FAD: Pauthors

Contact Info

Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf

Dalibor Satinsky

Abbrev:

Satinsky, D.

Other Names:

Dalibor Satínsky

Address:

Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, 500 05 Hradec Kralove, Czech Republic

Phone:

+420-495067274

Fax:

+420-495518718

Email:

satinsky@faf.cuni.cz

Citations 11

'Sequential Injection Chromatographic Determination Of Ambroxol Hydrochloride And Doxycycline In Pharmaceutical Preparations', Talanta, 2005 68(2) 214-218

"Sequential Injection Chromatographic Determination Of Ambroxol Hydrochloride And Doxycycline In Pharmaceutical Preparations"
Talanta 2005 Volume 68, Issue 2 Pages 214-218
Dalibor &Scaron;atínský, Lucia M. L. Dos Santos, Hana Sklenářová, Petr Solich, M.Conceição B.S.M. Montenegro and Alberto N. Araújo

Abstract: A new separation method based on a novel reversed-phase sequential injection chromatography (SIC) technique was used for simultaneous determination of ambroxol hydrochloride and doxycycline in pharmaceutical preparations in this contribution. The coupling of short monolith with SIA system results in an implementation of separation step to until no-separation low-pressure method. A Chromolith® Flash RP-18e, 25-4.6 mm column (Merck, Germany) and a FIAlab® 3000 system (USA) with a six-port selection valve and 5 mL syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-water (20:90, v/v), pH 2.5 adjusted with 98% phosphoric acid, flow rate 0.48 mL min-1, UV detection was at 213 nm. The validation parameters have shown good results: linearity of determination for both compounds including internal standard (ethylparaben) >0.999; repeatability of determination (RSD) in the range 0.5-5.4% at three different concentration levels, detection limits in the range 0.5-2.0 ?g mL -1, and recovery from the pharmaceutical preparation in the range 99.3-99.9%. The chromatographic resolution between peak compounds was >5.0 and analysis time was <9 min under the optimal conditions. The method was found to be applicable for routine analysis of the active compounds ambroxol hydrochloride and doxycycline in various pharmaceutical preparations. © 2005 Elsevier B.V. All rights reserved.

'Determination Of Ambroxol Hydrochloride, Methylparaben And Benzoic Acid In Pharmaceutical Preparations Based On Sequential Injection Technique Coupled With Monolithic Column', J. Pharm. Biomed. Anal., 2006 40(2) 287-293

"Determination Of Ambroxol Hydrochloride, Methylparaben And Benzoic Acid In Pharmaceutical Preparations Based On Sequential Injection Technique Coupled With Monolithic Column"
J. Pharm. Biomed. Anal. 2006 Volume 40, Issue 2 Pages 287-293
Dalibor &Scaron;atínský, Jitka Huclová, Raquel L.C. Ferreira, Maria Conceição B.S.M. Montenegro and Petr Solich

Abstract: The porous monolithic columns show high performance at relatively low pressure. The coupling of short monoliths with sequential injection technique (SIA) results in a new approach to implementation of separation step to non-separation low-pressure method.In this contribution, a new separation method for simultaneous determination of ambroxol, methylparaben and benzoic acid was developed based on a novel reversed-phase sequential injection chromatography (SIC) technique with UV detection.A Chromolith® SpeedROD RP-18e, 50-4.6 mm column with 10 mm precolumn and a FIAlab® 3000 system with a six-port selection valve and 5 mL syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-tetrahydrofuran-0.05 M acetic acid (10:10:90, v/v/v), pH 3.75 adjusted with triethylamine, flow rate 0.48 mL min-1, UV-detection was at 245 nm. The analysis time was <11 min.A new SIC method was validated and compared with HPLC. The method was found to be useful for the routine analysis of the active compounds ambroxol and preservatives (methylparaben or benzoic acid) in various pharmaceutical syrups and drops.

'Sequential Injection Extraction Based On Restricted Access Material For Determination Of Furosemide In Serum', J. Chromatogr. A, 2005 1087(1-2) 245-251

"Sequential Injection Extraction Based On Restricted Access Material For Determination Of Furosemide In Serum"
J. Chromatogr. A 2005 Volume 1087, Issue 1-2 Pages 245-251
Jitka Huclová, Dalibor &Scaron;atínský, Tiago Maia, Rolf Karlíček, Petr Solich and Alberto Nova Araújo

