• Journal of Biomedical and Translational Research
• /
• 제19권4호
• /
• pp.130-139
• /
• 2018

This study aimed to analyze a high-performance liquid chromatography (HPLC) separation using a pentafluorophenyl column of parent drug hydroxychloroquine (HCQ) and its active metabolite, desethylhydroxchloroquine (DHCQ) applying to determine bioequivalence of two different formulations administered to patients. A rapid, simple, sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for bioanalysis of HCQ and its metabolite DHCQ in human whole blood using deuterium derivative $hydroxychloroquine-D_4$ as an internal standard (IS). A triple-quadrupole mass spectrometer was operated using electrospray ionization in multiple reaction monitoring (MRM) mode. Sample preparation involves a two-step precipitation of protein techniques. The removed protein blood samples were chromatographed on a pentafluorophenyl (PFP) column ($50mm{\times}4.6mm$, $2.6{\mu}m$) with a mobile phase (ammonium formate solution containing dilute formic acid) in an isocratic mode at a flow rate of 0.45 mL/min. The standard curves were found to be linear in the range of 2 - 500 ng/mL for HCQ; 2 - 2,000 ng/mL for DHCQ in spite of lacking a highly sensitive MS spectrometry system. Results of intra- and inter-day precision and accuracy were within acceptable limits. A run time of 2.2 min for HCQ and 2.03 min for DHCQ in blood sample facilitated the analysis of more than 300 human whole blood samples per day. Taken together, we concluded that the assay developed herein represents a highly qualified technology for the quantification of HCQ in human whole blood for a parallel design bioequivalence study in a healthy male.

• 분석과학
• /
• 제32권4호
• /
• pp.139-146
• /
• 2019

A simple and reliable analytical method based on high-performance liquid chromatography-ultraviolet detection was established for the analysis of the flowers of Chrysanthemum morifolium (CM). Luteolin-7-O-glucoside (LU7G) was chosen as a target analyte considering its content, availability, and ease of analysis. Chromatographic separation of LU7G was achieved using a Phenomenex Gemini $C_{18}$ column ($250{\times}4.6mm$, $5{\mu}m$) run with a mobile phase consisting of 0.5 % acetic acid in water and 0.5 % acetic acid in acetonitrile at a flow rate of $1.0mL\;min^{-1}$. The detection wavelength and column temperature were set at 350 nm and $40^{\circ}C$, respectively. Method validation was performed according to the AOAC guidelines and the method was specific, linear ($R^2=0.9991$ for $50-300{\mu}g\;mL^{-1}$), precise (${\leq}3.91%$RSD), and accurate (100.1-105.7 %). The limits of detection and quantification were 3.62 and $10.96{\mu}g\;mL^{-1}$, respectively. The established method was successfully applied to determine the contents of LU7G in various batches of bulk CM extracts and labscale CM extract. The developed method is a readily applicable method for the quality assessment of CM and its related products.

• Mass Spectrometry Letters
• /
• 제10권1호
• /
• pp.18-26
• /
• 2019

We developed a bioanalytical method for simultaneous determination of nine NBOMe derivatives (25H-NBOMe, 25B-NBOMe, 25E-NBOMe, 25N-NBOMe, 25C-NBOH, 25I-NBOH, 25B-NBF, 25C-NBF, and 25I-NBF) in human plasma using liquid chromatography tandem mass spectrometry (LC-MS/MS). Human plasma samples were pre-treated using solid-phase extraction. Separation was achieved on a C18 column under gradient elution using a mobile phase containing 0.1% formic acid in acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Mass detection was performed in the positive ion mode using multiple reaction monitoring. The calibration range was 1-100 ng/mL for all quantitative analytes, with a correlation coefficient greater than 0.99. The intra- and inter-day precision and accuracy varied from 0.85 to 6.92% and from 90.19 to 108.69%, respectively. The recovery ranged from 86.36 to 118.52%, and the matrix effects ranged from 27.09 to 99.72%. The stability was acceptable in various conditions. The LC-MS/MS method was validated for linearity, accuracy, precision, matrix effects, recovery and stability in accordance with the FDA guidance. The proposed method is suitable for reliable and robust routine screening and analysis of nine NBOMe derivatives in forensic field.

