• Title/Summary/Keyword: Reaction monitoring

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Determination of methamphetamine and amphetamine enantiomers in human urine by chiral stationary phase liquid chromatography-tandem mass spectrometry

  • Sim, Yeong Eun;Ko, Beom Jun;Kim, Jin Young
    • Analytical Science and Technology
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    • v.32 no.5
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    • pp.163-172
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    • 2019
  • Methamphetamine (MA) is currently the most abused illicit drug in Korea and its major metabolite is amphetamine (AP). As MA exist as two enantiomers with the different pharmacological properties, it is necessary to determine their respective amounts in a sample. Thus a chiral stationary phase liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed for identification and quantification of d-MA, l-MA, d-AP, and l-AP in human urine. Urine sample ($200{\mu}L$) was diluted with pure water and purified using solid-phase extraction (SPE) cartridge. A $5-{\mu}L$ aliquot of SPE treated sample solution was injected into LC-MS/MS system. Chiral separation was carried out on the Astec Chirobiotic V2 column with an isocratic elution for each enantiomer. Identification and quantification of enantiomeric MA and AP was performed using multiple reaction monitoring (MRM) detection mode. Linear regression with a $1/x^2$ as the weighting factor was applied to generate a calibration curve. The linear ranges were 25-1000 ng/mL for all compounds. The intra- and inter-day precisions were within 3.6 %, while the intra- and inter-day accuracies ranged from -5.4 % to 11.8 %. The limits of detection were 2.5 ng/mL (d-MA), 3.5 ng/mL (l-MA), 7.5 ng/mL (d-AP), and 7.5 ng/mL (l-AP). Method validation parameters such as selectivity, matrix effect, and stability were evaluated and met acceptance criteria. The applicability of the method was tested by the analysis of genuine forensic urine samples from drug abusers. d-MA is the most common compound found in urine and mainly used by abusers.

Ultrasonic, Chemical Stability and Preparation of Self-Assembled Fullerene$[C_{70}]$-Gold Nanoparticle Films (자기조립 풀러렌$[C_{70}]$-금 나노입자 필름 제조와 초음파적, 화학적 안정성)

  • Ko, Weon-Bae;Shon, Young-Seok
    • Elastomers and Composites
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    • v.40 no.4
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    • pp.272-276
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    • 2005
  • [ $C_{70}$ ]-gold nanoparticle multilayer films were self-assembled using a 'dirt-ball' method on the reactive surface of glass slides functionalized with 3-aminopropyltrimethoxysilane. The functionalized glass slides were soaked in the solution containing both unmodified $C_{70}$ and ${\omega}$-amino-functionalized gold nanoparticles. Organic reaction (amination) facilitated the assembly of multilayer $C_{70}$-gold nanoparticle films, which have grown up to several layers. Chemical stability of $C_{70}$-gold nanoparticle films was studied by monitoring the changes in absorbance after the immersion of the films in acidic solution. In addition, ultrasonic stability of these nanoparticle films was studied by exposing them to ultrasonic irradiated surrounding, which resulted in partial desorption and a little aggregation of nanoparticles on solid surfaces.

The method for total organic carbon analysis employing TiO2 photocatalyst (이산화티타늄 광촉매를 이용한 총유기탄소 분석방법)

  • Park, Buem Keun;Kim, Sung Mi;Lee, Young-Jin;Paik, Jong-Hoo;Shin, Jeong Hee
    • Journal of Sensor Science and Technology
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    • v.30 no.5
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    • pp.320-325
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    • 2021
  • Biochemical oxygen demand (BOD) and chemical oxygen demand (COD) methods are conventional analytical methods to analyze water quality. Both of these methods are technically indirect measurement methods, require complicated preconditions, and are time-consuming. On the other hand, the total organic carbon (TOC) method is a direct and fast measurement method which is more intuitive and accurate than the BOD and COD methods. However, general TOC analysis methods involve complicated processes and high power consumption owing to the process of phase transition from liquid to gas by a high-temperature heater. Furthermore, periodic consumables are also required for the removal of inorganic carbon (IC). Titanium dioxide (TiO2) is one of the most suitable photocatalysts for simple processes. Its usage involves low power consumption because it only reacts with the organic carbon (OC) without the requirement of any other reagents and extra processes. We investigated a TiO2 photocatalyst-based TOC analysis for simple and affordable products. TiO2-coated fiber substrate maintained under carbon included water was exposed to ultraviolet (UV) radiation of wavelength 365 nm. This method is suitable for the real-time monitoring of water pollution because of its fast reaction time. Its linear property is also sufficient to match the real value.

