• Mass Spectrometry Letters
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• 제10권1호
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• pp.38-42
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• 2019

Damaurone D belongs to the genus Rosa and is a traditional medicinal product used for the treatment of depression, inflammation, and infectious diseases. The purpose of this study was to develop a simple liquid chromatography-tandem mass spectrometry method for the detection of damaurone D in rat plasma and to demonstrate its application in pharmacokinetic studies. Damaurone D and berberine (internal standard) were extracted with acetonitrile using a protein precipitation method. Mass transition was monitored in multiple reaction monitoring mode at m/z $323.2{\rightarrow}267.0$ for damaurone D and m/z $336.1{\rightarrow}320.0$ for berberine in positive ion mode. Analytical validation was conducted by evaluating the specificity, linearity, accuracy, precision, matrix effect, extraction recovery, and stability. The calibration curves were linear over 2-1000 ng/mL. The intra- and inter-day precision and accuracy of quality control samples were 4.79-13.33% and 86.23-102.75%, respectively. The matrix effect and extraction recovery were 96.11-98.47% and 96.11-102.25%, respectively. In the pharmacokinetic study after intravenous administration of damaurone D at a dose of 3 mg/kg in rats, the area under the curve and clearance of damaurone D in rat plasma were $16750.26{\pm}2676.10min{\cdot}ng/mL$ and $182.44{\pm}31.36mL/min/kg$, respectively.

• 한국방사선학회논문지
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• 제13권5호
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• pp.819-824
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• 2019

본 연구에서 서로 다른 양성자 에너지를 사용하여 핵반응에 의해 생성된 감마선의 차이를 통해 고에너지 양성자 Pb(p, nx) 핵반응에서 생성된 동위원소를 식별하는 방법을 제안했다. 한국원자력연구원의 100-M eV 양성자 선형 가속기에서 생성된 고 에너지 양성자를 이용하여 실험을 수행 하였다. 양성자 핵반응을 통해 생성된 다양한 핵종에 의해 생성된 감마선은 HPGe 검출기로 구성된 감마선 분광법 시스템을 사용하여 측정되었습니다. 감마선 표준선원은 감마선 검출기의 정확한 에너지교정 및 효율측정을 위해 사용되었습니다. 제안한 방법을 위하여 동일한 천연 납 시료에 서로 다른 100 및 60 MeV 양성자 에너지빔을 사용하였다. 이 방법은 동일한 시료에서 발생되는 감마선들을 서로 비교함으로써 생성된 핵종들을 확인하는데 매우 효과적임을 알 수 있었다. 이 연구의 결과는 향후 다른 양성자 핵반응 결과를 얻는데도 매우 효과적으로 적용될 것이라 생각된다.

• 대한수의학회지
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• 제60권4호
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• pp.209-213
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• 2020

This study examined the residue of dl-methylephedrine hydrochloride (MEP) on the muscle of pigs administered orally with MEP 12 g/ton feed for seven consecutive days. Twenty healthy cross swine were administered MEP. Four treated animals were selected arbitrarily to be sacrificed at 1, 2, 3, 4, and 5 days after treatment. MEP residue concentrations in the muscle were determined by liquid chromatography coupled with tandem mass spectrometry. The drug was extracted from muscle samples using 10 mM ammonium formate in acetonitrile followed by clean-up with n-hexane. The analyte was separated on an XBridgeTM hydrophilic interaction liquid chromatography column using 10 mM ammonium formate in deionized distilled water and acetonitrile. The correlation coefficient (R2) of the calibration curve was 0.9974, and the limits of detection and quantification were 0.05 and 0.15 ㎍/kg, respectively. The recoveries at three spiking levels were 94.5-101.2%, and the relative Standard Deviations was less than 4.06%. In the MEP-treated group, MEP residues on one day post-treatment were below the maximum residue limit in the muscle. The developed method is sensitive and reliable for the detection of MEP in porcine muscle tissues. Furthermore, it exhibits low quantification limits for animal-derived food products destined for human consumption.