• 한국동물위생학회지
• /
• 제43권4호
• /
• pp.261-265
• /
• 2020

Each commercial cyromazine insecticide has different HPLC conditions. The aim of this study was to establish a standardized chromatographic method for the determination of cyromazine in commercial insecticides. The separation was achieved on two C18 columns - Waters® Bondapak C (4×300 nm i.d., 10 ㎛) and X bridge (4.6×250 nm i.d., 5 ㎛) using a mobile phase composed of water/methanol/ethanolamine (76:24:0.1, v/v), with UV detection at wavelengths 230 nm and 254 nm. A total of six commercial cyromazine insecticides were analyzed. In this study, the optimal high-performance liquid chromatography conditions for the analysis of cyromazine were as follows: a mobile phase of water/methanol/ethanolamine (76:24:0.1, v/v) at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm using a X bridge C18 column (4.6×250 nm i.d., 5 ㎛) at a column temperature of 25℃. The calibration curve was linear in the concentration range of 5~50 ㎍/mL, with a correlation coefficient of 0.99995. The cyromazine detection limit was 0.2 ㎍/mL, and the limit of quantification was 0.59 ㎍/mL. The percentage recovery ranged from 99.8% to 101.0% for cyromazine, and the relative standard deviation was not over 2.0%. The cyromazine concentration ranged from 92.7% to 109.4% and was within the acceptable range (90~120%) for the percent of the labeled amount. This method was found to be suitable for determining cyromazine in commercial insecticides.

• 한국해안·해양공학회논문집
• /
• 제32권6호
• /
• pp.420-433
• /
• 2020

기존 케이슨방파제의 안정성을 높이기 위해 케이슨 전면 또는 후면에 추가로 신규 케이슨을 설치하여 보강하는 경우 박리에 의한 에너지 손실효과와 케이슨과 케이슨 사이의 공극률 변화에 따른 개별 원형케이슨에 작용하는 파력 및 파처오름 특성 평가는 중요하다. 본 연구에서는 고유함수전개법에 투과성판에서의 속도는 판 전후의 압력차에 선형적으로 비례한다는 Darcy의 법칙을 이용하여 원형케이슨들간의 공극률 계수 변화에 따른 2열 배치된 원형방파제에 작용하는 파랑 특성을 분석하였다. 수치해석의 신뢰성을 확보하기 위해 Sankarbabu et al.(2008)의 수치 해석결과와 비교를 수행하였으며, 다양한 변수에 따른 개별 이중 원형케이슨에 작용하는 파력 및 파처오름 특성을 나타내었다.

• Natural Product Sciences
• /
• 제27권1호
• /
• pp.54-59
• /
• 2021

Bergenia ciliata (Family: Saxifragaceae) is a folklore remedy for the treatment of various ailments in Asian countries. Bergenin (1) has been isolated as an active constituent in many studies, however, the amount of bergenin has not been determined in all parts of the plant. A simple RP-HPLC method was developed to determine the amount of bergenin in methanol extracts of leaves, rhizomes and roots of the plant. Separation was achieved on an Agilent Eclipse XDB-C18 column maintained at 25 ℃ using isocratic solvent system (water: methanol: acetic acid; 62.5:37:0.5 v/v/v) adjusted at pH 2 0 at a flow rate of 1.0 mL/min. and detected at 275 nm. Correlation coefficient (0.9952) showed linearity of concentration (5-200 ㎍/mL) and response. The values of LOD (0.00947 ㎍/mL) and LOQ (0.02869 ㎍/mL) indicated that method was sensitive. The recovery of bergenin was 99.99-100% indicating accuracy of method. The methanol extract of rhizomes contained higher amount of bergenin (19.4%) than roots (9.2%) and leaves (6.9%). It is concluded that methanol extract of rhizomes is a better source of bergenin than other parts of the plant. The findings are useful for standardization of bergenin containing extracts and herbal preparations.

• Tribology and Lubricants
• /
• 제37권3호
• /
• pp.91-98
• /
• 2021

This paper presents a hydrostatic bearing design and rotordynamic analysis of a turbo expander for a hydrogen liquefaction plant. Th~e turbo expander includes the turbine and compressor wheel assembled to a shaft supported by two hydrostatic radial and thrust bearings. The rated speed is 75,000 rpm and the rated power is 6 kW. For the bearing operation, we use pressurized air at 8.5 bar as the lubricant that is supplied to the bearing through the orifice restrictor. We calculate the bearing stiffness and flow rate for various gauge pressure ratios and select the orifice diameter providing the maximum bearing stiffness. Additionally, we conduct a rotordynamic analysis based on the calculated bearing stiffness and damping considering design parameters of the turbo expander. The predicted Cambell diagram indicates that there are two critical speeds under the rated speed and there exists a sufficient separation margin for the rated speed. In addition, the predicted rotor vibration is under 1 ㎛ at the rated speed. We conduct the operating test of the turbo expander in the test rig. For the operation, we supply pressurized air to the turbine and monitor the shaft vibration during the test. The test results show that there are two critical speeds under the rated speed, and the shaft vibration is controlled under 2.5 ㎛.

