• Mass Spectrometry Letters
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• v.9 no.4
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• pp.95-99
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• 2018

An innovative, simple, and rapid assay method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed and validated for the simultaneous determination of eight statin drugs in human urine. A simple sample clean-up procedure using the "dilute and shoot" (DAS) approach enabled a fast and reliable analysis. The influence of the dilution factor was investigated to ensure detectability and reduce the matrix effect. Chromatographic separation was performed on a Phenomenex Kinetex C18 column ($50{\times}3.0mm$ i.d., $2.6{\mu}m$) using an elution gradient of mobile phase A composed of 0.1% acetic acid, and mobile phase B composed of acetonitrile, at a flow rate of 0.35 mL/min. Quantitation was performed on a triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode using electrospray ionization in positive ion mode. The total chromatographic run time was 15 min. The method was validated for selectivity, sensitivity, recovery, linearity, accuracy, precision, and stability. The present method was successfully applied to the analysis of Rosuvastatin in urine samples after oral administration to healthy human subjects.

• Mass Spectrometry Letters
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• v.11 no.4
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• pp.82-89
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• 2020

A systematic isolation and characterization study for Cassia auriculata (CA) seeds resulted in identifying antidiabetic compounds 1,3,8-trihydroxyanthraquinone and quercetin, quercetin-3-O-rutinoside, gallic acid, caffeic acid, ferulic acid, and ellagic acid. The ultra-high-performance liquid chromatography based triple quadrupole mass spectrometry methodology was developed and validated for simultaneous identification and confirmation of these compounds from CA seeds. Multiple reaction monitoring (MRM) based quantification method was developed with MRM optimizer software for MS1 and MS2 mass analysis. The method was optimized on precursor ions and product ions with the ion ratio of each compound. The calibration curves of seven bioactive analytes showed excellent linearity (r2 ≥ 0.99). The quantitation results found precise (RSD, < 10 %) with good recoveries (84.58 to 101.42%). The matrix effect and extraction recoveries were found within the range (91.66 to 102.11%) for the CA seeds. This is the first MS/MS-based methodology applied to quantifying seven antidiabetic compounds in CA seeds and its extract for quality control purposes.

• Journal of Korea Society of Industrial Information Systems
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• v.14 no.5
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• pp.131-137
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• 2009

Ionizer is used in removal of static-electricity charge from several production processes such as flat panel display, organic EL, etc. In this paper, we introduce remote monitoring systems for ionizer which have been built to communicate with multiple ionizer and to control the power and ionizing state independently. Based on a series of tests, we verified the key functions of this controller such as unit connection, quantity of ion and electric charge, alarm, and successful communication between PC and controller. This system may be directly applicable to monitor systems for ionizer in the manufacturing processes of TFT-LCD, PDP, organic EL, and others.

• The Journal of the Petrological Society of Korea
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• v.10 no.3
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• pp.148-156
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• 2001

We report $^{230}Th/^{234}U$ disequilibrium ages of fracture-filling carbonate veins from the Ipsil and Janghangri fault zones, Gyeongju, Korea by multiple collector inductively coupled plasma mass spectrometry. The U and Th fraction was extracted from totally dissolved samples by rapid and convenient coprecipitation and ion exchange chemistry. The recovery was around 80% for Th and 70% for U. The $^{234}U/^{238}U,\;^{230}Th/^{232}Th$ ratios were analysed for this preconcentrated fraction and the U/Th ratio was directly analysed for untreated sample solution. The $^{234}U-^{230}Th$ system is in secular equilibrium for the Ipsil carbonate samples, supporting previously reported ESR ages. The detrital-corrected $^{230}Th/^{234}U$ age of the Janghangri carbonate samples is $48\pm$41 ka, which constrains the minimum age of the fracture zone.

• Journal of Chest Surgery
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• v.30 no.8
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• pp.786-792
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• 1997