Abstract: Restricted access material (RAM) column containing 25 µm C18 alkyl-diol support was integrated into the sequential injection analysis (SIA) manifold and the SIA-RAM system was tested for direct determination of furosemide in serum. LiChrospher[trademark] ADS column based on restricted access material is proposed to direct injection of biofluids. The integration of RAM material into SIA enabled creation of a comprehensive on-line sample clean-up technique combined with fluorescence quantitation of analyte.Centrifuged and diluted serum sample was aspirated into the system and loaded onto the column using acetonitrile-water (2:98), pH 2.7. The analyte was retained on the column while proteins contained in the sample were removed to the waste without precipitation and clogging the column. Interfering substances complicating the detection were washed out by acetonitrile-water (15:85), pH 2.7 in the next step. The extracted analyte was eluted by means of acetonitrile-water (25:75), pH 2.3 to the fluorescence detector (emission filter 385 nm). The whole procedure comprising sample pre-treatment, analyte detection and column reconditioning took 20 min. The recoveries of furosemide from serum lay between 101.4 and 103.4% for three concentrations of analyte.

'Reversed-phase Porous Silica Rods, An Alternative Approach To High-performance Liquid Chromatographic Separation Using The Sequential Injection Chromatography Technique', J. Chromatogr. A, 2003 1015(1-2) 239-244

"Reversed-phase Porous Silica Rods, An Alternative Approach To High-performance Liquid Chromatographic Separation Using The Sequential Injection Chromatography Technique"
J. Chromatogr. A 2003 Volume 1015, Issue 1-2 Pages 239-244
Dalibor Satínský, Jitka Huclová, Petr Solich and Rolf Karlícek

Abstract: A commercially available porous silica rod column was used as a separation tool for the sequential injection analysis (SIA). A porous solid monolithic column showed high performance at a low pressure, allowing sequential injection analysis to be used for the first time for separation in HPLC fashion. In this contribution, we tried to demonstrate a new separation concept with SIA manifold for the simultaneous determination of four different compounds (methylparaben (MP), propylparaben (PP), triamcinolone acetonide (TCA) and internal standard ketoprofen (KP)) in a pharmaceutical triamcinolon cream 0.1% formulation. A Chromolith Flash RP-18e, 25 mm x 4.6 mm column with a 10 mm pre-column (Merck, Germany) and a FIAlab 3000 system (USA) with an 8-port selection valve and 10 mL syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-methanol-water (35:5:65, v/v/v) + 0.05% nonylamine, pH 2.5, flow rate 0.6 mL min-1. The analysis time was sequential injection chromatography (SIC) technique with UV spectrophotometric detection was optimized and validated.

'Determination Of Bopindolol By Sequential Injection Technique With Spectrophotometric Detection', Il Farmaco, 2003 58(10) 1057-1062

"Determination Of Bopindolol By Sequential Injection Technique With Spectrophotometric Detection"
Il Farmaco 2003 Volume 58, Issue 10 Pages 1057-1062
Dalibor Satínský, Hana Sklenáová, Jitka Huclová and Rolf Karlícek

Abstract: In the proposed procedure, the determination of bopindolol using a sequential injection technique (SIA) with spectrophotometric detection at 560 nm is described. The new method of determination is based on the color reaction of the indole group in the molecule of bopindolol with 4-dimethylaminobenzaldehyde (Ehrlich's reagent) in acidic medium with production of a violet water-soluble complex. Due to the kinetic standpoint of reaction, the 'stopped flow' technique with mixing coil between the valve and detector was tested and optimized. The proposed SIA system was used for the direct determination of bopindolol in tablets, negative effects of interfering substances (excipients of tablets) were not observed. The selectivity of the proposed method of determination was tested in the presence of seven interfering substances from the group of β-blockers with good results. The interference effect was observed only in the presence of pindolol. The sample throughput with stopped flow technique was 40 samples per hour. Bopindolol was determined in the linear range from 1 to 10 µg mL-1, RSD was less than 1% (n=10), with limit of detection (3s) 0.1 µg mL-1 and limit of quantification 0.5 µg mL-1. Obtained results were compared with conventional HPLC method, both analytical techniques were in good agreement.

'Solid Phase Reactors In Flow Injection Analysis', Chem. Listy, 2001 95(3) 150-156

"Solid Phase Reactors In Flow Injection Analysis"
Chem. Listy 2001 Volume 95, Issue 3 Pages 150-156
D. Satinsky and R. Karlicek

Abstract: The review deals with the principles and practical applications of the use of the solid phase reactors in FIA (flow injection analysis) techniques. The article is confined to the advances in the development of the analysis of samples in the flow systems, mainly on-line preparation (derivatization, separation and pre-concentration) of samples inside the flow injection manifold. The article involves 82 references covering the period from 1985 to 1999.

