• YAKHAK HOEJI
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• v.60 no.2
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• pp.64-72
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• 2016

Jakyakgamcho-tang is a well-known traditional herbal medicine and has been used for the treatment of mainly pains in oriental medicine. In this study, analytical method for the quantitative determination of the eleven marker components, gallic acid (1), oxypaeoniflorin (2), paeoniflorin (3), albiflorin (4), liquiritin (5), isoliquiritin (6), ononin (7), liquiritigenin (8), benzoylpaeoniflorin (9), paeonol (10), and glycyrrhizin (11) in Jakyakgamcho-tang decoction was performed using an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer. The analytical column for separation of the compounds 1~11 was used an UPLC BEH $C_{18}$ ($100{\times}2.1mm$, $1.7{\mu}m$) column and column oven temperature was maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid (A) and acetonitrile (B) by gradient elution. The flow rate was 0.3 ml/min and injection volume was $2.0{\mu}l$. Correlation coefficient in the calibration curves of the compounds 1~11 were showed a good linearity with more than 0.99. The limit of detection and limit of quantification values of the compounds 1~13 were detected in the ranges 0.06~18.43 ng/ml and 0.18~58.29 ng/ml, respectively. Among the compounds 1~11, the compounds 10 were not detected in this sample, while the ten compounds, 1~9 and 11, were detected $44.05{\sim}19,289.05{\mu}g/g$ in Jakyakgamcho-tang extract.

• Korean Journal of Veterinary Research
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• v.63 no.3
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• pp.23.1-23.9
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• 2023

This study was conducted to investigate tiamulin (TML) residues in the edible tissues of orally dosed broiler chickens and to re-establish the withdrawal time (WT). Thirty-six healthy Ross broiler chickens were administered 0.5 (TML-1) and 2.5 kg (TML-2) per ton feed, respectively, of the drug containing TML 78 g/kg for 10 days. Twenty-four tissue samples were collected from 6 chickens in each of the TML-1 and TML-2 groups on 0, 1, 3, and 5 days after drug administration, respectively. The residual concentrations of TML were measured using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The correlation coefficient of the calibration curves was 0.9978 to 0.9998, and the limits of detection and the limits of quantification (LOQ) were in the range of 0.03 to 0.06, and 0.1 to 0.2 ㎍/kg, respectively. Recoveries ranged between 89.0% to 116.7%, and the coefficients of variation were less than 13.9%. After the drug administration, TML in the TML-1 and TML-2 groups was detected above the LOQ in 1 and 6 samples of liver, respectively, at day 0, and in 1 liver sample from both groups on day one. At 3 days after administration, TML was detected below the LOQ in all samples of TML-1 and TML-2. The calculated WT of TML in both TML-1 and TML-2 using the WT calculation program WT 1.4 was 0 days. In conclusion, the developed analytical method is suitable for detection, and the calculated WT of TML in poultry edible tissues is shorter than the current recommended WT of 7 days for TML in broiler chickens.

• Journal of the Korean Chemical Society
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• v.54 no.5
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• pp.523-532
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• 2010

The proposed method is simple, sensitive and specific Liquid chromatography-tandem mass spectrometry (LCESI-MS/MS) method for the quantification of Entacapone (EA) in human plasma using Entacapone-d10 (EAD10) as an internal standard (IS). Chromatographic separation was performed on Zorbax SB-C18, $2.1{\times}50\;mm$, $5\;{\mu}m$ column, mobile phase composed of 10 mM Ammonium formate (pH 3.0): Acetonitrile (60:40 v/v), with a flow-rate of 0.7 mL/min, followed by Liquid-liquid extraction. EA and EAD10 were detected with proton adducts at m/z $306.1{\rightarrow}233.1$ and $316.3{\rightarrow}233.0$ in multiple reaction monitoring (MRM) positive mode respectively. The method was validated over a linear concentration range of 1.00 - 2000.00 ng/mL with correlation coefficient ($r^2$) $\geq$ 0.9993. Intra and inter-day Precision within 3.60 to 7.30 and 4.20 to 5.50% and Accuracy within 97.30 to 104.20 and 98.30 to 105.80% proved for EA. This method is successfully applied in the bioequivalence study of healthy Indian human volunteers.

