• Analytical Science and Technology
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• v.22 no.3
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• pp.235-246
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• 2009

The analyses of minor and trace elements in glass debris were performed using LA-ICP-MS in order to identify manufacturers using real commercial samples. At first, a calibration curve was made using standard glass samples of NIST 610, 612, 614 and 616. $^{29}Si$ was used as an internal standard, and the ratios of metal/Si for each metal were compared with their concentrations. Based on elements in each sample and standard materials, 24 metals were quantified and the LOD in analysis, according to the blank sample, was in the range of 0.11 mg/kg (Ti)-4.91 mg/kg (Ca). Eleven samples from two manufacturers were collected and five sub-samples were taken from each sample for analysis. 15 elements (Co, Ce, Ca, Mn, Sr, Ba, Li, Rb, U, La, Th, Na, Al, Zr and Hf) were selected to identify manufacturers because some elements (Cu, Cr, Cd and Ni) were below the detection limit and some elements (Ti, Pr, Mg, Nb, Nd) were absent in the analysis of standards and others (Pb and Sn) had a problem of homogeneity. The attempts to identify manufacturers and the manufacturing period were performed through a triangular diagram. In the manufacturer discrimination by discriminant analysis, a canonical discriminant function was made based on Mn, Ce and Rb, and each sample could be identified.

• Tuberculosis and Respiratory Diseases
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• v.42 no.1
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• pp.84-92
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• 1995

Background: Nasal applied continuous positive airway pressure(CPAP) is a highly effective method of treatment for obstructive sleep apnea syndrome. More than a decade of accumulated experience with this treatment modality confirmed that it is unquestionably the medical treatment of choice for patients with obstructive sleep apnea syndrome. However it takes long time to reach optimal CPAP pressure. To save the time to reach optimal pressure, it is necessary to clarify the time to reach optimal pressure for treatment of obstructive sleep apnea syndrome. Method: CPAP pressure is titrated during an overnight study according to a standardized protocol. Just before the presleep bio-calibration procedures, the technician applies the nasal mask and switches on the clinical CPAP unit. Initial positive for pressure is typically 3.0 centimeters of water pressure. After sleep onset, the technician gradually increases the pressure until sleep-disordered breathing events disappear or become minimal. The pressure must maintain maximal airway patency during both NREM and REM sleep to be considered effective. Before recommending a final pressure setting, sleep recording and oximetry data are reviewed by an American Board of Sleep Medicine certified Sleep Specialist and a Registrered Polysomnographic Technologist. Results: We examined the time required to reach optimal pressure during routine CPAP titration in 127 consecutively evaluated individuals diagnosed with sleep-disordered breathing. Results indicate that 33% of patients required more than four hours to attain satisfactory titration. This indicates that a four-hour session is marginally enough time, at best, to determine a proper CPAP pressure setting. Moreover, 60 of 127 patients required further adjustment after optimal pressure was reached. These additional pressure trials were needed to confirm that higher pressures were not superior for eliminating sleep-disordered breathing events. Conclusions: The data presented underscore the logistical difficulty of titrating CPAP during split-night studies without modifying the titration procedure. Futhermore, the time needed to reach optimal pressure makes it improbable that proper CPAP titration can be performed during a 2-3 hour nap study.

• The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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• v.18 no.1
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• pp.40-46
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• 2013

The isotope ratios of $^{13}C/^{12}C$ and $^{18}O/^{16}O$ for a sample in a mass spectrometer are measured relative to those of a pure $CO_2$ reference gas (i.e., laboratory working standard). Thus, the calibration of a laboratory working standard gas to the international isotope scales (Pee Dee Belemnite (PDB) for ${\delta}^{13}C$ and Vienna Standard Mean Ocean Water (V-SMOW) for ${\delta}^{18}O$) is essential for comparisons between data sets obtained by other groups on other mass spectrometers. However, one often finds difficulties in getting well-calibrated standard gases, because of their production time and high price. Additional difficulty is that fractionation processes can occur inside the gas cylinder most likely due to pressure drop in long-term use. Therefore, studies on laboratory production of pure $CO_2$ isotope standard gas from stable solid calcium carbonate standard materials, have been performed. For this study, we propose a method to extract pure $CO_2$ gas without isotope fractionation from a solid calcium carbonate material. The method is similar to that suggested by Coplen et al., (1983), but is better optimized particularly to make a large amount of pure $CO_2$ gas from calcium carbonate material. The $CaCO_3$ releases $CO_2$ in reaction with 100% pure phosphoric acid at $25^{\circ}C$ in a custom designed, evacuated reaction vessel. Here we introduce optimal procedure, reaction conditions, and samples/reactants size for calcium carbonate-phosphoric acid reaction and also provide the details for extracting, purifying and collecting $CO_2$ gas out of the reaction vessel. The measurements for ${\delta}^{18}O$ and ${\delta}^{13}C$ of $CO_2$ were performed at Seoul National University using a stable isotope ratio mass spectrometer (VG Isotech, SIRA Series II) operated in dual-inlet mode. The entire analysis precisions for ${\delta}^{18}O$ and ${\delta}^{13}C$ were evaluated based on the standard deviations of multiple measurements on 15 separate samples of purified $CO_2$. The pure $CO_2$ samples were taken from 100-mg aliquots of a solid calcium carbonate (Solenhofen-ori $CaCO_3$) during 8-day experimental period. The multiple measurements yielded the $1{\sigma}$ precisions of ${\pm}0.01$‰ for ${\delta}^{13}C$ and ${\pm}0.05$‰ for ${\delta}^{18}O$, comparable to the internal instrumental precisions of SIRA. Therefore, we conclude the method proposed in this study can serve as a way to produce an accurate secondary and/or laboratory $CO_2$ standard gas. We hope this study helps resolve difficulties in placing a laboratory working standard onto the international isotope scales and does make accurate comparisons with other data sets from other groups.