• 한국환경농학회지
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• 제39권4호
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• pp.368-374
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• 2020

BACKGROUND: The residual analysis of polar pesticides has remained a challenge. It is even more difficult to simultaneously analyze multiple polar pesticides. Diquat, paraquat, and chlormequat are typical examples of highly polar pesticides. The existing methods for the analysis of diquat, paraquat and chlormequat are complex and time consuming. Therefore, a simple, quick and effective method was developed in the represent study for simultaneous analysis of diquat, paraquat and chlormequat in animal products, meat and fat using UPLC-MS/MS. METHODS AND RESULTS: Sample extraction was carried out using acidified acetonitrile and water and re- extracted with acidified acetonitrile and combine the extracts followed by centrifugation. The extract was then cleaned up with a HLB cartridge after reconstitution with acidic acetonitrile and water. The method was validated in quintuplicate at three different concentrations. The limits of detection (LOD) and quantification (LOQ) were 0.0015 and 0.005 mg/L, respectively. Matrix suppression effect was observed for all of the analytes. A seven point matrix matched calibration curve was constructed for each of the compound resulted excellent linearity with determination coefficients (R2) ≥ 0.991. Accuracy and precision of the method was calculated from the recovery and repeatability and ranged from 62.4 to 119.7% with relative standard deviation less than 18.8%. CONCLUSION: The recovery and repeatability of the developed method were in the acceptable range according to the Codex Alimentarius guideline. The developed method can be applied for the routine monitoring of diquat, paraquat, and chlormequat in animal products, meat and fat.

• 한국동물위생학회지
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• 제43권4호
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• pp.261-265
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• 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.

• 공업화학
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• 제34권1호
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• pp.9-14
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• 2023

본 논문에서는 용액의 이온 농도 측정이 가능한 나피온 폴리머(Nafion polymer) 코팅 기반 2상 금 전극의 임피던스(Impedance) 센서를 개발하였다. 스퍼터링(Sputtering) 공정을 통해서 제작된 금 전극의 표면을 나피온 폴리머를 사용하여 표면 개질 하였다. 상기 제작된 전극은 분극 현상 제어가 가능하여 전기화학적 신호를 안정적으로 측정할 수 있도록 하였다. 분광학과 전자주사현미경 관찰을 통하여 박막의 나피온 폴리머 코팅을 확인하였다. 나피온 코팅이 된 전극은 기존 금 전극에 비해 안정적인 임피던스 신호를 보여 주었으며, 표준 염화나트륨(NaCl) 용액 사용 시 임피던스 센서의 신뢰성 높은 검정 곡선(R² = 0.983)을 나타내었다. 또한, 임피던스 센서는 상용화 전도도 장치와 인공 눈물의 이온 농도 측정 비교 실험을 진행하였으며, 유사한 결과값을 확인하였다.

• Nuclear Engineering and Technology
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• 제54권4호
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• pp.1421-1430
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• 2022

The computation of the solid angle and the detector efficiency is considering to be one of the most important factors during the measuring process for the radioactivity, especially the cylindrical γ-ray NaI(Tl) detectors nowadays have applications in several fields such as industry, hazardous for health, the gamma-ray radiation detectors grow to be the main essential instruments in radiation protection sector. In the present work, a generic numerical simulation method (NSM) for calculating the efficiency of the γ-ray spectrometry setup is established. The formulas are suitable for any type of source-to-detector shape and can be valuable to determine the full-energy peak and the total efficiencies and P/T ratio of cylindrical γ-ray NaI(Tl) detector setup concerning the truncated conical radioactive source. This methodology is based on estimate the path length of γ-ray radiation inside the detector active medium, inside the source itself, and the self-attenuation correction factors, which typically use to correct the sample attenuation of the original geometry source. The calculations can be completed in general by using extra reasonable and complicate analytical and numerical techniques than the standard models; especially the effective solid angle, and the detector efficiency have to be calculated in case of the truncated conical radioactive source studied condition. Moreover, the (NSM) can be used for the straight calculations of the γ-ray detector efficiency after the computation of improvement that need in the case of γ-γ coincidence summing (CS). The (NSM) confirmation of the development created by the efficiency transfer method has been achieved by comparing the results of the measuring truncated conical radioactive source with certified nuclide activities with the γ-ray NaI(Tl) detector, and a good agreement was obtained after corrections of (CS). The methodology can be unlimited to find the theoretical efficiencies and modifications equivalent to any geometry by essential sufficiently the physical selective considered situation.