• Food Science and Biotechnology
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• v.18 no.4
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• pp.1001-1012
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• 2009

A total of 49 phenolic compounds were identified from the aged red wines made from Cabernet Gernischt (Vitis vinifera L. cv.) grapes, a Chinese characteristic variety, including 13 anthocyanins, 4 pryanocyanins, 4 flavan-3-ol monomers, 6 flavan-3-ol polymers, 7 flavonols, 6 hydroxybenzoic acids, 5 hydroxycinnamic acids, 3 stilbenes, and 1 polymeric pigment. Evolution of these compounds was investigated in wines aged 1 to 13 months. Variance analysis showed that the levels of most phenolics existed significant difference in between wines aged 3 and 9 months. Cluster analysis indicated that 2 groups could be distinguished, one corresponding to wines aged 1 to 3 months and the other to wines aged 4 to 13 months. It was thus suggested that there were 2 key-stages for the development of fine wine quality, at the aged 3 and 9 months, respectively. This work would provide some helpful information for quality control in wine production.

• YAKHAK HOEJI
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• v.59 no.2
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• pp.49-54
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• 2015

In the present study we evaluated comparative herb-drug interaction potential of red ginseng total powder, ginsenoside Rg1, and Rb1 by inhibition of CYP isoforms including CYP1A2, CYP2A6, CYP2B6, CYP2C9, CYP2C19, CYP2D6, CYP2E1 and CYP3A4 using pooled human liver microsomes (HLMs). As measured by liquid chromatography-electrospray ionization tandem mass spectrometry, red ginseng total powder inhibited significantly activities of CYP1A2, CYP2A6, CYP2B6, CYP2C9, CYP2C19, CYP2D6, CYP2E1 and testosterone 6-beta hydroxylation by CYP3A4, but the $IC_{50}$ values were higher than $556{\mu}g/ml$. Activities of CYP2B6, CYP2C9, CYP2D6 and CYP3A4 were inhibited by ginsenoside Rb1. Also, activities of CYP1A2, CYP2A6, CYP2B6, CYP2C9, CYP2C19, CYP2D6 and testosterone 6-beta hydroxylation by CYP3A4 were inhibited by ginsenoside Rg1. The $IC_{50}$ values of ginsenoside Rb1 and Rg1 were higher than $200{\mu}g/ml$. Based on $IC_{50}$ values against CYP isoforms, ginsenosides-drug interactions by CYP inhibition may be very low in clinical situations.

• Journal of Microbiology and Biotechnology
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• v.29 no.11
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• pp.1806-1816
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• 2019

Candida albicans is an opportunistic fungus possessing multiple virulence factors controlling pathogenicity. Cell wall proteins are the most important among these factors, being the first elements contacting the host. Ddr48 is a cell wall protein consisting of 212 amino acids. A DDR48 haploinsufficient mutant strain was previously found necessary for proper oxidative stress response and drug resistance. In this study, we aimed to further elucidate the role of Ddr48 by performing additional phenotypic characterization assays. A combinatory proteomic and bioinformatics approach was also undertaken to determine differentially expressed cell wall proteins. Results showed that the mutant strain exhibited a 10% decrease in adhesion mirrored by a 20% decrease in biofilm formation, and slight sensitivity to menadione, diamide, and SDS. Both strains showed similar hyphae formation, virulence, temperature tolerance, and calcofluor white and Congo red sensitivities. Furthermore, a total of 8 and 10 proteins were identified exclusively in the wild-type strain grown under filamentous and non-filamentous conditions respectively. Results included proteins responsible for superoxide stress resistance (Sod4 and Sod6), adhesion (Als3, Hyr4, Pmt1, and Utr2), biofilm formation (Hsp90, Ece1, Rim9, Ipp1, and Pra1) and cell wall integrity (Utr2 and Pga4). The lack of detection of these proteins in the mutant strain correlates with the observed phenotypes.

• Analytical Science and Technology
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• v.29 no.4
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• pp.155-161
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• 2016

Distribution of various illegal or counterfeit drugs of seven approved erectile dysfunction drugs and their analogues has been increased, causing health problems such as cardiovascular disorder, tachycardia, headache, or vision disturbance. We used liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) to determine the erectile dysfunction drugs and their analogues in various counterfeit drugs. Eleven erectile dysfunction drugs and their analogues were detected, with sildenafil and its analogues being the most counterfeited compounds (73.8 %), followed by tadalafil and its analogues (25.4 %). The limits of detection (LOD) and the limits of quantitation (LOQ) of liquid-type and solid-type negative samples ranged from 0.1 to 3.3 ng/mL or ng/g and from 0.3 to 10.0 ng/mL or ng/g, respectively. The recoveries ranged from 84.3 to 112.3 % and 83.2 to 110.2 %, respectively. The contents of sildenafil and tadalafil in the various counterfeit drugs ranged from 21.0 to 947.5 mg/g and from 0.2 to 170.2 mg/g, respectively.

