• Proceedings of the PSK Conference
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• 2003.10b
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• pp.239.1-239.1
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• 2003

This study was to develop a quantification method of lisinopril using liquid chromatography tendem mass spectrometry in human plasma. Quntitation of lisinopril by MRM(multiple reaction monitoring) in the electrospray positive mode was validated according to FDA guideline. Extraction of lisinopril and enalapril as internal standard from plasma was perfomed by means solide phase extraction. The calibration curve of lisinopril showed a good linerarity in the concentration range 2∼200ng/ml. The coefficients of variations for the inter-day and intra-day precision was less than 15%, and the inter-day and intra-day accuracy was 97.6∼101.0%. (omitted)

• Analytical Science and Technology
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• v.11 no.6
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• pp.499-504
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• 1998

An analytical method for the simultaneous measurement of trace Cu, Sn, and Bi in sea water has been investigated by Inductively Coupled Plasma-Mass Spectrometry. Amberlite IRC-718 resin was used as a solid phase in solid-liquid extraction technique for the removal of matrix interferences such as Na, S, P, and other polyatomic ion species. Recoveries of 99.8% for Cu, 99.6% for Sn, and 97.9% for Bi were obtained for the standard spiked sample. The developed method was applied to analysis of trace metals in sea water.

• Journal of Life Science
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• v.19 no.12
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• pp.1698-1704
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• 2009

Gemcitabine is an anticancer drug used to treat a variety of solid tumors. The drug is rapidly inactivated by cytidine deaminase in plasma and its hydrophilicity restricts the extent of quantification that is possible using reversed-phase liquid chromatography. In this paper, we report a rapid and precise method to analyze velocity and peak efficiency using ultra-performance liquid chromatography (UPLC) with a reversed-phase column. The retention periods of gemcitabine and 2'-deoxycytidine at 283 nm were 3.2 and 2.1 min, respectively. The assay provided highly linear results in the range of $0.1{\sim}20{\mu}g/ml$ ($r^2$ > 0.999). The coefficients of variation of the intra-day and inter-day assays were less than 10.0%. We observed that the estimated average concentrations of the intra-day and inter-day assays ranged from 97.3 to 113.5% to verify the accuracy. These results suggest that this new reversed-phase UPLC method is a rapid and reliable way of determining gemcitabine levels.

• Mass Spectrometry Letters
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• v.10 no.1
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• pp.18-26
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• 2019

We developed a bioanalytical method for simultaneous determination of nine NBOMe derivatives (25H-NBOMe, 25B-NBOMe, 25E-NBOMe, 25N-NBOMe, 25C-NBOH, 25I-NBOH, 25B-NBF, 25C-NBF, and 25I-NBF) in human plasma using liquid chromatography tandem mass spectrometry (LC-MS/MS). Human plasma samples were pre-treated using solid-phase extraction. Separation was achieved on a C18 column under gradient elution using a mobile phase containing 0.1% formic acid in acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Mass detection was performed in the positive ion mode using multiple reaction monitoring. The calibration range was 1-100 ng/mL for all quantitative analytes, with a correlation coefficient greater than 0.99. The intra- and inter-day precision and accuracy varied from 0.85 to 6.92% and from 90.19 to 108.69%, respectively. The recovery ranged from 86.36 to 118.52%, and the matrix effects ranged from 27.09 to 99.72%. The stability was acceptable in various conditions. The LC-MS/MS method was validated for linearity, accuracy, precision, matrix effects, recovery and stability in accordance with the FDA guidance. The proposed method is suitable for reliable and robust routine screening and analysis of nine NBOMe derivatives in forensic field.

• Journal of Pharmaceutical Investigation
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• v.22 no.4
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• pp.317-321
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• 1992

A high-performance liquid chromatographic (HPLC) method was developed for the determination of diltiazem (DTZ) and its major metabolite, deacetyldiltiazem (DAD), in rat plasma. DTZ, DAD and imipramine, the internal standard, were selectively fractionated from plasma on a $C_{18}$ reversedphase column $({\mu}-Bondapak,\;10\;{\mu}m\;silica,\;300{\times}3.9\;mm\;ID)$. The composition of the mobile phase was methanol: acetonitrile: 0.04 M ammonium bromide: triethylamine (40:24:36:0.06 in volume). The pH of the mobile phase of their method was lowered to 6.4. The eluents from the column were detected for DTZ and DAD using a UV detector at 237 nm. The recovery was >85% for DTZ and DAD, and average intra-day and inter-day coefficients of variation were <6% for DTZ and DAD at the concentration ranges of 20-1000 ng/ml. Detection limit of DTZ and DAD in plasma was 20 ng/ml with signal-to-noise ratio of 3. This method would be applicable to practical pharmacokinetic studies without detriment to the HPLC column.

