• Title/Summary/Keyword: MS analysis

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Rapid Quantitative Analysis of Vancomycin in Human Plasma and Urine Using LC-MS/MS (LC - MS/MS를 이용한 혈장과 뇨중에서 Vancomycin의 빠른정량분석)

  • Kim, Hohyun;Roh, Hyeongjin;Han, Sang-Beom
    • Analytical Science and Technology
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    • v.15 no.5
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    • pp.410-416
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    • 2002
  • In this study, a new quantitative analytical method has been developed for the rapid determination of vancomycin in human plasma and urine using liquid chromatography/tandem mass spectrometry (LC - MS/MS). Chromatography was carried out on a $C_{18}$ XTerra MS column ($2.1{\times}30mm$) with a particle size of $3.5{\mu}m$. The mobile phase was 0.25% formic acid in 10% acetonitrile and the flow rate was $250{\mu}L/min$. Vancomycin and caffeine (internal standard) were detected by MS/MS using multiple reaction monitoring (MRM). Vancomycin gives a predominant doubly protonated precursor molecule ($[M+2H]^{2+}$) at m/z 725.0 and a corresponding product ion of m/z 100.0. Detection of vancomycin was good, accurate and precise, with a limit of detection of 1 nM in plasma. The calibration curves for vancomycin in human plasma was linear in a concentration range of $0.01{\mu}M$ - $100{\mu}M$ for plasma. This method has been successfully applied to determine the concentration of vancomycin in human plasma and urine from pharmacokinetic study and relative studies.

Manufacturing and Characteristics Analysis of a Testing Device for the Evaluation of a Distribution Board Management System (분전반 관리시스템 평가를 위한 시험 장치의 제작 및 특성 분석)

  • Ko, Wan Su;Lee, Byung Seol;Choi, Chung Seog
    • Journal of the Korean Society of Safety
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    • v.34 no.5
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    • pp.31-36
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    • 2019
  • This study made a testing device to evaluate the distribution board management system. Power was supplied to the testing device using a loading-back method and the voltage applied to it was 440 V at the same turn ratio. When the human body electric shock current is 30 mA, the breaking time is set to be less than 240 ms while 30~45 mA current is flowing. The test result shows that in the case of the R-phase it was measured to be 5.19 Hz (193 ms). And the S-phase and T-phase were perfectly cut off at 5.39 Hz (186 ms) and 5.71 Hz (175 ms), respectively. When the human body electric shock current is 60mA, the breaking time is set to be less than 120 ms while 45~75 mA current is flowing. The test result shows that the R-phase, S-phase, and T-phase were accurately cut off at 8.39 Hz (11 ms), 8.87Hz (113 ms) and 9.69 Hz (103 ms), respectively. When the human body electric shock current is 90 mA, the breaking time is set to be less than 48 ms while 75 mA current is flowing. The test result shows that the R-phase, S-phase, and T-phase were accurately cut off at 19.8 Hz (50.4 ms), 16.9 Hz (59.2 ms), and 17.9 Hz (56.0 ms), respectively. That is, the developed testing device satisfied all the requirements of the distribution board evaluation criteria, and it becomes available for the performance evaluation of the distribution board management system.

Comparison of Ignition Delay Time of Petroleum-based and Bio Aviation Fuel (석유계 및 바이오 항공유의 점화지연시간 비교)

  • Kang, Saetbyeol;Han, Jeongsik;Jeong, Byunghun
    • Journal of the Korean Society of Propulsion Engineers
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    • v.22 no.6
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    • pp.118-125
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    • 2018
  • This study aimed to obtain data for a comparative analysis of the properties of bio aviation fuel to be developed in the future by measuring and comparing the ignition delay times of various presently used aviation fuels. In the case of petroleum-based aviation fuel, the ignition delay time of exo-THDCP was 4.92 ms, which was 3.42 times longer than 1.44 ms of Jet A-1 at $590^{\circ}C$ / 55 bar. In the case of foreign bio aviation fuel, the ignition delay time of 11POSF7629 was the longest (1.16 ms), while the ignition delay time of 10POSF6308 (1.06 ms), 12POSF7720 (1.07 ms), and 07POSF5172 (1.05 ms) were similar.

The feasibility of percutaneous transhepatic gallbladder aspiration for acute cholecystitis after self-expandable metallic stent placement for malignant biliary obstruction: a 10-year retrospective analysis in a single center

  • Akihisa Ohno;Nao Fujimori;Toyoma Kaku;Masayuki Hijioka;Ken Kawabe;Naohiko Harada;Makoto Nakamuta;Takamasa Oono;Yoshihiro Ogawa
    • Clinical Endoscopy
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    • v.55 no.6
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    • pp.784-792
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    • 2022
  • Background/Aims: Patients with acute cholecystitis (AC) after metallic stent (MS) placement for malignant biliary obstruction (MBO) have a high surgical risk. We performed percutaneous transhepatic gallbladder aspiration (PTGBA) as the first treatment for AC. We aimed to identify the risk factors for AC after MS placement and the poor response factors of PTGBA. Methods: We enrolled 401 patients who underwent MS placement for MBO between April 2011 and March 2020. The incidence of AC was 10.7%. Of these 43 patients, 37 underwent PTGBA as the first treatment. The patients' responses to PTGBA were divided into good and poor response groups. Results: There were 20 patients in good response group and 17 patients in poor response group. Risk factors for cholecystitis after MS placement included cystic duct obstruction (p<0.001) and covered MS (p<0.001). Cystic duct obstruction (p=0.003) and uncovered MS (p=0.011) demonstrated significantly poor responses to PTGBA. Cystic duct obstruction is a risk factor for cholecystitis and poor response factor for PTGBA, whereas covered MS is a risk factor for cholecystitis and an uncovered MS is a poor response factor of PTGBA for cholecystitis. Conclusions: The onset and poor response factors of AC after MS placement were different between covered and uncovered MS. PTGBA can be a viable option for AC after MS placement, especially in patients with covered MS.