• 한국동물위생학회지
• /
• 제45권3호
• /
• pp.243-248
• /
• 2022

The HPLC conditions for analysis of ivermectin in solutions dosage forms of commercial anthelmintics are different for each product. The purpose of this study was to establish a standardized chromatographic method for the quantification of ivermectin in solution. The separation was achieved on Waters Xbridge C18 column (4.6×150 nm, 5 ㎛) using different kinds of mobile phase composed of water/methanol/acetonitrile (15/34/51, v/v and 19.5/27.5/53, v/v), with UV detection at wavelengths 245 nm and 254 nm. A total of five commercial ivermectin in solution samples were analyzed. In this study, the optimal chromatographic conditions for analysis of ivermectin in solution were mobile phase of water/methanol/acetonitrile (15/34/51, v/v) at a flow rate of 1.0 mL/min and a detection wavelength of 245 nm using a Waters Xbridge C18 column (4.6×250 nm, 5 ㎛) at a column temperature of 25℃. The linearity was observed in the concentration range of 50~150 ㎍/mL, with a correlation coefficient, r²= 0.99999. The limit of detection and the limit of quantification were 0.88 and 2.68 ㎍/mL, respectively. The accuracy (% recovery) was found to be 98.9 to 100.3%. Intra-day and Intermediate precisions with relative standard deviations were less than 1.0%. The content of ivermectin for five market samples ranged 91.2~102.7%. The proposed method was also found to be robust, therefore, the method can be used for the routine analysis of ivermectin in solutions dosage forms.

• 한국해안·해양공학회논문집
• /
• 제34권1호
• /
• pp.11-18
• /
• 2022

본 연구는 대한해협 인근 입자추적 예측 기법의 정확도 개선을 위해서 해수유동 수치모델 결과를 이용하여 만든 입자추적 모델과 현장 관측 자료를 이용한 기계학습 기반 입자 추적 모델을 비교 및 분석하였다. 세부 연구 방법으로는 대한해협에서 관측된 표층 뜰개 이동 궤적 자료, 3개 관측소(가거도, 거제도, 교본초 관측소)의 조위 및 바람자료를 학습시켜 만든 기계 학습(선형 회귀, 의사결정나무) 기반 예측자료, 수치모델 예측자료(ROMS, MOHID)를 3가지 오차평가방법(CC, RMSE, NCLS)을 통해 비교하였다. 최종 결과로서 CC와 RMSE에서는 의사결정나무 모델의 예측 정확도가 가장 우수하였고 NCLS에서는 MOHID 모델의 예측 결과가 가장 우수하였다.

• 청정기술
• /
• 제15권4호
• /
• pp.287-294
• /
• 2009

DME (dimethyl ether, $CH_3OCH_3$) 직접합성 반응기로부터 생산되는 DME 혼합물(DME: 19~20 mol%)을 DME 흡수탑과 DME 정제탑 장치 2기를 사용하여 대체연료로 사용할 수 있는 순도로 분리하였다. DME 흡수탑에서는 메탄올을 세정용매로 사용하였고 운전압력 50 bar내에서 원료 중 DME를 탑 하부로 99% 이상 회수하는 것을 목적으로 하였으며, 이를 위해 실험실 규모의 실험장치를 통해 얻은 실험식을 사용하여 운전압력 50 bar내에서 DME를 99% 회수하기 위해 필요한 메탄올의 유량을 산출하였다. 그리고 95 wt% 이상의 DME 순도를 얻기 위해 DME 정제탑을 사용하였으며, 경질 생성물(이산화탄소, 질소 등)이 소량(5~10 mol%)이고, 중간생성물(DME)의 양(20~30 mol%)이 적지 않은 것을 감안하여 측면흐름(4단)의 액상 생성물로서 최대 98.2 wt% 순도의 DME를 얻었다.