A clinical study of 71 cases of pulmonary tuberculosis that had had surgical resection during the period of 7 years and 6months from January 1989 to June 1996 in National Masan Tuberculosis Hospital. The results were as follows. 1. The ratio of male to female was 3.7:1 and in the age incidence the fourth decade was 22%, the third decade 15%. Although medical treatment was performed for more than 3 to 6 months, preoHeratively the conversion failure rate of positive sputum to negative state was 66.2%(47 cases). Of the failure cases, multiple-drug-resistant(MDR) patients were 41 cases(87.2%), 3. In MDR group, preoperatively conversion failure rate was 71.9%. 4. From the view of indica ion for lung resection on the radiographic finding, cavitary lesions were 43 cases(60.6%), destroyed lung lesions were 24 cases(33.8%). 5. The incidence of postoperative complication was 28.2%(20 cases). All cases were MDR 6. group and the most common of complication was tuberculosis spreading. In bilateral lesion, incidence of postoperative tuberculosis spreading was 25%(7 cases). Of the 7 cases, there was the cavitary lesion in 6 cases(86.7%). Total conversion rate of AFB positive sputum to negative state related to resectional sugery was 76.6% and in MDR group conversion rate of AFB positive sputum to negative state was 73.2% Conversion rate of MDR group with bilateral lesion was the lowest(60%). Conversion rate of drug-sensitivity group was 100% regardeless of lesions Slt to. In conclusion, despite of long-standing medical treatment, it is difficult to converse sputum-positive to negative state in multiple-drug resistance patients and that increases postoperative complications su h as tuberculosis relapse as a lack of appropriate drugs postoperatively. Postoperative conversion rate of sputum-positive to negative state was decreased in multiple-drug resistance patients. Because multiple-drug resistance patients have inireased due to several factors in Korea, it is important to prevent spreading of multiple-drug resistnce patients through the aggressive operative treatment. When the first medical therapy is fail or drug-resistance is found, operative treatment should be considered with the secondary medical therapy. The operation should be aggressively attempted even though at first medical treatment if indicated.

• Journal of the Korean Chemical Society
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• v.40 no.8
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• pp.542-548
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• 1996

Electrodes modified with threonine, methionine and serine as ligands, which are incorporated by ion exchange into a polycationic film of electropolymerized $[Ru(v-bpy)_3]^{2+}$, have been employed in the determination of mercury in solution. The redox response of the surface-immobilized mercury/ligand complex was used as the analytical signal. When the polymeric film was electropolymerized, the supporting electrolytes were TBAP and $KPF_6$ to compare the morphology and anodic stripping of resulted polymer electrodes. At the case of the latter, the film had high porosity to give an easy incorporation of dopant anions into polymeric film matrix and a high sensitivity in determination of mercury ion. Especially, this polymer modified electrode exhibited possibility of multiple use in mercury determination over ten times. In all cases, calibration curves which were plotted by log of the surface coverage-normalized redox response vs. log[Hg] exhibited an excellent correlation (r=0.99) for mercury concentrations ranging from 1.0{\times}10^{-8}{\sim}1.0{\times}10^{-2}M$. At these curves relative standard deviation was 5∼8% and saturation response was not observed at high concentration region. Serine of the employed ligands had the best sensitivity in analytical application, which had greater stability constant in forming a complex with mercury than others as $pK_{Hg}=8.54$. The formation constants of threonine and methionine were respectively 7.04 and 7.80.

• Mass Spectrometry Letters
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• v.5 no.2
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• pp.42-48
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• 2014

A specific and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method (LC-ESI-MS/MS) was developed and validated for the simultaneous quantification of porphyrins (coproporphyrin, pentacarboxylporphyrin, hexacarboxylporphyrin, heptacarboxylporphyrin, and uroporphyrin) in human plasma and urine. Acidified plasma samples and urine samples were prepared by using liquid-liquid extraction using ethyl acetate and protein precipitation with acetonitrile, respectively. The separation was achieved onto a Synergi Fusion RP column ($150mm{\times}2.0mm$, $4{\mu}m$) with a gradient elution of mobile phase A (0.1% formic acid in 2 mmol/L ammonium acetate, v/v) and mobile phase B (20% methanol in acetonitrile, v/v) at a flow rate of $450{\mu}L$/min. Porphyrins and the internal standard (IS), coproporphyrin I-$^{15}N_4$, were detected by a tandem mass spectrometer equipped with an electrospray ion source operating in positive ion mode. Multiple reaction monitoring (MRM) transitions of the protonated precursor ions and the related product ions were optimized to increase selectivity and sensitivity. The proposed method was validated by assessing selectivity, linearity, limit of quantification (LOQ), precision, accuracy, recovery, and stability. The calibration curves were obtained in the range of 0.1-100 nmol/L and the LOQs were estimated as 0.1 nmol/L for all porphyrins. Results obtained from the validation study of porphyrins showed good accuracy, precision, recovery, and stability. Finally, the proposed method was successfully applied to clinical studies on the autism spectrum disorder (ASD) diagnosis of 203 Korean children.

• Restorative Dentistry and Endodontics
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• v.21 no.1
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• pp.321-338
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• 1996

