• Journal of Pharmaceutical Investigation
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• v.36 no.5
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• pp.331-338
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• 2006

A rapid, selective and sensitive reverse-phase HPLC methods for the determination of atenolol and chlorthalidone in human serum and whole blood were validated, and applied to the pharmacokinetic study of atenolol and chlorthalidone combination therapy. Atenolol and an internal standard, pindolol, were extracted from human serum by liquid-liquid extraction, and analyzed on a $\mu$-Bondapak C18 $10-{\mu}$ column in a mobile phase of methanol-0.01 M potassium dihydrogenphosphate(30:70, v/v, adjusted to pH 3.5) and fluorescence detection(emission: 300 nm, excitation: 224 nm). Chlorthalidone and an internal standard, probenecid, were extracted form human whole blood by liquid-liquid extraction, and analyzed on a Luna C18 $5-{\mu}$ column in a mobile phase of acetonitrile containing 77% 0.01 M sodium acetate and UV detection at 214 nm. These analysis were performed at three different laboratories using the same quality control(QC) samples. The chromatograms showed good resolution, sensitivity, and no interference by human serum and whole blood, respectively. The methods showed linear responses over a concentration range of 10-1,000 ng/mL for atenolol and 0.05-20 ${\mu}g/mL$ for chlorthalidone, with correlation coefficients of greater than 0.999 at all the three laboratories. Intra- and inter-day assay precision and accuracy fulfilled international requirements. Stability studies(freeze-thaw, short-, long-term, extracted sample and stock solution) showed that atenolol and chlorthalidone were stable. The lower limit of quantitation of atenolol and chlorthalidone were 10 ng/mL and 0.05 ${\mu}g/mL$, respectively, which was sensitive enough for pharmacokinetic studies. These methods were applied to the pharmacokinetic study of atenolol and chlorthalidone in human volunteers following a single oral administration of Hyundai $Tenoretic^{\circledR}$ tablet(atenolol 50 mg and chlorthalidone 12.5 mg) at three different laboratories.

• Bulletin of the Korean Chemical Society
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• v.31 no.5
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• pp.1159-1164
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• 2010

Several triterpenoid saponins from root of Pulsatilla koreana Nakai (Ranunculaceae) were studied and their biological activities were reported. It is difficult to analyze triterpenoid saponins using HPLC-UV due to the lack of chromophores. So, evaporative light scattering detection (ELSD) is used as a valuable alternative to UV detection. More recently, a charged aerosol detection (CAD) has been developed to improve the sensitivity and reproducibility of ELSD. In this study, we developed and validated a novel method of high performance liquid chromatography coupled with a charged aerosol detector for the simultaneous determination of four triterpenoid saponins: pulsatilloside E, pulsatilla saponin H, anemoside B4 and cussosaponin C. Analytes were separated by the Supelco Ascentis$^{(R)}$ Express C18 column (4.6 mm ${\times}$ 150 mm, 2.7 ${\mu}m$) with gradient elution of methanol and water at a flow rate of 0.8 mL/min at $30^{\circ}C$. We examined various factors that could affect the sensitivity of the detectors, including various concentrations of additives, the pH of the mobile phase, and the CAD range. Linear calibration curves were obtained within the concentration ranges of 2 - 200 ${\mu}g$/mL for pulsatilloside E, anemoside $B_4$ and cussosaponin C, and 5 - 500 ${\mu}g$/mL for pulsatilla saponin H with correlation coefficient ($R^2$) greater than 0.995. The limit of detection (LOD) and quantification (LOQ) were 0.04 - 0.2 and 2 - 5 ${\mu}g$/mL, respectively. The validity of the developed HPLC-CAD method was confirmed by satisfactory values of linearity, intra- and inter-day accuracy and precision. This method could be successfully applied to quality evaluation, quality control and monitoring of Pulsatilla koreana.

• Korean Journal of Soil Science and Fertilizer
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• v.44 no.1
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• pp.1-7
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• 2011

Application of biochar to soils is proposed as a significant, long-term, sink for atmospheric carbon dioxide in terrestrial ecosystems. In addition to reducing emissions and increasing the sequestration of carbon, production of biochar and its application to soils will contribute improve soil quality and crop productivity. Objectives were i) to evaluate biochar productivity from crop residues using a low-cost field scale mobile pyrolyzer and ii) to evaluate characteristics of feedstocks and biochars from locally collected crop residues. Pyrolysis experiments were performed in a reactor operated at $400-500^{\circ}C$ for 3-4 hours using biomass samples of post-harvest residues of corn (Zea mays L.), cotton (Gossypium spp.), rice (Oryza sativa L.), sorghum (Sorghum bicolor L.) and wheat (Triticum aestivum L.). Feedstocks differed, but average conversion to biochar was 23%. Carbon content of biomass feedstock and biochar samples were 445 g $kg^{-1}$ and 597 g $kg^{-1}$, respectively. Total carbon content of biochar samples was 34% higher than its feedstock samples. Significant increases were found in P, K, Ca, Mg, and micro-nutrients contents between feedstock and biochar samples. Biochar from corn stems and rice hulls can sequester by 60% and 49% of the initial carbon input into biochar respectively when biochar is incorporated into the soils. Pyrolysis conversion of corn and rice residues sequestered significant amounts of carbon as biochar which has further environmental and production benefits when applied to soils. Field experiment with crop residue biochar will be investigated the stability of biochars to show long-term carbon sequestration and environmental influences to the cropping systems.

