• Bulletin of the Korean Chemical Society
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• v.34 no.12
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• pp.3659-3664
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• 2013

Eight representative explosives (ammonium perchlorate (AP), ammonium nitrate (AN), trinitrotoluene (TNT), 2,4-dinitrotoluene (DNT), cyclonite (RDX), cyclotetramethylenetetranitramine (HMX), pentaerythritol tetranitrate (PETN), and hexanitrostilbene (HNS)) were comprehensively analyzed with an ion trap mass spectrometer in negative ion mode using direct infusion electrospray ionization. MS/MS experiments were performed to generate fragment ions from the major parent ion of each explosive. Explosives in salt forms such as AP or AN provided cluster parent ions with their own anions. Explosives with an aromatic ring were observed as either $[M-H]^-$ for TNT and DNT or $[M]^{{\cdot}-}$ for HNS, while explosives without an aromatic ring such as RDX, HMX, and PETN were detected as an adduct ion with a formate anion, i.e., $[M+HCOO]^-$. These findings provide a guideline for the rapid and accurate detection of explosives once portable MS instruments become more readily available.

• Bulletin of the Korean Chemical Society
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• v.28 no.8
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• pp.1383-1388
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• 2007

Recently, the semiconductor and display industries have tried to reduce the emissions of perfluorocompounds (PFCs) from the globally environmental regulation. Total amount of PFC emission can be calculated from the flow rate and the partial pressures of PFCs. For the precise measurement of PFC emission amount, the mass flow controlled helium gas was continuously injected into the equipment of which scrubber efficiency is being measured. The partial pressures of PFCs and helium were accurately measured using a mass spectrometer in each sample extracted from inlet and outlet of the scrubber system. The flow rates are calculated from the partial pressures of helium and also, PFC destruction and removal efficiency (DRE) of the scrubber is calculated from the partial pressure of PFC and the flow rate. Under this method, the relative expanded uncertainties of the flow rate and the partial pressures of PFCs are ± 2% (k = 2) in case the concentrations of NF3 and SF6 are as low as 100 μmol/mol.

• YAKHAK HOEJI
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• v.60 no.1
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• pp.29-35
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• 2016

Traditional Korean medicines may be managed more scientifically, through the development of logical criterion to verify their cultivation region. It contributes to advance the industry of traditional herbal medicines. Volatile compounds were obtained from 14 samples of domestic Taeksa and 30 samples of Chinese Taeksa by steam distillation. The metabolites were identified by NIST mass spectral library in the obtained gas chromatography/mass spectrometer (GC/MS) data of 35 training samples. The multivariate statistical analysis, such as Principal Component Analysis (PCA), Partial Least Squares Discriminant Analysis (PLS-DA), and Orthogonal Partial Least Squares Discriminant Analysis (OPLS-DA), were performed based on the qualitative and quantitative data. Finally trans-(2,3-diphenylcyclopropyl)methyl phenyl sulfoxide (47.265 min), 1,2,3,4-tetrahydro-1-phenyl-naphthalene (47.781 min), spiro[4-oxatricyclo[5.3.0.0.(2,6)]decan-3-one-5,2'-cyclohexane] (54.62 min), 6-[7-nitrobenzofurazan-4-yl]amino-morphinan-4,5-epoxy (54.86 min), p-hydroxynorephedrine (55.14 min) were determined as marker metabolites to verify candidates for the origin of Taeksa. The statistical model was well established to determine the origin of Taeksa. The cultivation areas of test samples, each 3 domestic and 6 Chinese Taeksa were predicted by the established OPLS-DA model and it was confirmed that all 9 samples were precisely classified.

