• Journal of Biomedical and Translational Research
• /
• v.19 no.4
• /
• pp.130-139
• /
• 2018

This study aimed to analyze a high-performance liquid chromatography (HPLC) separation using a pentafluorophenyl column of parent drug hydroxychloroquine (HCQ) and its active metabolite, desethylhydroxchloroquine (DHCQ) applying to determine bioequivalence of two different formulations administered to patients. A rapid, simple, sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for bioanalysis of HCQ and its metabolite DHCQ in human whole blood using deuterium derivative $hydroxychloroquine-D_4$ as an internal standard (IS). A triple-quadrupole mass spectrometer was operated using electrospray ionization in multiple reaction monitoring (MRM) mode. Sample preparation involves a two-step precipitation of protein techniques. The removed protein blood samples were chromatographed on a pentafluorophenyl (PFP) column ($50mm{\times}4.6mm$, $2.6{\mu}m$) with a mobile phase (ammonium formate solution containing dilute formic acid) in an isocratic mode at a flow rate of 0.45 mL/min. The standard curves were found to be linear in the range of 2 - 500 ng/mL for HCQ; 2 - 2,000 ng/mL for DHCQ in spite of lacking a highly sensitive MS spectrometry system. Results of intra- and inter-day precision and accuracy were within acceptable limits. A run time of 2.2 min for HCQ and 2.03 min for DHCQ in blood sample facilitated the analysis of more than 300 human whole blood samples per day. Taken together, we concluded that the assay developed herein represents a highly qualified technology for the quantification of HCQ in human whole blood for a parallel design bioequivalence study in a healthy male.

• Mass Spectrometry Letters
• /
• v.12 no.1
• /
• pp.1-10
• /
• 2021

A simple, specific, and economical LC-MS/MS method was investigated for the screening of 43 prescribed antihypertensive and related drugs in human urine. The urine samples were simply prepared by diluting and mixing with internal standard before directly introduced to the LC-MS/MS system, which is fast, straightforward, and cost-effective. Fractional factorial, Box-Behnken, and I-optimal design were applied to screen and optimize the mass spectrometric and chromatographic factors. The analysis was carried out on a triple quadrupole mass spectrometer system utilizing multiple reaction monitoring with positive and negative electrospray ionization method. Chromatographic separation was performed on a Thermo Scientific Accucore RP-MS column (50 × 3.0 mm ID., 2.6 ㎛) using two separate gradient elution programs established with the same mobile phases. Chromatographic separation was performed within 12 min. The optimal method was validated based on FDA guideline. The results indicated that the assay was specific, reproducible, and sensitive with the limit of detection from 0.1 to 50.0 ㎍/L. The method was linear for all analytes with coefficient of determination ranging from 0.9870 to 0.9981. The intra-assay precision was from 1.44 to 19.87% and the inter-assay precision was between 2.69 and 18.54% with the recovery rate ranges from 84.54 to 119.78% for all drugs measured. All analytes in urine samples were stable for 24 h at 25℃, and for 2 weeks at -60℃. The developed method improves on currently existing methods by including larger number of cardiovascular medications and better sensitivity of 12 analytes.

• Korean Journal of Veterinary Service
• /
• v.45 no.3
• /
• pp.145-153
• /
• 2022

Pathogens such as feline herpesvirus, feline calicivirus, Bordetella bronchiseptica, Chlamydia felis, Mycoplasma felis and Pasteurella multocida usually cause feline upper respiratory tract disease (URTD). Real-time PCR was used to analyze the detection and prevalence of the most common respiratory pathogens in cats with (n=69) and without respiratory signs (n=31). Pathogens were detected in 53 cats, divided into 37 (69.8%) with a single pathogen, 15 (28.3%) with two pathogens, and 1 (1.9%) with three pathogens. M. felis had the highest detection rate in 29 (42.0%) cats, P. multocida was detected in 18 (26.1%), FHV in 10 (14.5%), FCV in 7 (10.1%), B. bronchiseptica in 3 (4.3%), and C. felis in 2 (2.9%). M. felis was the most frequently detected pathogen in cats living outdoors without vaccination. Of the 37 cats infected with single pathogen, nasal discharge was observed in 13 (35.1%), ocular signs in 6 (16.2%), drooling in 5 (13.5%), dyspnea in 3 (8.1%), and asymptomatic in 10 (27.0%). In 51 outdoor and 49 indoor cats, pathogens were detected in 35 (68.6%) and 18 (36.7%) cats, respectively. Of the 29 cats infected with M. felis, 22 (75.9%) showed respiratory signs, and 7 (24.1%) were healthy. In the age of the 53 positive cats, 10 (18.9%) were under the age of 1 year, 26 (49.1%) were aged 1~3 years, and 17 (32.1%) were aged 3 years or older. Although the number of cats in the study was small, the results can provide valuable data on the prevalence of URTD in Korean cats.