Design of a scintillator-based prompt gamma camera for boron-neutron capture therapy: Comparison of SrI2 and GAGG using Monte-Carlo simulation

  • Kim, Minho;Hong, Bong Hwan;Cho, Ilsung;Park, Chawon;Min, Sun-Hong;Hwang, Won Taek;Lee, Wonho;Kim, Kyeong Min
    • Nuclear Engineering and Technology
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    • v.53 no.2
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    • pp.626-636
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    • 2021
  • Boron-neutron capture therapy (BNCT) is a cancer treatment method that exploits the high neutron reactivity of boron. Monitoring the prompt gamma rays (PGs) produced during neutron irradiation is essential for ensuring the accuracy and safety of BNCT. We investigate the imaging of PGs produced by the boron-neutron capture reaction through Monte Carlo simulations of a gamma camera with a SrI2 scintillator and parallel-hole collimator. GAGG scintillator is also used for a comparison. The simulations allow the shapes of the energy spectra, which exhibit a peak at 478 keV, to be determined along with the PG images from a boron-water phantom. It is found that increasing the size of the water phantom results in a greater number of image counts and lower contrast. Additionally, a higher septal penetration ratio results in poorer image quality, and a SrI2 scintillator results in higher image contrast. Thus, we can simulate the BNCT process and obtain an energy spectrum with a reasonable shape, as well as suitable PG images. Both GAGG and SrI2 crystals are suitable for PG imaging during BNCT. However, for higher imaging quality, SrI2 and a collimator with a lower septal penetration ratio should be utilized.

The Development and Selection of SSR Markers for Identification of Peanut (Arachis hypogaea L.) Varieties in Korea

  • Han, Sang-Ik;Bae, Suk-Bok;Ha, Tae Joung;Lee, Myong-Hee;Jang, Ki-Chang;Seo, Woo-Duck;Park, Geum-Yong;Kang, Hang-Won
    • Korean Journal of Breeding Science
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    • v.43 no.2
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    • pp.133-138
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    • 2011
  • The groundnut or cultivated peanut (Arachis hypogaea L.) in Korea consists of 36 domestic varieties which have been developed and registered as cultivars for the public during last 25 years. To screen and identify of Korean peanut varieties and genetic resources, we present a simple and reliable method. A methodology based on simple sequence repeat (SSR) markers developed and widely used for prominent gene identification and variety discrimination. For identification of those 36 Korean peanut varieties, 238 unique peanut SSR markers were selected from some previously reported results, synthesized and used for polymerase chain reaction (PCR). Data were taken through acryl amide gel electrophoresis and changed into proper formats for application of data mining analysis using Biomine (all-in-one functional genomics data mining program). Consequently, twelve SSR primers were investigated and revealed the differences between those 36 varieties. These primer pairs amplified 27 alleles with an average of 2.3 allele per primer pair. In addition, those results showed genetic relationship by classification method within 36 varieties. The approach described here could be applied to monitoring of our varieties and adapting to peanut breeding program.

Development and validation of LC-MS/MS for bioanalysis of hydroxychloroquine in human whole blood

  • Park, Jung Youl;Song, Hyun Ho;Kwon, Young Ee;Kim, Seo Jin;Jang, Sukil;Joo, Seong Soo
    • Journal of Biomedical and Translational Research
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    • v.19 no.4
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    • pp.130-139
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    • 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.