• 한국전기전자재료학회논문지
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• 제35권6호
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• pp.594-602
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• 2022

Cast-resin transformers are widely installed in various electrical power systems because of their low operating cost and low influence on external environmental factors. However, when they have an internal defect during the manufacturing process or operation, a partial discharge (PD) occurs, and eventually destroys the insulation. In this paper, a Rogowski-type PD sensor was studied to replace commercial PD sensors used for the insulation diagnosis of power apparatus. The proposed PD sensor was manufactured with four different types of PCB-based winding structures, and it was analyzed in terms of the detection characteristics for standard calibration pulses and the changes of the output voltage according to the distance. The output increased linearly in accordance with the applied discharge amount. It was confirmed that the hexagon structure sensor had the highest sensitivity, because the winding cross-sectional area of the sensor was larger than others. In addition, as the distance from the defect increased, the output voltage of the sensors decreased by 7.32% on average. It was also confirmed that the attenuation rate according to the distance decreased as the input discharge amount increased. For the application of this new type sensor, PD electrode system was designed to simulate the void defect. Waveforms and PRPD patterns measured by the proposed PD sensors at DIV and 120% of DIV were the same as the results measured by MPD 600 based on IEC 60270. The proposed PD sensors can be installed on the inner wall of the transformer tank by coating its surfaces with a non-conductive material; therefore, it is possible to detect internal defects more effectively at a closer distance from the defect than the conventional sensors.

• Natural Product Sciences
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• 제28권4호
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• pp.187-193
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• 2022

Lysimachia christinae Hance was commonly used in Oriental medicine for treating the hepatitis virus, cholecystitis and cholagogic efficiency. According to the previous study, it possesses high antioxidant and anti-inflammatory activity. Simultaneous determination analytical method of isolated eight compounds, cynaroside (1), 2-(3,4-dimethoxyphenyl) ethyl O-α-L-arabinopyranosyl-(1→2)-O-[6-deoxy-α-L-mannopyranosyl-(1→3)] β-D-glucopyranoside (2), stearylester ricinoleic acid (3), (E)-4-(3,4-dimethoxyphenyl) but-3-en-1-yl palmitate (4), 2-hydroxy-24-methoxy-4-tetracosenoic acid (5), 2-hydroxy-24-propoxy-4-tetracosenoic acid (6), β-sitosterol (7), and androst-16-ene-3,6-diol (8) were established by using HPLC-DAD. This HPLC analysis was detected on a Dionex C18 column (5 ㎛, 120 Å, 4.6 mm × 150 mm) at 25℃. The mobile phase consisted of 0.1% trifluoroacetic acid and acetonitrile at a flow rate of 1 mL/min. Validation of the method was assessed by linearity, precision and accuracy test. Calibration curve was good at r² > 0.9998. Limits of detection (LOD) ranged from 0.19 to 8.18 g/ml and Limits of quantification (LOQ) ranged from 0.19 to 24.80 g/ml. The relative standard deviations (RSD) values of precision test, intra- and inter- day, were less than 0.99% and 1.0%. The accuracy test results ranged from 98.81% to 106.49% and RSD values were less than 0.95%. These results showed that the HPLC-DAD method was very reliable and accurate for the quantity analysis of eight compounds in L. christinae extract for quality control.

• 한국수산과학회지
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• 제56권4호
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• pp.428-437
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• 2023

A simultaneous analytical method was developed and validated for the analysis of prohibited fluoroquinolone (FQ) antibiotics including norfloxacin, ofloxacin, and pefloxacin, released by aquaculture in seawater and effluents. The samples were filtered, and extracts were obtained using a solid phase extraction cartridge with methanol (MeOH). The extracts were concentrated, and analyzed using ultra-performance liquid chromatography-tandem mass spectrometry. Two different columns and four different mobile phases were compared to achieve optimal separation and sensitivity for target compounds. Typical validation parameters including linearity, recovery of surrogate standard, instrument detection limit (IDL), limit of quantification (LOQ), and method detection limit (MDL) were evaluated. The linearity of calibration curves was over 0.999. Recoveries of surrogate ranged from 87.6% to 113%. The LOQ of target compounds was approximately 3-8 times lower than those reported in previous studies. The IDL and MDL were 0.06-0.57 and 0.06-0.37 ng/L, respectively. Seven effluent samples collected from an aquaculture located in Jeju were analyzed; however, not all target compounds were detected in the samples, suggesting that the banned antibiotics were not used. Overall, this established method was able to simultaneously analyze the three FQ antibiotics, and may be useful for monitoring prohibited antibiotics in the fishery industry.