• Biomolecules & Therapeutics
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• v.14 no.1
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• pp.40-44
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• 2006

Mirtazapine is an antidepressant agent with dual action on both the noradrenergic and serotonergic neurotransmitter systems. A simple high performance liquid chromatographic method has been developed and validated for the quantitative determination of mirtazapine in human plasma. A reversed-phase Cl8 column was used for the determination of mirtazapine with a mobile phase composed of 0.01M ammonium acetate solution (pH 4.2) and acetonitrile (75:25, v/v%) at a flow rate of 1.2 mL/min. Terazosin hydrochloride was used as an internal standard. The fluorescence detector was set at excitation and emission wavelengths of 290 and 350 nm, respectively. Intra- and inter-day precision and accuracy were acceptable for all quality control samples including the lower limit of quantification of 3 ng/mL. Mirtazapine was stable in human plasma under various storage conditions. This method was used successfully for a pharmacokinetic study using plasma samples after oral administration of a single 30 mg dose as mirtazapine base to 8 healthy volunteers. The maximum plasma concentration of mirtazapine was $64.1{\pm}28.0ng/mL$ at 1.8 h, and the area under the curve and elimination half-life were calculated to be $674.1{\pm}218.5ng\;h/mL\;and\;23.4{\pm}3.8h$, respectively.

• Archives of Pharmacal Research
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• v.19 no.5
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• pp.396-399
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• 1996

High-performance liquid chromatographic method with UV detecction was developed for the determination of theophylline and its metabolites in human urine using ${beta}$-hydroxyethyl theophylline$({beta} -HET)$ as an internal standard. For extraction of urine sample, quality control sample and xanthine-free blank urine were mixed with decylamine (ion-paring reagent) and ${beta}$-HET. After saturation with ammonium sulfate, the mixture was then extracted with organic solvent at pH values of 4.0-4.5. All separations were performed with ion-pair chromatography using decylamine as an ion-pairing reagent and 3mM sodium acetate buffered mobile phase (pH 4.0) containing 1% (v/v) acetonitrile and 0.75 mM decylamine. The detection limits of theophylline, 1, 3-DMU, 1-MU, 3-MX and 1-MX in human urine were 0.17, 0.17, 0.39, 0.19 and 0.19 ${\mu}g$/ml, based on a signal-to-noise ratios of 3.0. The mean intraday coefficients of variation (C.V.s) of each compound on nine replicates were lower than 2.0%, while mean interday C.V.s on three days were lower than 1.6%. All separations were finished within 40miutes.

• Journal of Food Hygiene and Safety
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• v.23 no.4
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• pp.324-329
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• 2008

An analytical method for the simultaneous determination of nine quinolones (QNs) namely, marbofloxacin, norfloxacin(IS), ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid, and flumequine in flatfish and egg was developed and validated using liquid chromatography with fluorescence detection (LC-FD). The samples were extracted using a traditional liquid-liquid extraction process; deproteinization was accomplished by the addition of trichloroacetic acid and acetonitrile (ACN), and defatting was performed with hexane. Chromatographic separation was achieved on a reverse phase C8 column with gradient elution using a mobile phase of 200 mM ammonium acetate buffer (pH 4.5) and ACN. The proposed method was validated according to the CODEX guideline. Mean recoveries of QNs from flatfish and egg were 89.6-106.5% with relative standard deviations (RSDs) below 15% at three different concentrations of 50, 100 and $500{\mu}g/kg$. Linearity was obtained with a correlation coefficient ($r^2$) of 0.9989-1.0000. The LOD for the investigated QNs was $1-16{\mu}g/kg$ depending on flatfish and egg. The present method can be applied simultaneously to determine QNs in muscle of flatfish and egg.

• Archives of Pharmacal Research
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• v.21 no.2
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• pp.217-222
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• 1998

A stereospecific HPLC method has been developed for the resolution of the enantiomers of salbutamol in human urine. After solid-phase extraction and derivatization with 2,3,4,6-tetra-O-acetyl-$\beta$-D-glucopyranosyl isothiocyanate, the diastereomeric derivatives were resolved (Rs=1.83) on $5{\mu}m$ octadecylsilan column using 35% acetonitrile in 0.05M ammonium acetate buffer (pH=6) as a mobile phase with electrochemical detection. The diastereomeric derivatives were formed within 30 min. The detection limit of each enantiomer was 20 ng/ml (S/N=3).

