Chromatographia (CHROMATOGRAPHIA)

Publications in this journal

• Article: Stress Degradation Studies of Tebipenem and a Validated Stability-Indicating LC Method.

  Judyta Cielecka-Piontek, Przemysław Zalewski, Bolesław Barszcz, Kornelia Lewandowska, Magdalena Paczkowska
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  ABSTRACT: A inexpensive and rapid isocratic LC method has been developed for the quantitative determination of tebipenem-a new β-lactam antibiotic. Stress degradation studies were performed on tebipenem in acidic (0.2 N hydrochloric acid) and basic (0.02 N sodium hydroxide) solutions, in a solution with oxidizing agent (3 % hydrogen peroxide), and in the solid state, during thermolysis and photolysis. For a chromatographic separation of tebipenem and its degradation products, a C-18 stationary phase and 12 mM ammonium acetate-acetonitrile (96:4 v/v) were used. A quantitative determination of tebipenem was carried out by using a PDA detector at 298 nm, with a flow rate of 1.2 mL min(-1). The linear regression analysis for the calibration plots showed a good linear relationship (r = 0.999) in the concentration range 0.041-0.240 mg mL(-1). The method demonstrated good precision (1.14-1.96 % RSD) and recovery (99.60-101.90 %). The limits of detection and quantitation were 9.69 and 29.36 μg mL(-1), respectively. The analysis of tebipenem reactivity was supported by quantum chemical calculations based on the density functional theory (DFT). The analysis of the electron density of the HOMO and LUMO of tebipenem suggested the possibility of electron transport in the molecule during the degradation of bi-cyclic 4:5 fused penem rings.
  Chromatographia 04/2013; 76(7-8):381-386.
• Article: Determination of Pyrethroid Pesticides in Environmental Waters Based on Magnetic Titanium Dioxide Nanoparticles Extraction Followed by HPLC Analysis

  Chenyu Li, Ligang Chen
  Chromatographia 04/2013;
• Article: Stability-Indicating HPLC Method for the Determination of Cefcapene Pivoxil.

  Przemysław Zalewski, Judyta Cielecka-Piontek, Piotr Garbacki, Anna Jelińska, Marta Karaźniewicz-Łada
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  ABSTRACT: The stability-indicating LC assay method was developed and validated for quantitative determination of cefcapene pivoxil in the presence of degradation products formed during forced degradation studies. An isocratic RP-HPLC method was developed with a Lichrospher RP-18 (250 mm × 4.6 mm, 5 μm) column and the mobile phase composed of 45 volumes of acetonitrile and 55 volumes of mixture composed of citric acid 10 mmol L(-1) and potassium chloride 18 mmol L(-1). The flow rate of the mobile phase was 1 mL min(-1). Detection wavelength was 270 nm and temperature was 30 °C. Cefcapene pivoxil, similar to other cephalosporins, was subjected to stress conditions of degradation in aqueous solutions including hydrolysis, oxidation, and thermal degradation. The method was validated with regard to linearity, accuracy, precision, selectivity, and robustness. The method was applied successfully for the determination of cefcapene pivoxil during kinetic studies in aqueous solutions (pH and thermal degradation) and in solid state (oxidative, thermal, and radiolytic degradation).
  Chromatographia 04/2013; 76(7-8):387-391.
• Article: Chromatographia March 2013 Simultaneous Quantification of Aliskiren, Valsartan and Sitagliptin by LC with Fluorescence Detection: Evidence of Pharmacokinetic Interaction in Rats Vishal Goyani, Rajeshwari Rathod, Ranjeet Prasad Dash, Manish Nivsarkar

  Vishal Goyani, Rajeshwari Rathod, Ranjeet Prasad Dash, Manish Nivsarkar
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  ABSTRACT: Abstract A sensitive, precise and simple LC method for the simultaneous quantification of aliskiren, valsartan and sitagliptin in rat plasma has been developed and validated. The chromatographic separation was achieved on a C18 column (250 mm × 4.6 mm, 5 μm) maintained at room temperature, using isocratic elution with acetonitrile/20 mM ammonium acetate buffer (35:65, v/v), pH adjusted to 4.85 with glacial acetic acid, and detected using a fluorescence detector. Liquid–liquid extraction of the aliskiren, valsartan and sitagliptin from the rat plasma with t-butyl methyl ether resulted in their high recoveries. LC calibration curves based on the extracts from the rat plasma were linear in the range of 25–2,000 ng mL−1 for aliskiren and sitagliptin and 50–4,000 ng mL−1 for valsartan. The limits of quantification were 25 ng mL−1 for aliskiren and sitagliptin and 50 ng mL−1 for valsartan. The precision and accuracy of the method were well within the generally accepted criteria for biomedical analysis. The described method was successfully applied to study the pharmacokinetics of aliskiren, valsartan and sitagliptin following oral administration, individually as well as in combination in Sprague–Dawley rats. The results of the study implied the occurrence of pharmacokinetic interaction upon the co-administration of these three drugs.
  Chromatographia 03/2013; online.
• Article: Effect of electronegativity of donor atoms on RF valued of tris (b-diketonato) complexes of cobalt(III), chromium(III) and ruthenium(III) by thin-layer chromatohraphy on silica gel