• Bulletin of the Korean Chemical Society
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• v.24 no.5
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• pp.559-565
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• 2003

An analytical method the determination of benzo(a)pyrene (BaP) and its hydroxylated metabolites, 1-hydroxybenzo(a)pyrene (1-OHBaP), 3-hydroxybenzo(a)pyrene (3-OHBaP), benzo(a)pyrene-4,5-dihydrodiol (4,5-diolBaP) and benzo(a)pyrene-7,8-dihydrodiol (7,8-diolBaP), in rat urine and plasma has been developed by HPLC/FLD and GC/MS. The derivatization with alkyl iodide was employed to improve the resolution and the detection of two mono hydroxylated metabolites, 1-OHBaP and 3-OHBaP, in LC and GC. BaP and its four metabolites in spiked urine were successfully separated by gradient elution on reverse phase ODS $C_{18}$ column (4.6 mm I.D., 100 mm length, particle size 5 ㎛) using a binary mixture of MeOH/H₂O (85/15, v/v) as mobile phase after ethylation at 90 ℃ for 10 min. The extraction recoveries of BaP and its metabolites in spiked samples with liquid-liquid extraction, which was better than solid phase extraction, were in the range of 90.3- 101.6% in n-hexane for urine and 95.7-106.3% in acetone for plasma, respectively. The calibration curves has shown good linearity with the correlation coefficients (R²) varying from 0.992 to 1.000 for urine and from 0.996 to 1.000 for plasma, respectively. The detection limits of all analytes were obtained in the range of 0.01-0.1 ng/mL for urine and 0.1-0.4 ng/mL for plasma, respectively. The metabolites of BaP were excreted as mono hydroxy and dihydrodiol forms after intraperitoneal injection of 20 mg/kg of BaP to rats. The total amounts of BaP and four metabolites excreted in dosed rat urine were 3.79 ng over the 0-96 hr period from adminstration and the excretional recovery was less than 0.065% of the injection amounts of BaP. The proposed method was successfully applied to the determination of BaP and its hydroxylated metabolites in rat urine and plasma for the pharmacokinetic studies.

• Korean Journal of Materials Research
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• v.21 no.2
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• pp.106-110
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• 2011

A high thermal conductive AlN composite coating is attractive in thermal management applications. In this study, AlN-YAG composite coatings were manufactured by atmospheric plasma spraying from two different powders: spray-dried and plasma-treated. The mixture of both AlN and YAG was first mechanically alloyed and then spray-dried to obtain an agglomerated powder. The spray-dried powder was primarily spherical in shape and composed of an agglomerate of primary particles. The decomposition of AlN was pronounced at elevated temperatures due to the porous nature of the spray-dried powder, and was completely eliminated in nitrogen environment. A highly spherical, dense AlN-YAG composite powder was synthesized by plasma alloying and spheroidization (PAS) in an inert gas environment. The AlN-YAG coatings consisted of irregular-shaped, crystalline AlN particles embedded in amorphous YAG phase, indicating solid deposition of AlN and liquid deposition of YAG. The PAS-processed powder produced a lower-porosity and higher-hardness AlN-YAG coating due to a greater degree of melting in the plasma jet, compared to that of the spray-dried powder. The amorphization of the YAG matrix was evidence of melting degree of feedstock powder in flight because a fully molten YAG droplet formed an amorphous phase during splat quenching.

• Mass Spectrometry Letters
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• v.2 no.4
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• pp.88-91
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• 2011

The pharmacokinetic properties of S-amlodipine were studied using racemic amlodipine and single S-enantiomer (SK310) administration to rats. Plasma levels of the drug were determined using chiral liquid chromatography coupled with tandem mass spectrometry following solid phase extraction. The stereospecific analysis of amlodipine was performed on an ${\alpha}$-acid glycoprotein (AGP) column using a mobile phase comprising 10 mM ammonium acetate (pH 4.0) and propanol at a flow rate of 0.2 mL/min. This method was used to perform a comparative study of the pharmacokinetics of amlodipine and SK310. The results revealed that the pharmacokinetic profile of S-amlodipine after the administration of SK310 was comparable to that following the administration of the racemic mixture.

• Proceedings of the PSK Conference
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• 2003.04a
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• pp.277.2-278
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• 2003

A liquid chromatography-tandem mass spectrometric (LC/MS/MS) method for the determination of tiropramide in human plasma was developed. Tiropramide and internal standard, cisapride were extracted from human plasma with MTBE at basic pH. A reverse-phase LC separation was performed on Luna C8 column with the mixture of acetonitrile-ammonium formate (10 mM, pH 4.5) (5:5, v/v) as mobile phase. (omitted)

• Archives of Pharmacal Research
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• v.23 no.5
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• pp.441-445
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• 2000

Achiral-chiral column switching HPLC assay was developed to allow the separation and quantification of the enantiomers of terbutaline in human plasma by means of fluorescence detection. Plasma samples were prepared by solid-phase extraction with sep-pak silica, followed by HPLC assay. The enantiomers of terbutaline and the internal standard were separated from the biological matrix on a silica column, and the two enantiomers were resolved and quantified on a Sumichiral OA-4900 column. The two columns were connected by a switching valve equipped with silica trap column, The trap column was used to concentrate the terbutaline in the eluent from the achiral column before back flushing onto the chiral phase. For each enantiomers, the assay was linear between 2.5-125 ng/$m\ell$ (r=0.9999) and detection limit was 1.0 ng/$m\ell$ .