• Korean Journal of Veterinary Service
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• v.25 no.3
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• pp.221-227
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• 2002

This study was carried out to confirm analytical method of residual macrolides in livestock products by LC/MS. 1. Macrolides were analyzed by LC/MS on XTerra C$\sub$18/ column with 0.1% TFA(trifluoroacetic acid)-methanol in a gradient mode as mobile phase, and that were identified by positive chemical ionization with selective ion monitoring at 50～1000 mass range. 2. Residual macrolides were extracted from tissue with acetonitrile, and the extract is purified with a Sep-pak C$\sub$18/ cartridge, and elute macrolides with 0.1M methanolic ammonium acetate. 3. The procedure confirms the presence of each macrolide at 50$\mu\textrm{g}$/kg in spiked sample.

• Journal of Environmental Health Sciences
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• v.22 no.2
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• pp.32-42
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• 1996

This study was performed to evaluate accuracy and precision of filter method and impinger method for analyzin airborne isocyanates in mixture (2, 6-TDI, HDI, 2, 4-TDI, MDI). Filter method was performed using the OSHA Method 42 and impinger method using the NIOSH Method 5521. The samples were analyzed by high performance liquid chromatography-ultraviolet detector (HPLC-UVD). After the optimum operating conditions for each method were investigated, samples with various concentration levels were quantified at the conditions. The precision was expressed by the pooled coefficient of variation(C.V.) and the accuracy by overall accuracy. The results are summarized as follows: 1. The optimum condition of filter method was determined at 35/65 ACN/buffer (0.01 M ammonium acetate) in mobile phase. And in case of impinger method, it was at 30/70 ACN/buffer(0.2 M sodium acetate). The effect of concentrations of acetate on the separation of the peaks was not significant, but, the effect of ACN/buffer ratio was significant. 2. The correlation coefficients for the two methods were above 0.9 in all isocyanate compounds. Average recovery efficiencies for 2, 6-TDI, HDI, 2, 4-TDI and MDI in filter method were 92.4%, 102.6%, 87.3% and 101.0%, respectively. Those in impinger method were 106.6%, 106.7%, 99.0% and 103.6%, respectively. As a result, the recovery efficiency of impinger method was higher than those of filter method in analyzing isocyanate compounds. 3. The pooled coefficients of variations of the methods were slightly higher than expected. The overall accuracies of the methods were within $\pm 25%$ for each isocyanate compound. Since these results satisfy NIOSH criteria, the accuracy of the experiment is appropriate. 4. As seen above, impinger method is more efficient than filter method. But, there are many disadvantages in impinger method. Therefore, solid sorbent such as a glass fiber filter must be developed in order to have the high efficiency not less than that of impinger method in the future.

• Mass Spectrometry Letters
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• v.5 no.2
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• pp.52-56
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• 2014

Glycated hemoglobin (HbA1c) is used as an index of mean glycemia over prolonged periods. This study describes an optimization of enzyme digestion conditions for quantification of non-glycated hemoglobin (HbA0) and HbA1c as diagnostic markers of diabetes mellitus. Both HbA0 and HbA1c were quantitatively determined followed by enzyme digestion using isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) with synthesized N-terminal hexapeptides as standards and synthesized isotope labeled hexapeptides as internal standards. Prior to quantification, each peptide was additionally quantified by amino acid composition analysis using ID-LC-MS/MS via acid hydrolysis. Each parameter was considered strictly as a means to improve digestion efficiency and repeatability. Digestion of hemoglobin was optimized when using 100 mM ammonium acetate (pH 4.2) and a Glu-C-to-HbA1c ratio of 1:50 at $37^{\circ}C$ for 20 h. Quantification was satisfactorily reproducible with a 2.6% relative standard deviation. These conditions were recommended for a primary reference method of HbA1c quantification and for the certification of HbA1c reference material.