The purpose of this study was to evaluate the effect of moistening and air-drying of acid conditioned dentin and enamel on the marginal microleakage. In this study, Class V cavity were prepared on both buccal and lingual surface of sixty extracted human premolars with cementum margin. These specimens were randomly devided into three groups and three dentin adhesives(Scotchbond Multi-Purpose, All bond 2, Prisma Universal Bond 3) were applied to each group. The specimens in each group were subdevided into four groups (Wet/primed, Dry/primed, Wet/not primed, Dry/not primed) and the etched dentin and enamel surface were treated these four surface treatments prior to the placement of a bonding agent or adhesive. Wet/primed group was simply blot-dried with a damp facial tissue before primer placement ; Dry/primed group was air dried for 30 seconds before the placement of a primer ; Wet/not primed group and Dry/not primed group were not primed after blot dried and air dried for 30 seconds each group. The bonding agent and composite resin were applied for each group. All specimens were exposed to 500 cycle of thermal stress. Specimens were placed in a silver nitrate solution and then sectioned buccolingually through the center of the restoration. The dye penetrations of the specimens were observed with a stereo microscope. The statistical test were applied to the results using a one way analysis variance (ANOVA) and Duncan's multiple range test. The aspects of silver ion penetration into the resin/dentin interface were examined under scanning electron microscopy. The results were as follows. 1. In all groups, the enamel margin showed significantly lower leakage value than the cementum margin (p<0.05). 2. Regardless of various surface treatment and dentin adhesives, there was no significant difference at the enamel margins (p>0.05). 3. At the dentin margins, the leakage values of Dry/not primed group showed significantly higher than that of the other groups (p<0.05). The leakage values of Wet/primed group showed significantly lower than that of the other groups, but, there was no significant difference between Wet group and Dry group. 4. There was no significantly difference between the dentin adhesives regarding the surface treatments in all groups(p>0.05). 5. On the backscatterd scanning electron microscopy observation, the penetration of the silver ion occured at the bonding resin/dentin interface. In the Wet/primed group, resindentin hybrid zone and resin penetration into the dentin was observed. The resin tags were compactively formed to a thickness of $3\sim4{\mu}m$ at the upper part of dentinal tubules. In the Dry/primed group, the thickness of the hybrid zone and the diameter, depth of the resin tags diminished. In the Non-primed groups, the hybrid zone was not identified and few resin tag was observed. There was the gap formation in the resin/dentin interface.

• Journal of Food Hygiene and Safety
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• v.32 no.3
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• pp.193-198
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• 2017

Scutellaria baicalensis, Eleutherococcus senticosus, and Angelica sinensis have been used as raw materials for health functional foods. This study was conducted to develop a novel method to analyze levels of baicalin (Scutellaria baicalensis), eleutheroside E (Eleutherococcus senticosus), and ligustilide (Angelica sinensis) simultaneously in health functional foods. The methanol extracted samples were analyzed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode and the negative ion mode using multiple reaction monitoring. Standard calibration curves confirmed linearity with the correlation coefficient ($r^2$) of > 0.99 at $100-2000{\mu}g/mL$ concentration range. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of $13.0{\sim}35.2{\mu}g/L$ and $39.3{\sim}106.7{\mu}g/L$, respectively. The recovery results ranged between 91.4~109.9% at 3 different concentration levels with relative standard deviations (RSDs) less than 5%. The proposed analytical method was characterized with high accuracy and acceptable precision. The new method would be an effective tool to analyze baicalin, eleutheroside E, and ligustilide simultaneously in raw materials of health functional foods.

• Asian Journal of Atmospheric Environment
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• v.6 no.1
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• pp.53-66
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• 2012

A comparison of analytical approaches for Levoglucosan ($C_6H_{10}O_5$, commonly formed from the pyrolysis of carbohydrates such as cellulose) and used for a molecular marker in biomass burning is made between the four different analytical systems. 1) Spectrothermography technique as the evaluation of thermograms of carbon using Elemental Carbon & Organic Carbon Analyzer, 2) mass spectrometry technique using Gas Chromatography/mass spectrometer (GC/MS), 3) Aerosol Mass Spectrometer (AMS) for the identification of the particle size distribution and chemical composition, and 4) two dimensional Gas Chromatography with Time of Flight mass spectrometry (GC${\times}$GC-TOFMS) for defining the signature of Levoglucosan in terms of chemical analytical process. First, a Spectrothermography, which is defined as the graphical representation of the carbon, can be measured as a function of temperature during the thermal separation process and spectrothermographic analysis. GC/MS can detect mass fragment ions of Levoglucosan characterized by its base peak at m/z 60, 73 in mass fragment-grams by methylation and m/z 217, 204 by trimethylsilylderivatives (TMS-derivatives). AMS can be used to analyze the base peak at m/z 60.021, 73.029 in mass fragment-grams with a multiple-peak Gaussian curve fit algorithm. In the analysis of TMS derivatives by GC${\times}$GC-TOFMS, it can detect m/z 73 as the base ion for the identification of Levoglucosan. It can also observe m/z 217 and 204 with existence of m/z 333. Although the ratios of m/z 217 and m/z 204 to the base ion (m/z 73) in the mass spectrum of GC${\times}$GC-TOFMS lower than those of GC/MS, Levoglucosan can be separated and characterized from D (-) +Ribose in the mixture of sugar compounds. At last, the environmental significance of Levoglucosan will be discussed with respect to the health effect to offer important opportunities for clinical and potential epidemiological research for reducing incidence of cardiovascular and respiratory diseases.