• KSBB Journal
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• v.29 no.4
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• pp.232-238
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• 2014

The simultaneous determination of creatine monohydrate (CrM), dicyandiamide and dihydrotriazine in dietary supplements using reversed-phase high performance liquid chromatography (HPLC) was developed. Chromatography was performed on a Nuclosil 100-5 SA ($4.6{\times}250mm$) column with a mobile phase of 2.3% ammonium phosphate (pH 5.5), and UV detection at 224 nm, 212 nm, and 237 nm, respectively. The performance characteristics of HPLC were determined in terms of selectivity, linearity, precision, recovery, limit of detection (LOD), and limit of quantification (LOQ). The calibration curves were linear within the concentration range of $40.0{\sim}500.0{\mu}g/mL$ for creatine, $0.1{\sim}12.8{\mu}g/mL$ for dicyandiamide, and $0.05{\sim}6.4{\mu}g/mL$ for dihydrotriazine. The detection limits of the method were 1.09, 0.01, and $0.08{\mu}g/mL$ for creatine, dicyandiamide, and dihydrotriazine, respectively. The recoveries of creatine, dicyandiamide, and dihydrotriazine were 97.2~100.9, 92.3~106.5, and 97.2~105.5%, respectively. It is expected that the chromatographic analytical method developed in this study will be usefully applicable to simultaneous determination of creatine, dicyandiamide, and dihydrotriazine contained in dietary supplements.

• Analytical Science and Technology
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• v.37 no.2
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• pp.98-113
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• 2024

The current investigation entails the characterization of five degradation products (DPs) formed under different stress conditions of loteprednol using liquid chromatography-tandem mass spectrometry (LC-MS/MS). In addition, this study developed a stable high-performance liquid chromatography (HPLC) method for evaluating loteprednol along with impurities. The method conditions were meticulously fine-tuned which involved the exploration of the appropriate solvent, pH, flow of the mobile phase, columns, and wavelength. The method conditions were carefully chosen to successfully resolve the impurities of loteprednol and were employed in subsequent validation procedures. The stability profile of loteprednol was exposed to stress degradation experiments conducted under five conditions, and DPs were structurally characterized by employing LC-MS/MS. The chromatographic resolution of loteprednol and its impurities along with DPs was effectively achieved using a Phenomenex Luna 250 mm C18 column using 0.1 % phosphoric acid, methanol, and acetonitrile in 45:25:30 (v/v) pumped isocratically at 0.8 mL/min with 243 nm wavelength. The method produces an accurate fit calibration curve in 50-300 ㎍/mL for loteprednol and LOQ (0.05 ㎍/mL) - 0.30 ㎍/mL for its impurities with acceptable precision, accuracy, and recovery. The stress-induced degradation study revealed the degradation of loteprednol under basic, acidic, and photolytic conditions, resulting in the formation of seven distinct DPs. The efficacy of this method was validated through LC-MS/MS, which allowed for the verification of the chemical structures of the newly generated DPs of loteprednol. This method was appropriate for assessing the impurities of loteprednol and can also be appropriate for structural and quantitative assessment of its degradation products.

• Analytical Science and Technology
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• v.37 no.4
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• pp.211-219
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• 2024

This study presents a sensitive and reliable method for determining tetracycline (TC), oxytetracycline (OTC), and chlortetracycline (CTC) residues in shrimp samples. A two-step process involving liquid-liquid extraction (LLE) followed by solid-phase extraction (SPE) was developed prior to HPLC analysis. The target analytes were effectively extracted using EDTA/McIlvaine buffer (pH 4.0): methanol (80:20, %v/v), with subsequent clean-up using a C18 SPE cartridge. HPLC separation was conducted on a C18 column (250 mm × 4.6 mm i.d., 5 ㎛) at 30 ℃, using 0.01 % trifluoroacetic acid (A) and acetonitrile (B) as the mobile phase. A gradient elution protocol was applied, transitioning from 85(A):15(B) %v/v to 70(A):30(B) %v/v at 7 min, with a 5 min hold, followed by adjustment to 85(A):15(B) %v/v for 13-14 min. The detection was performed using photodiode array (PDA) at 365 nm with a flow rate of 1.0 mL/min. The calibration curves exhibited good linearity within a concentration range of 0.4-6.0 ㎍/mL (R² > 0.995). The limits of detection (LOD) for TC, OTC, and CTC in shrimp were 0.034, 0.029, and 0.021 ㎍/mL, respectively. The limits of quantitation (LOQ) for TC, OTC, and CTC were found to be 0.114, 0.097, and 0.071 ㎍/mL, respectively. Recoveries of TC, OTC, and CTC from spiked shrimp samples ranged from 91.0 % to 95.5 %, 92.4 % to 97.2 %, and 93.3 % to 96.6 %, respectively. This method was successfully applied to the determination of TC, OTC, and CTC residues in shrimp samples sourced from various local markets.

