuminated with near-infrared LED was 5 ${\mu}g$/l, which was equivalent to that of cultures in test tubes illuminated with an incandescent lamp. A near-infrared LED array, in combination with a microplate, enabled the simultaneous handling of multiple cultures, including CrtIBS and a control strain, for normalization by the illumination of those with equal photon flux densities. Thus, the introduction of a near-infrared LED array to the assay is advantageous for the monitoring of arsenic in natural water samples that may contain a number of unknown factors and, therefore, need normalization of the reporter event.

• 대한방사선기술학회지:방사선기술과학
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• 제46권5호
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• pp.417-425
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• 2023

The glomerular filtration rate (GFR) has been the subject of much research as a key indicator for diagnosing, treating, and monitoring kidney function. The gamma camera method (Gates method) is simple and allows simultaneous acquisition of GFR and renal scintigraphy for each kidney, however its accuracy is inferior. This study aimed to investigate changes in GFR depending on how region of interest (ROI) are set up, which is one of many factors influencing accuracy. GFR was calculated by setting the ROI for each phase of the image acquisition time (Gates-1: 0~1 minutes, Gates-2: 1~3 minutes, Gates-3: 3~27 minutes), and statistical significance was verified based on probability value 0.05 through ANOVA analysis. While there was no statistically significant difference among results from Gates-1, 2, 3 (p=0.481>0.05), overall results from the Gates method tended to overestimate compared to those from the multiple blood sampling-dual exponential (MBSDE) method. When comparing averages between phases, results from Gates-2 were most similar to those from the MBSDE method. Moreover, paired t-test p-values between MBSDE method and phases were as follows Gates-1: 0.021 (p<0.05), Gates-2: 0.280 (p>0.05), and Gates-3: 0.164 (p>0.05) indicating that only Gates-1 had statistically significant differences compared with MBSDE method. Thus, setting ROI around 2~3 minutes is calculated can aid in accurately determining GFR when Gates Method.

• Journal of Advanced Marine Engineering and Technology
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• 제39권7호
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• pp.760-764
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• 2015

산업플랜트 현장에서 별도의 배선 없이 쉽고 빠르게 기계상태를 측정하기 위해서는 다중무선센서를 기계에 부착하고 측정과 전송이 동시에 가능한 시분할전송 방식이 필요하다. 그러나 아직까지 연속적인 신호를 동시에 100Hz이상 샘플로 시분할다중전송(TDMA;Time Division Multiple Access)하는 현장적용 연구가 알려지지 않고 있다. 따라서, 본 논문에서는 현장적용을 위해 100Hz이상의 샘플주기로 다수의 센서에서 동시에 취득할 수 있는 시분할다중전송 네트워크프로토콜을 구현하고 그 결과를 나타내고자 한다. 단일 클러스터 스타토폴로지를 대상으로 노드 개수와 거리에 따른 네트워크 가용성 확인을 위해 ns-2 시뮬레이터로 유사한 환경 조건으로 구동하여 결과를 분석하였다. 그 결과 4개의 센서노드로 동시에 연속적인 센서신호를 전송하는 비-시분할다중전송과 시분할다중전송프로토콜을 비교 분석하였다. 전송시간이 20초와 40초 일 경우는 수신율 차이가 작았지만 60초일 경우는 많은 차이를 나타냄을 관찰하였다.

• 분석과학
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• 제21권5호
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• pp.412-423
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• 2008