  Ž.Lj.Tešić, T.J.Janjić, R.M.Tošić, M.B.Ćelap
  Chromatographia 02/2013; 35:599-602.
• Article: Quantitative Retention-Property Relationships Studies of some Schiff Base Ligands and their Complexes by Reversed Phase Thin Layer Chromatography,

  R.Baošić, A.Radojević, T.Tripković, N.Aburas, Ž.Tešić
  Chromatographia 02/2013; 72(5):545-549.
• Article: Development of On-line Liquid Chromatography-Biochemical Detection for Soluble Epoxide Hydrolase Inhibitors in Mixtures.

  David Falck, Nils Helge Schebb, Setyo Prihatiningtyas, Jiawen Zhang, Ferry Heus, Christophe Morisseau, Jeroen Kool, Bruce D Hammock, Wilfried M A Niessen
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  ABSTRACT: In this study, an end-point-based fluorescence assay for soluble epoxide hydrolase (sEH) was transformed into an on-line continuous-flow format. The on-line biochemical detection system (BCD) was coupled on-line to liquid chromatography (LC) to allow mixture analysis. The on-line BCD was based on a flow system wherein sEH activity was detected by competition of analytes with the substrate hydrolysis. The reaction product was measured by fluorescence detection. In parallel to the BCD data, UV and MS data were obtained through post-column splitting of the LC effluent. The buffer system and reagent concentrations were optimized resulting in a stable on-line BCD with a good assay window and good sensitivity (S/N > 60). The potency of known sEH inhibitors (sEHis) obtained by LC-BCD correlates well with published values. The LC-BCD system was applied to test how oxidative microsomal metabolism affects the potency of three sEHis. After incubation with pig liver microsomes, several metabolites of sEHis were characterized by MS, while their individual potencies were measured by BCD. For all compounds tested, active metabolites were observed. The developed method allows for the first time the detection of sEHis in mixtures providing new opportunities in the development of drug candidates.
  Chromatographia 01/2013; 76(1-2):13-21.
• Article: GC Determination of Famotidine, Ranitidine, Cimetidine, and Metformin in Pharmaceutical Preparations and Serum Using Methylglyoxal as Derivatizing Reagent

  Subhan Ali Majidano, Muhammad Yar Khuhawar
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  ABSTRACT: A capillary gas chromatography (GC) procedure has been developed for the determination of four pharmaceutical preparations (famotidine, ranitidine, cimetidine, and metformin) after precolumn derivatization with methylglyoxal (MGo). GC was carried out using an HP-5 column (30 m 9 0.32 mm id) at an initial column temperature of 90 �C for 2 min, followed by heating rate of 25 �C min-1 up to 265 �C. Nitrogen flow rate was 2.5 mL min-1 with split ratio 10:1. A linear calibration curve was obtained within 50–1,000 ng mL-1 and the limit of detection (LOD) was within 17–25 ng mL-1 . The derivatization, GC elution, and separation were repeatable in terms of retention time and peak height/peak area with relative standard deviation within ±4.6 %. The procedure was applied to the determination of the drugs in pharmaceutical preparations and the sera of volunteers who were given oral doses of the drugs. The results of the analysis agreed with the labeled values of the pharmaceutical preparations and were 147–4,903 ng mL-1 in serum with an RSD within 1.0–4.2 %, after ingestion of a single dose of 40–500 mg of active ingredient in a tablet.
  Chromatographia 01/2013; 75:1311-1317.
• Article: Evaluation of the Chromatographic Performance of Conventional, Polar-Endcapped and Calixarene-Bonded Stationary Phases for the Separation of Water-Soluble Vitamins

  C. Chamseddin, Th. Jira
  Chromatographia 01/2013;
• Article: Linear Solvation Energy Relationships in the Determination of Specificity and Selectivity of Stationary Phases.