• The KIPS Transactions:PartC
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• v.11C no.6 s.95
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• pp.835-842
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• 2004

In this paper, we have analyzed the MC-DS/CDMA system with input signal synchronized completely through adjustment of the gain in the PLL loop, by using the hybrid SC/MRC-(2/3) technique, which is said to one of the optimal diversity techniques under the multi-path fading environment, assuming that phase error is defined to the phase difference between the received signal from the multi-path and the reference signal in the PLL of the receiver. Also, assuming that the regarded radio channel model for the mobile communication is subject to the Nakagami-m fading channel, we have developed the expressions and performed the simulation under the consideration of various factor, in the MC/DS-CDMA system with the hybrid SC.MRC-(2/3) diversity method, such as the Nakagami fading index(m), $the\;number\;of\;paths\;(L_p),$ the number of hybrid SC.MRC-(2/3) $diversity\;branches\;(L,\;L_c),$ the number of users (K), the number of subcarriers (U), and the gain in the PLL loop. As a result of the simulation, it has been confirmed that the performance improvement of the system can be achieved by adjusting properly the PLL loop in order for the MC/DS-CDMA system with the hybrid SC/MRC-(2/3) diversity method to receive a fully synchronized signal. And the value of the gain in the PLL loop should exceed 7dB in order for the system to receive the signal with prefect synchronization, even though there might be a slight difference according to the values of the fading index and the spread processing gain of the subcarrier.

• Analytical Science and Technology
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• v.20 no.2
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• pp.138-146
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• 2007

A simple and sensitive method for the determination of paroxetine in canine plasma was developed and validated by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC-/MS/MS). Fluoxetine was used as an internal standard. Paroxetine and internal standard in plasma samples were extracted using TBME (tert-butyl methyl ether). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 50% acetonitrile adjusted to pH 3 by formic acid. The reconstituted samples were injected into a Capcell Pak UG120 ($2.0{\times}150mm$, $5{\mu}m$) column. Using MS/MS with SRM (selective reaction monitoring) mode, the transitions (precursor to product) monitored were m/z $330{\rightarrow}192$ for paroxetine, and m/z $310{\rightarrow}148$ for internal standard. Linear detection responses were obtained for paroxetine concentration range of 0.02~5 ng/mL. A correlation coefficient of linear regression ($R^2$) was 0.9993. Detection of paroxetine in canine plasma was accurate and precise, with limit of quantification at 0.02 ng/mL. The method has been successfully applied to pharmacokinetic study of paroxetine in healthy beagle dogs.

• Analytical Science and Technology
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• v.32 no.6
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• pp.217-224
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• 2019

In this study, to evaluate the effectiveness and safety of oral therapy using Gastrodiae Rhizoma, a new HPLC-PDA analysis method was developed for the simultaneous quantitation of the three major components: (1) gastrodin, (2) gastrodigenin, and (3) p-hydroxybenzaldehyde, in steam processed and unprocessed tubers of Gastrodia elata Blume. The clear separation of the three components was achieved on a C18 column (250 × 4.6 mm, 5 ㎛) by gradient elution using water (including 0.1 % formic acid) and acetonitrile as the mobile phase. The flow rate was 1.0 mL/min, and the UV detector wavelength was set at 270 nm. The results demonstrate satisfactory linearity, recovery, precision, accuracy, stability, and robustness. The established HPLC-PDA method was applied to quantify three major compounds in 59 samples of G. elata Blume tubers. Finally, the steam processed and unprocessed tubers of G. elata Blume were successfully distinguished by pattern recognition analysis.

• Mass Spectrometry Letters
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• v.8 no.2
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• pp.29-33
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• 2017

Understanding the mechanisms that control and concentrate the observed electrospray ionisation (ESI) response from peptides is important. Controlling these mechanisms can improve signal-to-noise ratio in the mass spectrum, and enhances the generation of intact ions, and thus, improves the detection of peptides when analysing mixtures. The effects of different mixtures of aqueous: organic solvents (25, 50, 75%; v/v): formic acid solution (at pH 3.26) compositions on the ESI response and charge-state distribution (CSD) during mass spectrometry (MS) were determined in a group of biologically active peptides (molecular wt range 1.3 - 3.3 kDa). The ESI response is dependent on type of organic solvent in the mobile phase mixture and therefore, solvent choice affects optimal ion intensities. As expected, intact peptide ions gave a more intense ESI signal in polar protic solvent mixtures than in the low polarity solvent. However, for four out of the five analysed peptides, neither the ESI response nor the CSD were affected by the volatility of the solvent mixture. Therefore, in solvent mixtures, as the composition changes during the evaporation processes, the $pK_b$ of the amino acid composition is a better predictor of multiple charging of the peptides.