• Archives of Pharmacal Research
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• v.22 no.2
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• pp.189-193
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• 1999

Reversed-phase high-performance liquid chromatography/mass spectrometry (HPLC/MS) with an eletcrospray ionization (ESI) interface was applied to the identification of metabolites of IY81149 in the rat plasma. Fragments obtained using collision-induced dissociation (CID) in both positive and negative modes were utilized to elucidate the structure of metabolites. The eluent from the conventional HPLC column was split and directly introduced into an ESI-mass spectrometer for the identification of the structures. the CID technique allowed the sensitive identification of sulfonyl-IY81149 and hydroxy-IY81149 from the rat plasma.

• Journal of Korean Critical Care Nursing
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• v.5 no.2
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• pp.61-71
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• 2012

Purpose: The aim of this study was to measure the inter-rater reliability of Emergency severity index (ESI) version 4 among triage nurse. Methods: This study was carried out from August 11, 2010 to September 7, 2010 in a regional emergency department. Data collection was done by ten triage nurses who trained ESI v.4. Two research nurses and ten triage nurses scored the ESI version 4 to the patients as references, independently. We calculated the weighted kappa between the triage nurses and research nurses to evaluate the consistency of the ESI v.4. Results: A total of 233 patients were enrolled in this study. Classification of ESI level was as follows - level 1 (0.4%), level 2 (21.0%), level 3 (67.8%), level 4 (9.4%), and level 5 (1.3%). Inter-rater reliability by weighted kappa was 0.79 (95% Confidence Interval= 0.74-0.83) and agreement rate was 87.1%. Under-triage rate by triage nurse was 6.0% and over-triage rate was 6.9%. Conclusion: For this study, inter-rater reliability was measured good level between triage nurses and research nurses in Korean single ED.

• The Korean Journal of Pain
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• v.31 no.2
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• pp.87-92
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• 2018

Background: An epidural steroid injection (ESI) is a commonly administered procedure in pain clinics. An unintentional lumbar facet joint injection during interlaminar ESI was reported in a previous study, but there has not been much research on the characteristics of an unintentional lumbar facet joint injection. This study illustrated the imaging features of an unintentional lumbar facet joint injection during an interlaminar ESI and analyzed characteristics of patients who underwent this injection. Methods: From December 2015 to May 2017, we performed 662 lumbar ESIs and we identified 24 cases (21 patients) that underwent a lumbar facet joint injection. We gathered data contrast pattern, needle approach levels and directions, injected facet joint levels and directions, presence of lumbar spine disease as seen on magnetic resonance images (MRI), and histories of lumbar spine surgeries. Results: The contrast pattern in the facet joint has a sigmoid or ovoid contrast pattern confined to the vicinity of the facet joint. The incidence of unintentional lumbar facet joint injection was 3.6%. The mean age was 68.47 years. Among these 21 patients, 14 (66.7%) were injected in the facet joint ipsilaterally to the needle approach. Among the 20 patients who received MRI, all (100%) had central stenosis and 15 patients (75%) had severe stenosis. Conclusions: When the operator performs an interlaminar ESI on patients with central spinal stenosis, the contrast pattern on the fluoroscopy during interlaminar ESI should be carefully examined to distinguish between the epidural space and facet joint.

• Bulletin of the Korean Chemical Society
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• v.28 no.7
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• pp.1187-1194
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• 2007

The three major active isoflavonoids (calycosin-7-O-β -glucoside, isomucronulatol 7-O-β-glucoside, formononetin) and two main saponins (astragaloside I, astragaloside IV) in an extract of Radix Astragali were determined using rapid, sensitive, reliable HPLC/UV and LC-ESI-MS/MS methods. The separation conditions employed for HPLC/UV were optimized using a phenyl-hexyl column (4.6 × 150 mm, 5 μm) with the gradient elution of acetonitrile and water as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm. The specificity of the peaks was determined using a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization (ESI) source that was operated in multiple reaction monitoring (MRM) in the positive mode. These methods were fully validated with respect to the linearity, accuracy, precision, recovery and robustness. The HPLC/UV method was applied successfully to the quantification of three major isoflavonoids in the extract of Radix Astragali. The results indicate that the established HPLC/UV and LC-ESI-MS/MS methods are suitable for the quantitative analysis and quality control of multi-components in Radix Astragali.

• Analytical Science and Technology
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• v.23 no.5
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• pp.457-464
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• 2010

The analytical method of four pharmaceuticals (virginiamycin, erythromycin, tylosin and cimetidine) in drinking water was developed. Effective simultaneous sample clean-up and extraction by solid-phase extraction (SPE) using HLB cartridge prior to LC/ESI-MS/MS analysis were performed. A linear correlation observed in the calibration curves for drinking water in the range of 0.01~2.0 ng/mL showed above $r^2$=0.995. Absolute recovery was in the range of 64.7~118.1% (except cimetidine (37.7~48.1%)). Limit of detection (LOD) and limit of quantitation (LOQ) in spiked drinking water matrix were in the range of 1.6~74.8 pg/mL and 5.5~249.7 pg/mL, respectively. The established method can be used to determine low pg/mL levels of pharmaceuticals in the drinking water.