• YAKHAK HOEJI
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• v.58 no.3
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• pp.158-164
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• 2014

Dangguisu-san is a well-known traditional Korean herbal medicine prescription and has been widely used to treat ecchymosis, blood stagnation, and pain resulting from physical shock in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer method was established for the simultaneous determination of the 17 biomarker components in Dangguisu-san. All analytes were separated on an UPLC BEH $C_{18}$ ($100{\times}2.1$ mm, $1.7{\mu}m$) column and maintained at $45^{\circ}C$. The mobile phase consisted of two solvent systems, 0.1% (v/v) formic acid in water (A) and acetonitrile (B) by gradient flow. The injection volume was $2.0{\mu}l$ and the flow rate was 0.3 ml/min with detection at mass spectrometer. Calibration curves of the 17 biomarker components were acquired with $r^2$ values ${\geq}0.9951$. The values of limit of detection and quantification of all analytes were 0.02~6.32 ng/ml and 0.05~18.95 ng/ml, respectively. The amounts of the 17 components in Dangguisu-san sample were $3.17{\sim}13,224.50{\mu}g/g$.

• Analytical Science and Technology
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• v.26 no.6
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• pp.401-406
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• 2013

Oxygen($O_2$) consumption and carbon dioxide($CO_2$) excretion of a fertile chicken egg during incubation were measured by a gas mass spectrometer. A closed sample chamber was developed to collect gas samples during the 20 days of artificial incubation of both a fertile and an infertile egg. After leaving an egg in the sample chamber for an hour, using a gas-tight syringe, samples of 2 mL of gas were collected from the closed sample chamber and analyzed using a gas mass spectrometer in 2~4 day intervals. The $O_2$ consumption and $CO_2$ excretion of chicken embryos increased rapidly after 10 days from the starting point of incubation. After 20 days, 23 mL of $O_2$ was consumed and 16 mL of $CO_2$ was excreted per hour. Throughout the whole period of incubation, concentration of $O_2$ decreased 4.3 mol% and $CO_2$ increased only 3.1 mole%, i.e., the mole of consumed $O_2$ and the mole of excreted $CO_2$ were not the same. On the other hand, during the same period, concentration of $N_2$ increased about 1.3 mol% and the increased mole fraction of $N_2$ was comparable with the difference (1.2 mol%) between the mole fraction of consumed $O_2$ and excreted $CO_2$. Therefore, we can attribute the increase of $N_2$ mole% to the difference of mole fraction between consumed $O_2$ and excreted $CO_2$. In this study, through the analysis of gas, we could explain the respiration of a fertile chicken egg during incubation.

• Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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• 2001.06a
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• pp.1123-1123
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• 2001

In recent years, a miniature spectrometer has been extensively developed due to the marriage of fiber optics and semiconductor detector array. This type of miniature spectrometer has advantages of low price and robustness due to the capability of mass production and no moving parts are required such as lenses, mirrors and scanning monochromator. These systems are ideal for use in teaching labs, process monitoring and field analyses. A portable near infrared (NIR) system has been developed for qualitative and quantitative analysis. This system includes a tungsten halogen lamp for light source, a fiber optics connected a light source, and a sample module to the microspectrometer, The size of spectrometer can be as small as 2.5 cm x 1.5 cm x 0.1 cm. Wavelength ranges can be chosen as 360-800 nm, 800-1100 nm and 1100-1900 nm depending on the type of detector. The software consists of various tools for multivariate analysis and pattern recognition techniques. To evaluate the system, long and short-term stability, wavelength accuracy, and stray light have been investigated and compared with conventional scanning type NIR spectrometer. This developed system can be sufficiently used for quantitative and qualitative analysis for various samples such as agricultural product, herbal medicine, food, petroleum, and pharmaceuticals, etc.

• Journal of the Optical Society of Korea
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• v.13 no.2
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• pp.193-200
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• 2009

A compact imaging spectrometer (COMIS) is currently under development for use in the STSAT3 microsatellite. COMIS images the Earth's surface and atmosphere with ground sampling distances of ${\sim}30m$ in the $18{\sim}62$ spectral bands ($4.0{\sim}1.05{\mu}m$) for the nadir looking at an altitude of 700 km. COMIS has an imaging telescope and an imaging spectrometer box into which three electronics PCBs are embedded. These are designed into a single assembly with dimensions of 35(L) $\times$ 20(W) $\times$ 12(H) $cm^3$ and a mass of 4.3 kg. Optomechanical design efforts are focused on manufacturing ease, alignment, assembly, testing and improved robustness in space environments. Finite element analysis demonstrates that COMIS will survive in launch and space environments and perform the system modulation transfer function (MTF) in excess of 0.29 at the Nyquist frequency of the CCD detector (38.5 lines-per-mm).

• Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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• 2001.06a
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• pp.3114-3114
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• 2001

During the last years phytochemistry and phytopharmaceutical applications have developed rapidly and so there exists a high demand for faster and more efficient analysis techniques. Therefore we have established a near infrared transflectance spectroscopy (NIRS) method that allows a qualitative and quantitative determination of new polyphenolic pharmacological active leading compounds within a few seconds. As the NIR spectrometer has to be calibrated the compound of interest has at first to be characterized by using one or other a combination of chromatographic or electrophoretic separation techniques such as thin layer chromatography (TLC), high performance liquid chromatography (HPLC), capillary electrophoresis (CE), gas chromatography (GC) and capillary electrochromatography (CEC). Both structural elucidation and quantitative analysis of the phenolic compound is possible by direct coupling of the mentioned separation methods with a mass spectrometer (GC-MS, LC-MS/MS, CE-MS, CEC-MS) and a NMR spectrometer (LC-NMR). Furthermore the compound has to be isolated (NPLC, MPLC, prep. TLC, prep. HPLC) and its structure elucidated by spectroscopic techniques (UV, IR, HR-MS, NMR) and chemical synthesis. After that HPLC can be used to provide the reference data for the calibration step of the near infrared spectrometer. The NIRS calibration step is time consuming, which is compensated by short analysis times. After validation of the established NIRS method it is possible to determine the polyphenolic compound within seconds which allows to raise the efficiency in quality control and to reduce costs especially in the phytopharmaceutical industry.

• YAKHAK HOEJI
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• v.57 no.6
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• pp.400-405
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• 2013

In this study, we measured the complex efficiency of a physiologically active antibody, a chelator and radiosiotopes using the ESI-TOF/Ms system for develop good radiopharmaceuticals. For a precise measurement, TLC is a low accuracy method. Loading of same amount of sample is difficult for each test, and work to quantify accurately the results obtained through TLC cannot be afforded compared to the use of other analytical instruments. The method of analysis using a mass spectrometer is capable of a mass analysis of proteins for quantitative analysis. The conjugates of the chelator (CHX-A- DTPA) and the antibody (IgG) were separated through MWCO, and were analyzed using ESI-TOF and MALDI-TOF mass spectrometry. The analysis using MALDI-TOF is roughly divided into measurements on mass spectrometry. When conjugating a small molecular weight of CHX-A-DTPA and a large molecular weight of IgG, distinguishing the peak of the conjugate and the peak of IgG was difficult. However, an ESI-TOF mass spectrometer system is capable of an analysis of mass by decentralizing the IgG. It is utilized as a technique for measuring the metabolic processes during conjugation and the stability evaluation of radiopharmaceuticals. When establishing this technique, the accuracy of the overall radiophar-maceutical analysis is expected to be able to be improved.

• Mass Spectrometry Letters
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• v.9 no.3
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• pp.77-80
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• 2018

The focus of this paper is to present techniques to overcome certain difficulties in quantitative analysis with a time-of-flight mass spectrometer (TOF-MS). The method is based on conventional solid-phase extraction, followed by reversed-phase ultra high performance liquid chromatography of the extract, and mass spectrometric analysis. The target compounds included atenolol, atrazine, caffeine, carbamazepine, diclofenac, estrone, ibuprofen, naproxen, simazine, sucralose, sulfamethoxazole, and triclosan. The matrix effects caused by high concentrations of organic compounds in wastewater are especially significant in electrospray ionization mass spectroscopy. Internal-standard calibration with isotopically labeled standards corrects the results for many matrix effects, but some peculiarities were observed. The problems encountered in quantitation of carbamazepine and triclosan, due to nonlinear calibration were solved by changing the internal standard and using a narrower mass window. With simazine, the use of a quadratic calibration curve was the best solution.