Development and Verification of a Simultaneous Analytical Method for Whole Blood Metals and Metalloids for Biomonitoring Programs (바이오모니터링 프로그램을 위한 혈중 금속류 동시분석법 개발 및 확인 평가)

  • Cha, Sangwon;Oh, Eunha;Oh, Selim;Han, Sang Beom;Im, Hosub
    • Journal of Environmental Health Sciences
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    • v.47 no.1
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    • pp.64-77
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    • 2021
  • Objective: Biological monitoring of trace elements in human blood samples has become an important indicator of the health environment. The purpose of this study was to detect and evaluate multiple metal items in blood samples based on ICP-MS, to perform comparative evaluation with the existing analysis method, and to develop and verify a new method. Methods: 100 μL of whole blood from 80 healthy subjects was used to analyze ten metals (Sb, tAs, Cd, Pb, Mn, Hg, Mo, Ni, Se, Tl) using ICP-MS. Verification of the analysis method included calculation of linearity, accuracy, precision and detection limits. In addition, a comparative test with the conventional graphite furnace atomic absorption spectroscopy (GF-AAS) method was performed. In the case of Pb, Cd, and Hg in whole blood, cross-analysis between Pb, Cd, and Hg analysis methods was performed to confirm the difference between the existing method and the new method (ICP-MS). Results: The coefficient of determination (R2) was 0.999 or higher in seven items and 0.995 or higher in three items. The Pb result showed that Pearson's correlation coefficient was very high at 0.983, and the intraclass correlation coefficient was 0.966. The Cd result showed that Pearson's correlation coefficient was 0.917 between the existing method and the new analysis concentration value. Its intraclass correlation coefficient was 0.960, and there was no significant difference between the two groups. Hg had a low correlation at 0.687, and the intraclass correlation coefficient was 0.761, which was lower than that of Pb and Cd. The intra-day and inter-day accuracy of Pd and Cd were satisfactory, but Hg did not meet the criteria for both accuracy and precision when compared with the conventional analysis method. Conclusion: This study can be meaningful in that it proposes a more efficient and feasible analysis method by verifying a blood heavy metal concentration experiment using multiple simultaneous analyses. All samples were processed and analyzed using the new ICP-MS. It was confirmed that the agreement between the two methods was very high, with the agreement between the current and new methods being 0.769 to 0.998. This study proposes an efficient simultaneous methodology capable of analyzing multiple elements with small samples. In the future, studies of various applications and the reliability of ICP-MS analysis methods are required, and research on the verification of accurate, precise, and continuous analysis methods is required.

A Study on the Analysis of Five Artificial Sweetners in Beverages by HPLC/MS/MS (HPLC/MS/MS를 이용한 음료류 중 인공감미료 동시분석에 관한 연구)

  • Lee, Seong-Bong;Yong, Kum-Chan;Hwang, Sun-Il;Kim, Young-Su;Jung, You-Jung;Seo, Mi-Young;Lee, Chang-Hee;Sung, Jin-Hee;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.29 no.4
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    • pp.327-333
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    • 2014
  • A method for analysis of five artificial sweetners (sodium saccharin, aspartame, acesulfame-K, sucralose, cyclamate) in beverage samples was developed using high-performance liquid chromatography/triple quadrupole mass spectrometry (HPLC/MS/MS). The method uses a single-step dilution for sample preperation. Seperation was achieved on a $C_{18}$ column ($2.1{\times}150mm$, $3.5{\mu}m$) with A- 2% methanol (1 mM ammonium acetate), B-95% methanol (1 mM ammonium acetate) as mobile phase with gradient mode. The quantitation of target compounds was performed by external calibration in selected reaction monitorning (SRM) mode. The coefficient of determination of calibration curve for sodium saccharin, aspartame, acesulfame-K, sucralose and cyclamate were 0.9957, 0.9991, 0.9943, 0.9982 and 0.9948, respectively. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 0.001~0.022 mg/L and 0.004~0.073 mg/L, repectively. Recoveries for beverage samples were in the range of 92.76~113.50% with RSD < 10.91%. The method has applied to the determination of the five sweetners in 102 beverage samples. Three artificial sweetners-aspartame, acesulfame-K, sucralose were detected from 42 samples. Sodium saccharin and cyclamate were not detected in all samples.

Analysis of Fatty Acyl Groups of Diacyl Galactolipid Molecular Species by HPLC/ESI-MS with In-source Fragmentation

  • Gil, Ji-Hye;Hong, Jong-Ki;Choe, Joong-Chul;Kim, Young-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.24 no.8
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    • pp.1163-1168
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    • 2003
  • The structures of molecular species of galactolipids, such as monogalactosyl diacylglycerol (MGDG) and digalactosyl diacylglycerol (DGDG), isolated from wheat flour have been investigated using negative-ion electrospray ionization (ESI) mass spectrometry interfaced with high performance liquid chromatography (HPLC). According to the result of HPLC analysis, MGDG and DGDG were found to consist of mixtures of five and four molecular species, respectively. The galactolipids have been also analyzed to determine their fatty acid compositions, using HPLC/ESI-MS combined with in-source (or cone voltage) fragmentation. HPLC/ ESI-MS is very useful for one-step analysis of mixtures of galactolipids with a small sample quantity. Especially, the carboxylate anions produced in in-source fragmentations of the negative-ion of each component separated by HPLC provide valuable information on the composition of its fatty acyl chains.