• Journal of the Korea Academia-Industrial cooperation Society
• /
• v.19 no.3
• /
• pp.112-118
• /
• 2018

In order to meet the strict emission regulations for internal combustion engines based on fossil fuel, the proportion of after-treatments for vehicles and vessels is gradually increasing. Diesel engines have high power, good fuel economy, and lower $CO_2$ emissions, and their market shares are increasing in commercial vehicles and passenger cars. However, NOx is generated in the localized high-temperature combustion regions, and particulate matter is formed in the zones of diffusion combustion. LNT and urea-SCR catalysts have been developed for after-treatment of the exhaust gas to reduce NOx in diesel vehicles. This study aims to improve the NOx reduction performance of Cu SCR catalyst, which is widely used in light, medium, and heavy-duty diesel engines. The de-NOx performance of $5Cu-2ZrO_2$/93Zeolyst(Si/Al=13.7) SCR catalyst was about 5-50% higher than that of $5Cu-2ZrO_2$/93Zeolite(Si/Al=2.9) at catalyst temperatures of $300^{\circ}C$ or higher. The zeolite had lower metal dispersion than zeolyst, and the reaction rate of the catalyst decreased as the average particle size increased. The $10Cu-2ZrO_2$/88Zeolyst catalyst loaded with 10wt% Cu had the highest NOx conversion rate of 40% at $200^{\circ}C$ and about 65% at $350^{\circ}C$. The ion exchange rate of Cu ions increased with that of Al, the crystalline compound of zeolite, and the de-NOx performance was improved by 20-40% compared to other catalysts.

• Applied Biological Chemistry
• /
• v.41 no.5
• /
• pp.372-376
• /
• 1998

Internal mass transfer during osmotic dehydration of gingers in sugar solution was examined as a function of concentration, temperature and immersion time of those solutions using moisture loss, sugar gain, molality and rate parameter. Influence of osmotic dehydration on browning reaction and texture properties of air dried rehydrated was also evaluated. Increasing the concentration and temperature of sugar solutions increased moisture loss, sugar gain, molality and rate parameter. Water loss and sugar gain were rapid in the first 3 min and then changed gentle slope. Moisture loss during osmotic dehydration using a sugar solution $(60\;Brix,\;80^{\circ}C)$ with 18 min immersion time was 40.05 g moisture/100 g wet ginger which was 52% reduction of initial moisture content in ginger (83.02%, wet basis). The changes of rate parameter were more affected by temperature than by concentration of sugar solution. Minimum browning degree (O.D.=0.027) was carried out by osmotic dehydration in sugar solution $(40\;or\;50\;Brix,\;80^{\circ}C)$ with 15 min immersion time compared to control (O.D.=0.132). Influence of osmotic dehydration on puncture forces of 3 min rehydrated ginger in boiling water were $22{\sim}34%$ of reduction, while blanching treatment had not affected compared to those of control.