Psychiatric Symptoms after Taking Oseltamivir in a Child and Its Causality Assessment (Oseltamivir 복용 이후 소아에서 발생한 이상행동 및 그 인과성 평가)

  • Son, Pyoungwoo;Choi, Joonghyuk;Lee, Seungmin;Park, Seon Soon;Choi, Eunkyung;Yoo, Bong-Kyu;Ji, Eunhee
    • Korean Journal of Clinical Pharmacy
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    • v.29 no.1
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    • pp.56-60
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    • 2019
  • Oseltamivir is an antiviral medication prescribed to prevent and treat influenza A and B. A case from a community pharmacy in Korea was reported for an adverse event associated with oseltamivir administration. A 20-month-old boy had psychiatric symptoms after receiving 2 doses of oseltamivir. Therefore, an evaluation of whether the psychiatric symptoms were caused by oseltamivir was required. To determine whether the adverse event resulted from the administrated medication or other factors, three tools were used: the Naranjo scale, the Korean causality assessment algorithm (Ver.2), and the World Health Organization-Uppsala Monitoring Center (WHO-UMC) criteria. The psychiatric symptoms occurred after oseltamivir administration, and were attenuated after oseltamivir termination. A possible cause of the psychiatric symptoms is high fever, but information on the body temperature of the patient was not sufficient. Therefore, it was unclear whether there were other nonpharmacological causes of adverse drug reaction. For these reasons, in terms of causality, the results evaluated by the three tools represented, "possible", "probable", and "probable/likely", respectively.

Characterization of the Interaction between White Ginseng Extract and Selegiline Using Triple Quadrupole-Mass Spectrometry

  • Cho, Pil Joung;Liu, Kwang-Hyeon;Song, Im-Sook;Song, Kyung-Sik;Lee, Sangkyu
    • Mass Spectrometry Letters
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    • v.10 no.2
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    • pp.61-65
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    • 2019
  • Korean ginseng (Panax ginseng Meyer) is a traditional herb used across the world to treat various diseases. Although, red ginseng is this herb's most famous product and has demonstrated diverse pharmacological activities, white ginseng (WG) is another ginseng product that is made fresh and individually regulated in Eastern Asia. Red and white ginseng show different characteristics due to distinct processing steps despite originating from the same plant, and the drug interactions induced by WG have not been well documented. Selegiline is a selective monoamine oxidase (MAO) inhibitor used as an antidyskinetic and antiparkinsonian agent. Here we developed a quantification method for selegiline in mouse plasma using a C8 stationary phase in triple quadrupole-mass spectrometry (LC-MS/MS) with multiple reaction monitoring (MRM). The validated LC-MS/MS method was successfully applied to determine the potential interaction with WG extract (0.1 g/kg/day) pre-administered for 4 weeks. The $AUC_{0-240min}$ of selegiline was altered due to a decrease in the absorption of selegiline with repeated administration of WG extract.

Development and Validation of an LC-MS/MS Method for Determination of Damaurone D in Rat Plasma and its Application to Pharmacokinetic Study in Rats

  • Lee, Wonpyo;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Mass Spectrometry Letters
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    • v.10 no.1
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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.

Analysis of the Marker Compounds in Sagunja-tang by LC-ESI-MS (LC-ESI-MS에 의한 사군자탕의 지표성분 분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.50 no.1
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    • pp.65-71
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    • 2019
  • One of the oriental medicine prescriptions, Sagunja-tang consists of four herbal medicines (Ginseng Radix, Poria Sclerotium, Atractylodis Rhizoma Alba, and Glycyrrhiziae Radix et Rhizoma) and has been used as a medicine to enhance tonify the function of spleen and stomach in Korea. In this study, we conducted simultaneous analysis of the 9 marker components, liquiritin apioside, liquiritin, ginsenoside Rg1, liquiritigenin, ginsenoside Rb1, glycyrrhizin, atractylenolide III, atractylenolide II, and atractylenolide I in Sagunja-tang using a liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS/MS). Marker compounds were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, 1.7 mm) and the column was maintained at $45^{\circ}C$. The mobile phase consists of 0.1% (v/v) aqueous formic acid and acetonitrile with gradient condition. The LC-MS analysis was performed using a Waters ACQUITY TQD LC-MS/MS system with multiple reaction monitoring (MRM) method in the positive and negative modes. The calibration curves of the nine marker components showed good linearity with coefficient of determination ${\geq}0.9984$ within tested range. The limits of detection and limits of quantification values were 0.27-2.42 ng/mL and 0.81-7.27 ng/mL, respectively. The concentrations of tested 9 analytes in the lyophilized Sagunja-tang sample using the established LC-ESI-MS/MS MRM method were detected up to 16.593 mg/g. These results can be useful as a basic data for the quality control of an oriental medicine prescriptions.