• Analytical Science and Technology
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• v.31 no.4
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• pp.161-170
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• 2018

The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

• Progress in Medical Physics
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• v.9 no.3
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• pp.155-162
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• 1998

Ho-l66 was produced by neutron reaction in a reactor at the Korea Atomic Energy Institute (Taejon, Korea). Ho-l66 emits a high energy beta particles with a maximum energy of 1.85 MeV and small proportion of gamma rays (80 keV). Therefore, the radiation absorbed dose estimation could be based on the in-vivo quantification of the activity in tumors from the gamma camera images. Approximately 1 mCi of Ho-l66 in solution was mixed into the flood phantom and planar scintigraphic images were acquired with and without patient interposed between the phantom and scintillation camera. Transmission factor over an area of interest was calculated from the ratio of counts in selected regions of the two images described above. A dual-head gamma camera(Multispect2, Siemens, Hoffman Estates, IL, USA) equipped with medium energy collimators was utilized for imaging(80 keV${\pm}$10%). Fifty-nine year old female patient with hepatoma was enrolled into the therapeutic protocol after the informed consent obtained. Thirty millicuries(110MBq) of Ho-166-CHICO was injected into the right hepatic arterial branch supplying hepatoma. When the injection was completed, anterior and posterior scintigraphic views of the chest and pelvic regions were obtained for 3 successive days. Regions of interest (ROIs) were drawn over the organs in both the anterior and posterior views. The activity in those ROIs was estimated from geometric mean, calibration factor and transmission factors. Absorbed dose was calculated using the Marinelli formula and Medical Internal Radiation Dose (MIRD) schema. Tumor dose of the patient treated with 1110 MBq(30 mCi) Ho-l66 was calculated to be 179.7 Gy. Dose distribution to normal liver, spleen, lung and bone was 9.1, 10.3, 3.9, 5.0 % of the tumor dose respectively. In conclusion, tumor dose and absorbed dose to surrounding structures were calculated by daily external imaging after the Ho-l66 therapy for hepatoma. In order to limit the thresholding dose to each surrounding organ, absorbed dose calculation provides useful information.

• Analytical Science and Technology
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• v.24 no.5
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• pp.345-351
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• 2011

A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed and validated for the determination of finasteride in human serum. Beclomethasone was used as internal standard (IS) and liquid-liquid extraction (LLE) using methyl tert-butyl ether (MTBE) was carried out to isolate analyte. The mass transitions monitored in multiple reaction monitoring (MRM) in positive ion mode were m/z 373.2${\rightarrow}$305.2 for finasteride and m/z 409.3${\rightarrow}$391.2 for IS. Retention times of finasteride and IS were 5.81 and 5.46 min, respectively. The limit of quantitation (LOQ) was 0.1 ng/mL and the calibration curve showed good linearity in the range of 0.1~20.0 ng/mL ($R^2$=0.9997). The intra-day assay precision and accuracy were in the range 6.3~10.6% and 97.3~103.6%, respectively, and the inter-day assay precision and accuracy were in the range 0.8~5.2% and 99.8~102.5%, respectively. The sample extract recovery of the method was 80~83%.

• Analytical Science and Technology
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• v.25 no.1
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• pp.76-82
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• 2012

The determination and confirmation of dutasteride in human serum was performed by a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Beclomethasone as an internal standard (I.S.) was added to the serum and the mixed sample was pretreated by liquid-liquid extraction (LLE) with methyl tert-butyl ether (MTBE). The mass transitions of dutasteride and I.S. monitored in multiple reaction monitoring (MRM) were m/z 529.6${\rightarrow}$461.5 and m/z 409.3${\rightarrow}$391.2, respectively, and the retention times were 6.45 and 5.46 min, respectively. The calibration curve was linear in the concentration range of 0.5~30.0 ng/mL ($R^2$= 0.9999) and the limit of quantitation (LOQ) was found to be 0.5 ng/mL. The recovery of dutasteride was shown to be 66~72%. The intra-day assay precision and accuracy were in the range 3.5~5.5% and 85.7~89.9%, respectively, and the interday assay precision and accuracy were in the range 4.2~5.8% and 90.8~95.8%, respectively.