• Korean Journal of Pharmacognosy
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• v.49 no.3
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• pp.270-277
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• 2018

Pyungwi-san has been used to treat the digestive system diseases, physconia, nausea, anorexia, and dyspepsia in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was optimized for simultaneous determination of the 14 marker components, spinosin, liquiritirn apioside, liquiritin, narirutin, 6'''-feruloylspinosin, hesperidin, liquiritigenin, glycyrrhizin, 6-gingerol, atractylenolide III, honokiol, atractylenolide II, magnolol, and atractylenolide I in Pyungwi-san extract. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) with maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid and acetonitrile. The MS conditions were as follows: capillary voltage 3.3 kV, extractor voltage 3.0 V, RF lens voltage 0.3 V, source temperature $120^{\circ}C$, desolvation temperature $300^{\circ}C$, desolvation gas 600 L/h, cone gas 50 L/h and collision gas 0.14 mL/min. The coefficient of determination of 14 analytes was 0.9989-1.0000. The limits of detection and quantification values of the all analytes were 0.04-2.56 and 0.13-7.69 ng/mL, respectively. As a result of the analysis using the established LC-ESI-MS/MS method, the 5 components, spinosin, 6'''-feruloylspinosin, atractylenolide III, II, and I derived from Zizyphi Fructus and Atractylodis Rhizoma, were not detected in this extract. On the other hand, the 9 components except for the 5 components were 4.15-498.87 mg/kg in lyophilized Pyungwi-san extract. Among these components, glycyrrhizin, marker compound of Glycyrrhizae Radix et Rhizoma, was detected the most amount as a 498.87 mg/kg.

• Analytical Science and Technology
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• v.23 no.6
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• pp.572-578
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• 2010

The extraction/clean-up and concentrating of pharmaceuticals from surface water were performed by HLB (Hydrophilic-Lipophilic Balanced) cartridge. The method allows for the simultaneous determination of six pharmaceuticals by HPLC/ESI(+)-MS/MS. Recoveries of the pharmaceutical were between 71.1 to 92.6% (except fenbendazole) and the overall variability of the method was below 11.2% (RSD). The calibration curves for the pharmaceuticals from blank surface water showed good linearities (above $r^2$ = 0.99) in the concentration range of 0.007~1.2 ng/mL. The limit of detection (LOD) and the limit of quantification (LOQ) were 7.2~128.7 pg/mL and 23.8~429.1 pg/mL, respectively. The present analytical method can be useful for monitoring residual pharmaceuticals in surface water and other aquatic samples. High concentrations of iopromide and fenbendazole were detected in a few samples of surface water.

• Journal of Life Science
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• v.21 no.3
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• pp.464-467
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• 2011

Quercetin is a major flavonoid present in onions, which acts as an antioxidant. Quercetin exists both as a free compound and conjugated with carbohydrates, primarily as glucosides in onion. Aged black onion was made through a 30 day aging process in which the onions were kept in an environment of $60^{\circ}C$ and high humidity (90% RH). Quercetin and quercetin glucosides were assayed in onion bulbs before and after the aging process, using high performance liquid chromatography-electrospray ion trap mass spectrometry (HPLC-ESI/MS/MS). Quercetin mono- and diglucosides were identified in fresh onion bulbs, whereas quercetin aglycone was the only form present in aged black onion bulbs. These findings indicate that the quercetin mono- and di-glucosides present in fresh onions undergo complete deglycosylation during the aging process. Such profiling will provide a rapid method that can be used to assess changes in the two major quercetin glycosides during the aging process of onion bulbs.

• Journal of the Korean Chemical Society
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• v.55 no.4
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• pp.626-632
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• 2011

Phoxim, which is one of veterinary drugs, is a well-known antiparasitic agent in wide use. In this paper, phoxim was extracted from cattle and pig tissue using solid-phase extraction (SPE) employing a silica cartridge with acetonitrile. Liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) for the analysis of phoxim from animal tissue was presented. Phoxim was detected on a $C_{18}$ column ($2.1{\times}100\;mm$, $3.5\;{\mu}m$) using a mobile phase of 0.1% formic acid in water and acetonitrile. A linear correlation observed in the calibration curves for cattle (0.0048~2.0 mg/kg) and pig (0.0055~2.0 mg/kg) showed above $r^2$=0.995. Accuracy measured at concentrations ranging from 0.0048 to 0.2 mg/kg was the range of 68.2~106.9%. Limit of detection (LOD) and limit of quantitation (LOQ) were the range of 0.0014~0.0017 mg/kg and 0.0048~0.0055 mg/kg, respectively. The precision (RSD%) was below 11.2%.

• 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.