액체크로마토그래피/텐덤질량분석법을 이용하여 말 소변에서 55 가지 염기성 약물을 동시 분석하는 고체상 추출법을 개발하였다. 본 연구에서는 다양한 종류의 약물인 베타-차단제, 베타-길항제, 항저혈압제, 중추신경흥분제, 진정제, 정신 안정제, 항우울제, 항고혈압제 등을 분석하였다. 각 성분의 분리와 정량은 LC-MS/MS의 positive ion electrospray ionization (+ESI)과 multiple reaction monitoring (MRM)으로 수행하였다. 시판되고 있는 4 가지 SPE 상품(UCT XTRACT$^{(R)}$ XRDAH, Supelco DSC-MCAX$^{(R)}$, Varian Bond Elut Certify$^{(R)}$, Waters Oasis$^{(R)}$ MCX)의 혼합형 양이온 교환 흡착제를 비교하였고 최적의 추출 조건을 확립하였다. 그 결과, UCT XTRACT$^{(R)}$ XRDAH의 흡착제에서 분석 대상약물의 상대 회수율이 terbutaline (41.3%), salbutamol (71.5%), heptaminol (70.7%), phenylpropanolamine (66.3%)을 제외하고 80% 이상의 좋은 결과를 나타내었고, 직선성은 0.9804~0.9999를 갖는 55 개의 검정곡선을 얻을 수 있었으며, 검출한계는 0.2~8.3 ng/mL임을 확인하였다.

• Bulletin of the Korean Chemical Society
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• 제28권7호
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• pp.1187-1194
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• 2007

The three major active isoflavonoids (calycosin-7-O-β -glucoside, isomucronulatol 7-O-β-glucoside, formononetin) and two main saponins (astragaloside I, astragaloside IV) in an extract of Radix Astragali were determined using rapid, sensitive, reliable HPLC/UV and LC-ESI-MS/MS methods. The separation conditions employed for HPLC/UV were optimized using a phenyl-hexyl column (4.6 × 150 mm, 5 μm) with the gradient elution of acetonitrile and water as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm. The specificity of the peaks was determined using a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization (ESI) source that was operated in multiple reaction monitoring (MRM) in the positive mode. These methods were fully validated with respect to the linearity, accuracy, precision, recovery and robustness. The HPLC/UV method was applied successfully to the quantification of three major isoflavonoids in the extract of Radix Astragali. The results indicate that the established HPLC/UV and LC-ESI-MS/MS methods are suitable for the quantitative analysis and quality control of multi-components in Radix Astragali.

• 한국동물위생학회지
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• 제30권1호
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• pp.13-21
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• 2007

An atmospheric pressure chemical ionization (APcI) LC/MS/MS method was developed for the simultaneous analysis of fluoroquinolones (norfloxacin, ciprofloxacin, enrofloxacin, danofloxacin) residues in eggs. The spiked and blank samples were extracted from whole eggs using 50mM phosphate buffer (pH 7.4). The extract was cleaned up by passage though $Oasis^{(R)}$ MAX extraction cartridge for solid-phase extraction followed by elution with 4% formic acid in methanol. The extract of sample was separated on a Waters $Atlantis^{TM}$ $dC_{18}$ reversed-phase column ($4.6{\times}150mm,\;5{\mu}m$) and analyzed by APcI positive mode mass spectrometry. The mobile phase consists of aqueous 0.2% nonafluoropentanoic acid (NFPA) and methanol. Multiple reaction monitoring (MRM) using the precursor to product ion combinations of m/z $320\;{\dashrightarrow}\;302,\;332\;{\dashrightarrow}\;314,\;360\;{\dashrightarrow}\;342$ and m/z $358\;{\dashrightarrow}\;340$ were used to quantify norfloxacin (NOR), ciprofloxacin (CIP), enrofloxacin (ENR) and danofloxacin (DAN), respectively. The limits of quantification (LOQ) were 7.8ppb for NOR, 8.5ppb for CIP, 8.9ppb for ENR, and 4.8ppb for DAN. Average recoveries of fortified sample at levels of 0.025 to 0.1 ppm were estimated 71.29% for NOR, 75.27% for CIP, 85.51% for ENR and 81.22% for DAN. These results could be applied for the confirmation and quantification in eggs.