• Analytical Science and Technology
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• v.23 no.6
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• pp.531-536
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• 2010

A quantitative analytical method has been established for the measurement of inosine 5'-monophosphate dehydrogenase (IMPDH) activity in human peripheral blood mononuclear cells (PBMCs) by ion-pair reversed-phase high performance liquid chromatography equipped with ultraviolet detection (HPLC/UV). IMPDH is a ${\beta}$-nicotinamide adenine dinucleotide hydrate (NAD+)-dependent dehydrogenase in which the enzyme converts inosine 5'-monophosphate (IMP) into xanthosine 5'-monophosphate (XMP). Its activity was measured by quantifying a HPLC chromatogram corresponding to XMP produced during the incubation of lysed PBMCs with IMP as a substrate and $NAD^+$ as a coenzyme. XMP produced was detected at a wavelength of 260 nm. The mobile phase was composed of a mixture of 37 mM potassium dihydrogen phosphate containing 7 mM tetra-n-butylammonium hydrogen sulfate adjusted to pH 5.5 and methanol (85:15, v/v) with a flow rate of 1 mL/min. The calibration curve was linear ($r^2$=0.999999) in the range of $0.2-50.0\;{\mu}M$ and the limit of quantification (LOQ) was $0.2\;{\mu}M$. The intra- and inter-day precisions were between 0.88-1.47% and 0.85-5.24%, respectively. The intra- and inter-day accuracies were between 98.74-99.99% and 99.95-101.65%, respectively. IMPDH activity in 11 Korean healthy volunteers ranged from 18.29 to 36.60 nmol/h/mg protein (mean = $27.70{\pm}6.28\;nmol/h/mg$ protein).

• Korean Journal of Environmental Agriculture
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• v.34 no.4
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• pp.274-281
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• 2015

BACKGROUND: A lasting release of low levels of persistence chemicals including pesticides and pharmaceuticals into river has a bad influence on aquatic ecosystems and humans. The present study monitored pesticide residues in the Yeongsan and Seomjin river basins and their tributaries as a fundamental study for water quality standard of pesticides.METHODS AND RESULTS: Nine pesticides(aldicarb, carbaryl, carbofuran, chlorpyrifos, 2,4-D, MCPA, methomyl, metolachlor, and molinate) were determined from water samples using SPE-Oasis HLB(pH 2) and LC/MS/MS. Validation of the method was conducted through matrix-matched internal calibration curve, method detection limit(MDL), limit of quantification(LOQ), accuracy, precision, and recovery. MDLs of all pesticides satisfied the GV/10 values. Linearity(r²) was 0.9965- 0.9999, and a percentage of accuracy, precision, and recovery was 89.4-113.6%, 3.1-14.0%, and 90.8-106.2%, respectively. All pesticides exclusive of aldicarb were determined in the river samples, and there was a connection between the positive monitoring results and agricultural use of the pesticides.CONCLUSION: Monitoring outcomes of the present study implied that pesticides were a possible non-point pollutant source in the Yeongsan and Seomjin river basins and tributaries. Therefore, it is required to produce and accumulate more monitoring results on pesticides in river waters to set water quality standards, finally to preserve aquatic ecosystems.

• Journal of Wetlands Research
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• v.17 no.2
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• pp.193-202
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• 2015

In this study, a long term monitering of nonpoint source pollution runoff is conducted at the area of transportation related and EMCs(Event Mean Concentrations) in terms of water quality items, such as BOD, $COD_{Mn}$, SS, T-N and T-P are determined for each not only runoff event and but also observation site. On the other hands, SWMM(Storm Water Management Model) model is constructed using the data collected in the transportation areas selected. Model calibration and verification of SWMM is carried out based on the data collected. And simulated EMCs was compared with observed EMCs by monitoring and prior studies. SWMM applicability estimation was Using the compared result. The results of simulation showed that BOD 5.787 ~ 14.475 mg/L, $COD_{Mn}$ 12.946 ~ 59.611 mg/L, SS 13.742 ~ 46.208 mg/L, T-N 2.037 ~ 5.213 mg/L, T-P 0.117 ~ 0.415 mg/L. And a differential between simulated EMCs and observed EMCs is too low so comparing result show high fit(BOD 4.27 %, $COD_{Mn}$ 4.87%, SS 2.31%, T-N 5.78%, T-P 14.45%). A results of compared with the prior studies, BOD and T-P are included range of prior studies, $COD_{Mn}$ and SS are lower than range of prior studies, T-N is higher than range of prior studies. Differential between simulated EMCs and prior studies EMCs was showing for survey seasonal and changing land-use, so from now on, EMCs of using the internal representatives value will be calculated by more monitoring toward various precipitation events.