• Bulletin of the Korean Chemical Society
• /
• v.30 no.2
• /
• pp.363-367
• /
• 2009

An isotope-dilution flow-injection electrospray/mass spectrometric method was developed for the accurate determination of glucosamine contents in pharmaceutical formulations. Samples were extracted by methanol. After spiking glucosamine-1-$^{13}C_1$ as an internal standard, the extracts were then analyzed by flow-injection ESI/MS in a selected ion monitoring (SIM) mode to detect [M+H]$^+$ ions of the analyte and its isotope analogue at m/z 180 and m/z 181, respectively. Confirmatory measurements were made by selectively monitoring the collisionally induced dissociation channels of m/z 180 $\rightarrow$ m/z 72 and m/z 181 $\rightarrow$73, respectively, to test the possibility of bias in the SIM method due to matrix interferences, but any significant bias in the SIM mode was not observed. Repeatability and reproducibility studies showed that the flow-injection ESI/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0 %. Other results for the method validation are reported.

• Analytical Science and Technology
• /
• v.18 no.6
• /
• pp.520-528
• /
• 2005

Two biological Certified Reference Materials (CRMs), KRISS 108-04-001 (oyster tissue) and 108-05-001 (water dropwort stem), were prepared by Korea Research Institute of Standards and Science (KRISS)during FY '01. The certified values of these materials had been determined by Isotope Dilution Mass Spectrometry (IDMS) for six elements (Cd, Cr, Cu, Fe, Pb and Zn). Additional analytical works are now progressing to certify the concentrations of a number of the environmental and nutrimental elements in these CRMs. The certified values in a CRM are usually determined by using a single primary method with confirmation by other method(s) or using two independent critically-evaluated methods. Instrumental Neutron Activation Analysis (INAA) plays an important role in the determination of certified values as it can eliminate the possibility of common error sources resulting from sample dissolution. In this study INAA procedure was used in determination of 23 elements in these two biological CRMs to acquire the concentration information and the results were compared with KRISS certified values.

• Archives of Pharmacal Research
• /
• v.6 no.1
• /
• pp.7-16
• /
• 1983

A methadone-diazepam interaction study in rats was performed in which conjugated metabolites of methadone were analyzed using deuterated biosynthetic internal standards. Diazepam (5mg/kg) was given to rats through a cannulate djugular vein and a subcutaneous dose of methadone (10mg/kg) was given. Bile was collecte through the cannulate dbile duct over a period of 24 hours. The deuterium label of the internal standards was found to be stable under conditions of the prolonged incubation. There was no significant difference in the excretion of the metabolites between the control and the diazepam treated rats. Feasibility of using biosynthetic internal standards with selected ion monitoring was established for the drug metabolism and kinetic studies.

• International conference on construction engineering and project management
• /
• 2015.10a
• /
• pp.714-715
• /
• 2015

Drill and blast method has been most widely used in tunnel excavation, after NATM (New Austrian Tunneling Method) was introduced in 1983. The NATM method utilized mass of shotcrete to secure the bearing capacity of tunnels. Overbreak defined how much larger the actual excavation was than the planned. When it became larger, more shotcrete was required to fill in it Here, payline fixed allowable overbreak, referring to payable amounts of shotcrete. Since owner was not responsible for shotcrete exceeding payline, it was important to properly establish the standards for payline. Although the standards were provided in 'Poom-sam'(standardized quantity per unit), they did not properly reflect the actual conditions for excavation. Thus, this study reviewed existing domestic and foreign standards for overbreak, and estimated overbreak for each type of support using survey data, and finally provided the improvements on the current standards.

• Journal of the Korean Society for information Management
• /
• v.25 no.3
• /
• pp.231-247
• /
• 2008

The purpose of this study was to try to describe types of invasion of privacy caused by excessive information seeking on mass media. Recent 5 years of cases were gathered and analyzed to see the types of invasion of privacy, and extracted only those cases showing the results by excessive information seeking. Three standards such as the intension, the subject, and the characteristics were selected to differentiate the types and cases. Five types of those three standards were introduced by case by case. The issues regarding ways of privacy protection and correct attitude of information seeking were explored and a few suggestions were included at the end.

• Bulletin of the Korean Chemical Society
• /
• v.34 no.6
• /
• pp.1698-1702
• /
• 2013

Glucose is a common medical analyte measuring in human serum or blood samples. The development of a primary method is necessary for the establishment of traceability in measurements. We have developed an isotope dilution liquid chromatography tandem mass spectrometry as a primary method for the measurement of glucose in human serum. Glucose and glucose-$^{13}C_6$ in sample were ionized in ESI negative mode and monitored at mass transfers of m/z 179/89 and 185/92 in MRM, respectively. Glucose was separated on $NH_2P$-50 2D column, and the mobile phase was 20 mM $NH_4OAc$ in 30% acetonitrile/70% water. Verification of this method was performed by the comparison with NIST SRMs. Our results agreed well with the SRM values. We have developed two levels of glucose serum certified reference material using this method and distributed them to the clinical laboratories in Korea as samples for proficiency testings. The expended uncertainty was about 1.2% on 95% confidence level. In proficiency testings, the results obtained from the clinical laboratories showed about 3.6% and 3.9% RSD to the certified values. Primary method can provide the traceability to the field laboratories through proficiency testings or certified reference materials.