• Fisheries and Aquatic Sciences
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• v.24 no.10
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• pp.319-329
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• 2021

In the search for antibiotic alternatives from safe and effective medicinal plants against fish pathogenic bacteria, we found that a combined extract (CE) of 1:1 (w/w) ratio of Angelica gigas Nakai roots and aerial parts of Artemisia iwayomogi Kitamura showed antibacterial activity against the fish pathogenic bacteria. By antibacterial activity-guided fractionations and isolations, five compounds were isolated and identified as decursinol angelate (1), decursin (2), xanthotoxin (3), demethylsuberosin (4), and 2,4-dihydroxy-6-methoxyacetophenone (5) through spectroscopic analyses, such as nuclear magnetic resonance (NMR) and mass spectrometry (MS). Among the compounds, 1 and 2 showed the highest antibacterial activities against Streptococcus iniae and Vibrio anguillarum, showing minimum inhibitory concentrations (MICs) of 62.5-250 ㎍/mL. Compounds 3, 4, and 5 were also found to be active, with MICs of 31.25-1,000 ㎍/mL for those strains. Furthermore, active compounds, 1 and 2 in CE were simultaneously quantified using high-performance liquid chromatography-tandem MS (HPLC-MS/MS). The average contents of 1 and 2 in CE was 3.68% and 6.14%, respectively. The established method showed reliable linearity (r² > 0.99), good precision, accuracy, and specificity with intra- and inter-day variations of < 2 % and recoveries of 90.13%-108.57%. These results may be helpful for establishing the chemical profile of CE for its commercialization as an antibiotic alternative in aquaculture.

• Journal of Ginseng Research
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• v.42 no.2
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• pp.149-157
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• 2018

Background: Panax notoginseng leaves (PNL) exhibit extensive activities, but few analytical methods have been established to exclusively determine the dammarane triterpene saponins in PNL. Methods: Ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry (UPLC/Q-TOF MS) and HPLC-UV methods were developed for the qualitative and quantitative analysis of ginsenosides in PNL, respectively. Results: Extraction conditions, including solvents and extraction methods, were optimized, which showed that ginsenosides Rc and Rb3, the main components of PNL, are transformed to notoginsenosides Fe and Fd, respectively, in the presence of water, by removing a glucose residue from position C-3 via possible enzymatic hydrolysis. A total of 57 saponins were identified in the methanolic extract of PNL by UPLC/Q-TOF MS. Among them, 19 components were unambiguously characterized by their reference substances. Additionally, seven saponins of PNL-ginsenosides Rb1, Rc, Rb2, and Rb3, and notoginsenosides Fc, Fe, and Fd-were quantified using the HPLC-UV method after extraction with methanol. The separation of analytes, particularly the separation of notoginsenoside Fc and ginsenoside Rc, was achieved on a Zorbax ODS C8 column at a temperature of $35^{\circ}C$. This developed HPLC-UV method provides an adequate linearity ($r^2$ > 0.999), repeatability (relative standard deviation, RSD < 2.98%), and inter- and intraday variations (RSD < 4.40%) with recovery (98.7-106.1%) of seven saponins concerned. This validated method was also conducted to determine seven components in 10 batches of PNL. Conclusion: These findings are beneficial to the quality control of PNL and its relevant products.

• Biomolecules & Therapeutics
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• v.21 no.2
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• pp.170-172
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• 2013

The pyrimidine nucleoside uridine has recently been reported to have a protective effect on cultured human corneal epithelial cells, in an animal model of dry eye and in patients. In this study, we investigate the pharmacokinetic profile of uridine in rabbits, following topical ocular (8 mg/eye), oral (450 mg/kg) and intravenous (100 mg/kg) administration. Blood and urine samples were serially taken, and uridine was measured by high-performance liquid chromatography-tandem mass spectrometry. No symptoms were noted in the animals after uridine treatment. Uridine was not detected in either plasma or urine after topical ocular administration, indicating no systemic exposure to uridine with this treatment route. Following a single intravenous dose, the plasma concentration of uridine showed a bi-exponential decay, with a rapid decline over 10 min, followed by a slow decay with a terminal half-life of $0.36{\pm}0.05$ h. Clearance and volume of distribution were $1.8{\pm}0.6$ L/h/kg and $0.58{\pm}0.32$ L/kg, respectively. The area under the plasma concentration-time curves (AUC) was $59.7{\pm}18.2{\mu}g{\cdot}hr/ml$, and urinary excretion up to 12 hr was ~7.7% of the dose. Plasma uridine reached a peak of $25.8{\pm}4.1{\mu}g/ml$ at $2.3{\pm}0.8$ hr after oral administration. The AUC was $79.0{\pm}13.9{\mu}g{\cdot}hr/ml$, representing ~29.4% of absolute bioavailability. About 1% of the oral dose was excreted in the urine. These results should prove useful in the design of future clinical and nonclinical studies conducted with uridine.