• 생약학회지
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• 제49권1호
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• pp.76-83
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• 2018

A traditional herbal formula, Gyeji-tang has been used to treat the early colds, headache, chills, and fever in Asian countries. In this study, we were performed simultaneous determination of the 14 bioactive marker compounds, gallic acid, spinosin, paeoniflorin, albiflorin, liquiritin apioside, liquiritin, 6'''-feruloylspinosin, liquilitigenin, coumarin, cinnmamic acid, benzoylpaeoniflorin, cinnamaldehyde, glycyrrhizin, and 6-gingerol in Gyeji-tang using an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS). Analytical column was used a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) and maintained at $45^{\circ}C$ with a flow rate of 0.3 mL/min. The mobile phase consists of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was conducted using multiple reaction monitoring in the positive and negative modes by a Waters ACQUITY TQD LC-MS/MS system. The calibration curves of 14 bioactive marker compounds showed linearity with correlation coefficients ${\geq}0.9798$. The limits of detection and quantification values were in the range of 0.11-6.66 ng/mL and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the established LC-MS/MS method, the amounts of tested 14 compounds in the lyophilized Gyeji-tang sample were detected up to $85.7{\mu}g/g$. These results may be useful for quality assessment of a traditional herbal formulas.

• 한국식품과학회지
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• 제36권6호
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• pp.863-871
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• 2004

본 연구는 건강식품섭취 후 부작용 발생 현황과 건강기능식품 주원료 및 생산 및 출하액, 국내 생산 및 수입을 바탕으로 원료를 선정하고 공전시험법(2002)에 의하여 GC-ECD와 GC-NPD로 분석 가능한 농약(36종)에 대하여 분석한 후 GC-MS로 확인하여 분석하였다. 16종 139품목에 대하여 분석한 결과 19품목에서 농약이 검출되었으며, 국내산 원료와 수입 원료의 검출 현황은, 국내산 원료의 경우 61품목 중 12품목이 검출되었고, 수입 원료의 경우 78품목 중 7품목이 검출되었다. 국내산 원료인 인삼의 경우 13품목 중 3품목이 검출되었고, 운지버섯은 4품목 중 2품목, 구기자는 4품목 중 3품목, 오미자는 5품목 중 2품목, 천궁 4품목 중 2품목이 검출되었다. 수입 원료의 경우 인삼은 8품목 중 3품목이 검출되었으며, 홍삼은 4품목 중 1품목, 운지버섯 6품목 중 1품목, 쑥은 5품목 중 1품목, 천궁 5품목 중 1품목이 검출 되었다. 농약별 분포현황을 보면 총 16종 139품목에 대하여 불검출은 120건이었으며, chlorpyrifos는 13건으로 가장 높게 나타났다. 본 연구는 한정된 시료를 분석한 것이나, 건강기능식품에 사용되는 원료의 잔류농약 존재확인은 지속적인 모니터링의 필요성을 보여주고 있다. 또한 건강기능식품시장이 성장세를 이루고 있는 추세에 건강기능식품 섭취 후 부작용이 발생하였다는 원료에 대한 위해분석을 하는데 있어서의 기초 자료와 국내에서 기준 규격이 설정되어 있지 않은 식품 원료에 대한 기준 규격의 검토 자료로 활용 가능성이 기대된다.

• Wind and Structures
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• 제11권1호
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• pp.35-50
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• 2008

Wind and temperature have been shown to be the critical sources causing changes in the modal properties of large-scale bridges. While the individual effects of wind and temperature on modal variability have been widely studied, the investigation about the effects of multiple environmental factors on structural modal properties was scarcely reported. This paper addresses the modeling of the simultaneous effects of wind and temperature on the modal frequencies of an instrumented cable-stayed bridge. Making use of the long-term monitoring data from anemometers, temperature sensors and accelerometers, a neural network model is formulated to correlate the modal frequency of each vibration mode with wind speed and temperature simultaneously. Research efforts have been made on enhancing the prediction capability of the neural network model through optimal selection of the number of hidden nodes and an analysis of relative strength of effect (RSE) for input reconstruction. The generalization performance of the formulated model is verified with a set of new testing data that have not been used in formulating the model. It is shown that using the significant components of wind speeds and temperatures rather than the whole measurement components as input to neural network can enhance the prediction capability. For the fundamental mode of the bridge investigated, wind and temperature together apply an overall negative action on the modal frequency, and the change in wind condition contributes less to the modal variability than the change in temperature.