• Tuberculosis and Respiratory Diseases
• /
• v.45 no.5
• /
• pp.935-941
• /
• 1998

Background: As living and dead Mycobacteria could be amplified by polymerase chain reaction(PCR), it was considered that PCR was inappropriate for the monitoring of pulmonary tuberculosis after treatment. But we found negative conversion of PCR after successful treatment. We would like to know about the negative conversion rate of PCR and its conversion time after antituberculous treatment. Methods: We collected 113 sputums from the 16 patients of pulmonary tuberculsosis visiting Catholic University Hospital of Taegu Hyosung. We consecutively tested AFB smear, AFB culture and PCR by 2 to 4 weeks after antituberculous therapy. The patients were classified according to the chest X ray findings. Results: We detected negative conversion of PCR from all 16 patients of the pulmonary tuberculosis within 30 weeks after treatment. The average negative conversion time was $16{\pm}8$ weeks. The conversion time according to the chest X -ray findings were as follows : For the 8 cases of minimum were $9{\pm}5$ weeks, 4 cases of modreate advanced were $20{\pm}8$ weeks, and 4 cases of far advanced were $23{\pm}2$ weeks. The product of PCR was gradually decreased according to the duration of treatment. Conclusions: From the results of our study, we could utilize M. tubercuosis PCR for the prediction of therapy response and monitoring of the patient with pulmonary tuberculosis after treatment.

• Analytical Science and Technology
• /
• v.28 no.6
• /
• pp.460-466
• /
• 2015

An isotope dilution liquid chromatography tandem mass spectrometry was developed as a primary method for the quantitative analysis of cholesterol in infant formula. Cholesterol-d₄ was used as an internal standard and spiked into the infant formula sample. In order to release cholesterol out of cholesteryl ester, which is cholesterol bound to fatty acids in infant formula, saponification was carried out. Saponification conditions were optimized with heating temperature, reaction time and the concentration of KOH. The optimum conditions were as follows; heating temperature was 70 ℃, reaction time was 180 min and the concentration of KOH was 0.8 mL of 8 M KOH for about 0.1 g infant formula sample. Extraction of cholesterol out of sample solution was carried out with hexane uisng liquid-liquid extraction. Chromatographic analysis was carried out using Phenomenex Kinetex C₁₈ column. Mobile phase was 0.1% acetic acid in methanol/water (v/v, 99/1) and flow rate was 0.3 mL/min. Cholesterol and cholesterol-d₄ were monitored at mass transfer m/z 369/259 and 373/263 respectively. Reproducibility of the method was evaluated to be 0.23% of the measurement result. The expanded uncertainty of the measurement result of cholesterol in infant formula was approximately 1.9% at a 95% confidence level. NIST standard reference material having certified values of cholesterol in infant formula, was analyzed in order to verify this method. The ID-LC/MS/MS results were well agreed with the certified values of NIST SRM within the uncertainty.

• Journal of the Korean Chemical Society
• /
• v.10 no.4
• /
• pp.166-174
• /
• 1966

The multistep mechanism of photosensitized curing reaction cinnamoylated photosensitive polymer is proposed from the energy level diagram of cinnamic acid and sensitizer, and from the fact that excess of sensitizer brings the sensitivity to a limiting value etc. Various factors which have effects on the ability of sensitizer are also discussed. The mechanism involves following steps: activation to the first excited singlet states of cinnamoyl group(C) and sensitizer(S) by their absorption of photon, their intersystem crossing to the lowest triplet state, bimolecular internal quenching by formation of excimer of sensitizer, triplet excitation energy transfer and intermolecular addition between cinnamoyl group in ground state and that in triplet state. The rate equation derived from this mechanism is $-\frac{d[C]}{dt} = \frac{K_1[C]}{K_2 + [C]}[\frac{I^c_{abs}}{K_3 + [S]} + \frac{K_4[C]}{(K_5 + [C])(K_6 + [S])}(I^s_{abs} + \frac{K_7I^c_{abs}[S]}{K_8 + [S]})]$ where $I^c_{abs}\;and\;I^s_{abs}$: the rates of absorption of photon by cinnamoyl group and sensitizer $K_n$: Constants. It is proved with the cinnamate of poly(glyceryl phthalate)(PGC) in the absence of sensitizer using the infrared analytical method and successfully applied for the experimental data reported on the effects of the degree of cinnamoyl esterification and the concentration of sensitizer upon the sensitivity.