Review

'Using On-line Solid Phase Extraction For Determination Of Amiloride In Human Urine By Sequential Injection Technique', Anal. Chim. Acta, 2006 573(1) 376-382

"Using On-line Solid Phase Extraction For Determination Of Amiloride In Human Urine By Sequential Injection Technique"
Anal. Chim. Acta 2006 Volume 573, Issue 1 Pages 376-382
Jitka Huclová, Dalibor &Scaron;atínský, Ondřej Pavlíček, Lucie Vedralová and Rolf Karlíček

Abstract: This presented paper deals with a new methodology for the direct determination of amiloride in human urine. The methodology described is based on the sequential injection analysis technique (SIA) coupled with solid phase extraction (SPE) microcolumn. SPE microcolumn was used for selective retention of amiloride, while the urine matrix components were eluted with water carrier flow to the waste. Due to the acid-basic and polarity properties of amiloride molecule and principles of ion-exchange chromatography, it was possible to retain amiloride on the ion-exchange sorbent (SPE BAKER WCX-carboxy group). Eluting solution was 0.01 M HNO3 + 0.1 M KCl, flow rate 20 µl s-1. The fluorescence detection of amiloride was performed at λem 385 nm (secondary filter). Recovery was found in the range 96.8-99.4% for 10 times diluted urine, linearity of determination in the range 0.5-100 µg mL-1 (r = 0.998), and 3σ limit of detection (LOD) was 0.05 µg mL-1. The whole procedure comprising raw sample pre-treatment, analyte detection and column reconditioning took 8 min. The proposed SIA-SPE method has been applied for direct determination of amiloride in human urine.

'Monolithic Columns--a New Concept Of Separation In The Sequential Injection Technique', Anal. Chim. Acta, 2003 499(1-2) 205-214

"Monolithic Columns--a New Concept Of Separation In The Sequential Injection Technique"
Anal. Chim. Acta 2003 Volume 499, Issue 1-2 Pages 205-214
Dalibor Satínský, Petr Solich, Petr Chocholous and Rolf Karlícek

Abstract: In this contribution, the coupling of monolithic column with sequential injection technique (SIA), as a new possibility of implementation of a separation step in SIA is described.Monolithic columns were developed based on a new sol-gel technology. Due to the presence of macropores, the monolithic columns possess a much higher porosity than conventional particulate high pressure liquid chromatography (HPLC) columns. Consequently, monoliths can be coupled to the SIA system without loss of performance or limitations due to the very low column back-pressure.The aim of our study was to develop and test the new SI separation manifold and to demonstrate its functionality in the simultaneous determination of four different compounds (methylparaben, propylparaben, sodium diclofenac and internal standard butylparaben) in standard solutions and in a topical emulgel.A Chromolith(R) Flash RP-18e, 25 mm x 4.6 mm (Merck, Germany) column and a FIAlab(R) 3000 system (USA) with an eight-port selection valve and 10 mL syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile:water (40:70 (v/v)) + 0.05% triethylamine, pH 2.5, gradient flow rate 8-20 µl s-1.A novel reversed-phase sequential injection chromatography (SIC) technique with UV spectrophotometric detection was optimized and validated. The validation parameters showed very good results. The analysis time was less than 8 min. The method was found to be applicable for the routine analysis of the active compound sodium diclofenac and preservative propylparaben in a pharmaceutical product, topical diclofenac emulgel 1%.The coupling of the monolithic columns with sequential injection manifold provides an excellent tool to solve the separation problems without using HPLC instrumentation and with low cost per analysis and low consumption of organic solvents (non-continuous flow).

'Using On-line Solid Phase Extraction For Simultaneous Determination Of Ascorbic Acid And Rutin Trihydrate By Sequential Injection Analysis', Anal. Chim. Acta, 2003 497(1-2) 165-174

"Using On-line Solid Phase Extraction For Simultaneous Determination Of Ascorbic Acid And Rutin Trihydrate By Sequential Injection Analysis"
Anal. Chim. Acta 2003 Volume 497, Issue 1-2 Pages 165-174
Z. Legnerová, D. Satínský and P. Solich

Abstract: This presented paper deals with a new methodology for the separation and simultaneous determination of two active substances in combined pharmaceutical formulation, composed of ascorbic acid (AA) and rutin trihydrate (RT). The methodology described is based on the sequential injection analysis (SIA) technique analysis coupled with a solid phase extraction (SPE) microcolumn. The SPE microcolumn was used for retention of RT, while the AA was eluted with the solvent front phase. Due to the different acidobasic and polarity properties of both compounds and the principles of reversed phase chromatography, it was possible to separate AA and RT with one eluting solution methanol/water (28:72), pH 2.5, flow rate 10 µl s-1. The spectrophotometric detection of both substances was performed at 262 nm. Under the optimal conditions, the calibration was linear over the range 10^-100 µg mL-1 for AA with RSD of 0.70% (n=10) and 2-20 µg mL-1 for RT with RSD 0.40% (n=10), and was described by the following equations: A=0.0098 c+(-0.0005); r=0.9995 and A=0.0033 c+0.0080; r=0.9987, for AA and RT, respectively. The sample throughput was 26 h-1. The proposed SIA-SPE method has been applied for the simultaneous assay and dissolution test of AA and RT in pharmaceutical formulation.