• Mass Spectrometry Letters
• /
• v.8 no.4
• /
• pp.79-89
• /
• 2017

Ion mobility mass spectrometry (IM-MS) combines the advantages of ion mobility spectrometry (IMS) and MS for effective gas-phase ion analysis. Separation of ions based on their mobilities prior to MS can be performed without a great loss in other analytical figures of merit, and the extra dimension of analysis offered by IM can be beneficial for isomer and complex sample analyses. In this review, basic principles of IMS and IM-MS are described in addition to an introduction to various IMS techniques and commercial IM-MS instruments. The nature of collision cross-section (${\Omega}_D$), an important parameter determining the transport properties of ions in IMS, is also explained in detail.

• Mass Spectrometry Letters
• /
• v.7 no.4
• /
• pp.102-105
• /
• 2016

This study explored the feasibility of using a carburization technique to enhance the ion intensity of isotopic analysis of ultra-trace levels of uranium using thermal ionization mass spectrometry (TIMS). Prior to fixing uranium samples on TIMS filaments, graphite powder suspended in nitric acid was deposited on rhenium filaments. We observed an enhancement of $^{238}U^+$ intensity by a factor of two when carburization was used, and were able to roughly optimize the amount of graphite powder necessary for carburization. The positive shift in heating current when evaporating filaments upon carburization implies that uranium was chemically altered by carburization, when compared to normal fixation processes. The good agreement between our method and known standards down to an ultra-trace level shows that the proposed technique can be applied to isotopic uranium analysis down to abundances of ~10 pg.

• Mass Spectrometry Letters
• /
• v.5 no.1
• /
• pp.12-15
• /
• 2014

Thermal ionization mass spectrometry (TIMS) was used to determine the concentration and isotope ratio of uranium contained in samples of soil and groundwater collected from Korea. Quantification of uranium in ground water samples was performed by isotope dilution mass spectrometry. A series of chemical treatment processes, including chemical separation using extraction chromatography, was applied to the soil samples to extract the uranium. No treatments other than filtration were applied to the groundwater samples. Isotopic analyses by TIMS showed that the isotope ratios of uranium in both the soil and water samples were indistinguishable from those of naturally abundant uranium. The concentration of uranium in the groundwater samples was within the U.S. acceptable standards for drinking water. These results demonstrate the utility of TIMS for monitoring uranium in environmental samples with high analytical reliability.

• Analytical Science and Technology
• /
• v.35 no.5
• /
• pp.205-211
• /
• 2022

Deuterium (D) is an isotope with one more neutron number than hydrogen (H). Heavy elements rarely change their chemical properties with little effect even if the number of neutrons increases, but low-mass elements change their vibration energy, diffusion rate, and reaction rate because the effect cannot be ignored, which is called an isotope effect. Recently, in the semiconductor and display industries, there is a trend to replace hydrogen gas (H₂) with deuterium gas (D₂) in order to improve process stability and product quality by using the isotope effect. In addition, as the demand for D₂ in industries increases, domestic gas producers are making efforts to produce and supply D₂ on their own. In the case of high purity D₂, most of them are produced by electrolysis of heavy water (D₂O), and among D₂, hydrogen deuteride (HD) molecules are present as isotope impurities. Therefore, in order to maximize the isotope effect of hydrogen in the electronic industry, HD, which is an isotope impurity of D₂ used in the process, should be small amount. To this end, purity analysis of D₂ for industrial processing is essential. In this study, HD quantitative analysis of D₂ for high purity D₂ purity analysis was established and hydrogen isotope RM (Reference material) was developed. Since hydrogen isotopes are difficult to analyze with general gas analysis instrument, they were analyzed using a high-precision mass spectrometer (Gas/MS, Finnigan MAT271). High purity HD gas was injected into Gas/MS, sensitivity was determined by a signal according to pressure, and HD concentrations in two bottles of D₂ were quantified using the corresponding sensitivity. The amount fraction of HD in each D₂ was (4518 ± 275) μmol/mol, (2282 ± 144) μmol/mol. D₂, which quantifies HD amount using the developed quantitative analysis method, will be manufactured with hydrogen isotope RM and distributed for quality management and maintenance of electronic industries and gas producers in the future.