• Asian Pacific Journal of Cancer Prevention
• /
• v.15 no.1
• /
• pp.321-326
• /
• 2014

Background: Mutations in the tyrosine kinase domain of the epidermal growth factor receptor (EGFR) in non-small cell lung cancer (NSCLC) are predictive of response to EGFR-targeted therapy in advanced stages of disease. This study aimed to determine the frequency of EGFR mutations in NSCLCs and to correlate their presence with clinical characteristics in multiethnic Malaysian patients. Materials and Methods: In this prospective study, EGFR mutations in exons 18, 19, 20 and 21 in formalin-fixed paraffin-embedded biopsy specimens of consecutive NSCLC patients were asessed by real-time polymerase chain reaction. Results: EGFR mutations were detected in NSCLCs from 55 (36.4%) of a total of 151 patients, being significantly more common in females (62.5%) than in males (17.2%) [odds ratio (OR), 8.00; 95% confidence interval (CI), 3.77-16.98; p<0.001] and in never smokers (62.5%) than in ever smokers (12.7%) (OR, 11.50; 95%CI, 5.08-26.03; p<0.001). Mutations were more common in adenocarcinoma (39.4%) compared to non-adenocarcinoma NSCLCs (15.8%) (p=0.072). The mutation rates in patients of different ethnicities were not significantly different (p=0.08). Never smoking status was the only clinical feature that independently predicted the presence of EGFR mutations (adjusted OR, 5.94; 95%CI, 1.94-18.17; p=0.002). Conclusions: In Malaysian patients with NSCLC, the EGFR mutation rate was similar to that in other Asian populations. EGFR mutations were significantly more common in female patients and in never smokers. Never smoking status was the only independent predictor for the presence of EGFR mutations.

• Asian Journal of Atmospheric Environment
• /
• v.6 no.4
• /
• pp.288-303
• /
• 2012

In this study, real time measurements of particle number size distribution in urban Gwangju, coastal Taean, and industrial Yeosu in Korea were conducted in 2008 to understand the occurrence of ultrafine particle (UFP) (<100 nm) events, the variation of its concentration among different sampling sites, and UFP formation pathways. Also, to investigate seasonal and long-term variation of the UFP number concentration, data were collected for the period of 5 years (2007, 2008, 2010, 2011, and 2012) in urban Gwangju. Photochemical and combustion events were found to be responsible for the formation of UFP in the urban Gwangju site, whereas only photochemical event led to the formation of UFP in the coastal Taean site. The highest UFP concentration was found in industrial Yeosu (the average UFP number fractions were 79, 59 and 58% in Yeosu, Gwangju, and Taean, respectively), suggesting that high amount of gas pollutants (e.g., $NO_2$, $SO_2$, and volatile organic carbon (VOC)) emitted from industries and their photochemical reaction contributed for the elevated UFP concentration in the industrial Yeosu site. The UFP fraction also showed a seasonal variation with the peak value in spring (61.5, 54.5, 50.5, and 40.7% in spring, fall, summer, and winter, respectively) at urban Gwangju. Annual average UFP number concentrations in urban Gwangju were $5.53{\times}10^3\;cm^{-3}$, $4.68{\times}10^3\;cm^{-3}$, $5.32{\times}10^3\;cm^{-3}$, $3.99{\times}10^3\;cm^{-3}$, and $2.16{\times}10^3\;cm^{-3}$ in the year 2007, 2008, 2010, 2011, and 2012, respectively. Comparison of the annual average UFP number concentration with urban sites in other countries showed that the UFP concentrations of the Korean sites were lower than those in other urban cities, probably due to lower source strength in the current site. TEM/EDS analysis for the size-selected UFPs showed that the UFPs were classified into various types having different chemical species. Carbonaceous particles were observed in both combustion (soot and organics) and photochemical events (sulfate and organics). In the photochemical event, an internal mixture of organic species and ammonium sulfate/bisulfate was identified. Also, internal mixtures of aged Na-rich and organic species, aged Ca-rich particles, and doughnut shaped K-containing particles with elemental composition of a strong C with minor O, S, and K-likely to be originated from biomass burning nearby agricultural area, were observed. In addition, fly ash particles were also observed in the combustion event, not in the photochemical event.