'Using On-line Solid Phase Extraction For Flow Injection Spectrophotometric Determination Of Salbutamol', Anal. Chim. Acta, 2002 455(1) 103-109

"Using On-line Solid Phase Extraction For Flow Injection Spectrophotometric Determination Of Salbutamol"
Anal. Chim. Acta 2002 Volume 455, Issue 1 Pages 103-109
Dalibor &Scaron;atínský, Rolf Karlíček and Antonín Svoboda

Abstract: In the proposed procedure, the determination of salbutamol with Folin-Ciocalteau reagent (FC) using a flow injection analysis technique (FIA) with spectrophotometric detection at 750 nm is described. The lab-made FIA system consisted of a peristaltic pump Gilson Minipulse 3 equipped with Tygon tubes, double 6-port external Vici Valco sample injector and S 2000/SAD500 fiber optic spectrophotometer. It was controlled by a PC with use of originally compiled LabVIEW(R)- supported software containing the mathematical library with various statistical functions for off-line data evaluation. Concentration, volume of reagents and flow rate were optimized by a simplex method. The proposed system was used for the direct determination of salbutamol sulfate in the tablets and the human urine without preliminary pre-treatment of the sample. The negative effect of interfering substances (excipients of the tablets and matrix of the urine) is overcome by a solid phase extraction (SPE), when salbutamol is adsorbed on the solid phase in the microcolumn, which is integrated directly into the flow system. Pre-treatment of the sample takes place directly in the flowing stream. The sample throughput without carryover of on-line SPE was 60-80 samples per hour. With the SPE column (Baker-carboxylic acid), salbutamol was determined in the linear range from 1 to 15 µg mL-1 (RSD = 1.2%), with detection limit (3s) 0.1 µg mL-1 and a frequency of 40-60 samples per hour in the water solutions. The salbutamol was determined in the linear range from 2 to 20 µg mL-1 (RSD = 1.7%), with detection limit (3s) 1 µg mL-1 and a frequency of 30 samples per hour in the samples of the human urine.

Solid phase extraction

'On-line Coupling Of Sequential Injection Extraction With Restricted-access Materials For Sample Clean-up And Analysis Of Drugs In Biological Matrix', Analyst, 2003 128(4) 351-356

"On-line Coupling Of Sequential Injection Extraction With Restricted-access Materials For Sample Clean-up And Analysis Of Drugs In Biological Matrix"
Analyst 2003 Volume 128, Issue 4 Pages 351-356
Dalibor atínský, Hana Sklenáová, Jitka Huclová and Rolf Karlíek

Abstract: In this contribution, the on-line coupling of solid phase extraction (SPE), based on a restricted-access material (RAM), with sequential injection technique (SIA) for the analysis of biological samples, is described. The SIA-RAM system was tested with a new potential antileucotrienic drug (VUFB-19363 (Quinlukast)) for serum analysis. The method is based on SPE with the novel internal-surface reversed-phase column packing material - alkyl-diol silica (ADS). The supports tolerate direct and repetitive injection of proteinaceous fluids (plasma, serum) and allow reversed-phase partitioning at the internal surface. A column packed with a 25 ?m C18 alkyl-diol support was used for direct serum injection. Using a 6-port selection valve and the system of three mobile phases, the polar matrix compounds and metabolites are removed by sequentially aspirated mobile phases with lower content of the organic part (methanol-water (2:98) and following acetonitrile-water (20:80)) to the waste, and then, the analyte enriched on the column is eluted by a strong mobile phase (acetonitrile-methanol-water (40:20:40)) to the UV detector without transfer loss. With the fully automated SIA system, a total analysis time of less than 10 min was achieved. The only off-line sample pre-treatment step required to remove particulate matter was centrifugation. The studies showed a range of linearity (2-40 ?g mL-1) and a high recovery (93.6-96.8%) of drug from the biological matrix with coefficients of variation (RSD) less than 5.0% (n = 6). This paper introduces a new, simple and robust analytical technique suitable for screening determination and direct analysis of drugs in biological materials.