• Journal of Pharmaceutical Investigation
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• v.39 no.1
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• pp.73-78
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• 2009

A simple LC-MS/MS method of rabeprazole in human plasma was developed and validated. Rabeprazole and Internal standard (I.S), omeprazole, were extracted from human plasma by liquid liquid extraction, chromatographic separation of rabaprazole in plasma was achieved at $45^{\circ}C$ with a Shiseido UG120 $C_{18}$ column and methanol-10 mM ammonium acetate buffer (pH 9.42 with ammonium water), as mobile phase. Rabeprazole produced a protonated precursor ion [$(M+H)^+$] at m/z 360.10 and corresponding product ion at m/z 242.21. Internal standard produced a protonated precursor ion [$(M+H)^+$] at 346.09 and corresponding product ion at m/z 198.09. This method showed linear response over the concentration range of $1{\sim}500\;ng/mL$ with correalation coefficient greater than 0.99. The lower limit of quantitation (LLOQ) using 0.2 mL plasma was 1 ng/mL, which was sensitive enough for pharmacokinetics studies. The method was specific and validated with a limit of quantitation of 1 ng/mL. The intra-day and inter-day precision and accuracy were acceptable for all samples including the LLOQ. The applicability of the method was demonstrated by analysis of plasma after administration of a single 10 mg dose to 36 healthy subject. From the plasma rabeprazole concentration versus time curves, the mean $AUC_t$ (The area under the plasma concentration-time curve from time 0 to 12 hr ) was $691.36{\pm}321.88\;ng{\cdot}hr/mL$, $C_{max}$ (maximum plasma drug concentration) of $353.21{\pm}131.52\;ng/mL$ reached $3.4{\pm}1.1\;hr$ after adiministration. The mean biological half-life of rabeprazole was $1.37{\pm}0.75\;hr$. Based on the results, this simple method could readily be used in pharmacokinetics studies.

• Mass Spectrometry Letters
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• v.5 no.3
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• pp.89-93
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• 2014

Lincomycin is one of the major species among the Pharmaceuticals and Personal Care Products (PPCPs) detected from the four major rivers in Korea. The structure characterization was performed of six degradation products of lincomycin formed under the irradiation of electron beam, and the degradation efficiency as a function of the various irradiation dose and sample concentration was investigated. Electron beam (10 MeV, 0.5 mA and 5 kW) experiments for the structural characterization of degradation products that are fortified with lincomycin, were performed at the dose of 10 kGy. The separation of degradation products and lincomycin was carried out using a C18 column ($2.1{\times}100$ mm, $3.5{\mu}m$), using gradient elution with 20 mM ammonium acetate and acetonitrile. The structures of six degradation products of lincomycin were proposed by interpretation of mass spectra and chromatograms by LC-MS/MS. The mass fragmentation pathways of mass spectra in tandem mass spectrometry were also proposed. Experiments were performed of the degradation efficiency as a function of the irradiation dose intensity and the initial concentration of lincomycin in an aqueous environment. In addition, increased degradation efficiency was observed with a higher dose of electron beam and lower concentration.

• Korean Journal of Soil Science and Fertilizer
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• v.22 no.2
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• pp.116-121
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• 1989

An experiment on movements of copper in soils was conducted to evaluate the effectiveness of several soil extractants in predicting to be possibly the plant availability of copper in soils. Soil samples were taken six, from Las Virgines loam that the samples naturally included high contents of heavy metals near Los Angeles, Greenfield sandy loam and IDomino Loam that received 22.5, and $45.0mg.\;ha^{-1},\;yr^{-1}$ of composted sludge from Los Angeles from 1975 to 1983, respectively. Copper in soils were extracted with $4M\;HNO_3$, 0.1M HCl, 0.5M DTPA-0.1M TEA, 0.5M EDTA-0.1M $Ca(NO_3)_2$, and 1M ammonium acetate(pH 7), and analyzed by atomic absorption spectroscopy. The results were as follows: 1. The total copper contents in soil that received $45.0mg.\;ha^{-1},\;yr^{-1}$ of composted sludge were higher than that received $22.5mg.\;ha^{-1}.yr^{-1}$, regardless of soil samples. 2. The ratios of extractable copper contents with EDTA, DTPA, 0.1M HCl and 1M ammonium acetate to total copper contents extracted with 4M $HNO_3$ of long-term sludge applications were larger than those of natural, sludge-nontreated soils. 3. Statistically significant increase in total copper contents was found in the increasing values of multipling CEC, or OM% by R, ratio of extractable copper contents to those by 4M $HNO_3$ extraction as total copper contents in soils.