  S Studzińska, B Buszewski
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  ABSTRACT: The retention of fifty structurally different compounds has been studied using linear solvation energy relationships. Investigations were performed with the use of six various stationary phases with two mobile phases (50/50 % v/v methanol/water and 50/50 % v/v acetonitrile/water). Packing materials were home-made and functionalized with octadecyl, alkylamide, cholesterol, alkyl-phosphate and phenyl molecules. This is the first attempt to compare all of these stationary phases synthesized on the same silica gel batch. Therefore, all of them may be compared in more complex and believable way, than it was performed earlier in former investigations. The phase properties (based on Abraham model) were used to the classification of stationary phases according to their interaction properties. The hydrophilic system properties s, a, b indicate stronger interactions between solute and mobile phase for most of the columns. Both e and v cause greater retention as a consequence of preferable interactions with stationary phase by electron pairs and cavity formation as well as hydrophobic bonds. However, alkyl-phosphate phase has different retention properties, as it was expressed by positive sign of s coefficient. It may be concluded that most important parameters influencing the retention of compounds are volume and hydrogen bond acceptor basicity. The LSER coefficients showed also the dependency on the type of organic modifier used as a mobile phase component.
  Chromatographia 11/2012; 75(21-22):1235-1246.
• Article: Vortex Counter-Current Chromatography: Performance of a New Preparative Column.

  Yoichiro Ito, Robert Clary, Jacob J Witten, Yun Zeng
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  ABSTRACT: A New preparative column for the vortex counter-current chromatograph was fabricated by making many (966) cylindrical separation units to a high-dendity polyethylene disk and thenthreading them with 6-40 taps. The resulting column had a total capacity of 364 mL. The performance of this vortex column was examined with three different two-phase solvent systems each using a set of suitable test samples: hexane-ethyl acetate-methanol-0.1 M hydrochloric acid (1:1:1:1, v/v) for separation of DNP-amino acids; 1-butanol-acetic acid-water (4:1:5, v/v) for separation of dipeptides; and hexane-acetonitrile-water (20:15:2, v/v) for separation of Sudan dyes. Most of the separations show high partition efficiency of over a thousand theoretical plates, as expected based on the results previously obtained in preliminary separations with a small column. Overall, the results of the present study suggest that further improvement of the partition efficiency can be obtained by the modifying column configuration.
  Chromatographia 10/2012; 75(19-20):1091-1097.
• Article: Determination of Pyridinium Ionic Liquid Cations by Reversed Phase Ion-Pair Chromatography Using Gradient Elution

  Lingmin Meng, Hong Yu, Yuzhen Liu
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  ABSTRACT: Four pyridinium ionic liquid cations (N-ethyl-pyridinium, N-butyl-pyridinium, N-butyl-4-methyl-pyridinium, N-hexyl-pyridinium) were separated and determined by reversed phase ion-pair chromatography with ultraviolet-visible detection. The effects of ion-pair reagent, acetonitrile concentration and column temperature on the retention and separation of the cations were evaluated. Then the four pyridinium cations could be separated at baseline within 13min. The detection limits (S/N=3) were 0.30–0.70mgL−1, and relative standard deviations (n=5) for peak areas were 0.18–0.58%. The method was applied to analyze surface water with recoveries of 99.5–104.0%, which is accurate, reliable and practical. KeywordsIon-pair chromatography–Ionic liquids–Gradient elution–Ultraviolet-visible detection–Pyridinium cations
  Chromatographia 05/2012; 73(3):367-371.
• Article: Simultaneous Quantification of Oroxylin A and Its Metabolite Oroxylin A-7-O-Glucuronide: Application to a Pharmacokinetic Study in Rat

  Wenyuan Liu, Xiaozhen Xu, Feng Feng, Chunyong Wu
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  ABSTRACT: Oroxylin A shows reversal activity on multidrug resistance and has an attractive safety profile. A highly sensitive and specific method based on liquid chromatography coupled with tandem mass spectroscopy was developed and validated for simultaneous determination of oroxylin A and its major metabolite, oroxylin A-7-O-glucuronide in rat plasma. The assay procedure involved precipitation of plasma samples with acetonitrile after adding luteolin as an internal standard. Chromatographic separation was achieved on a C18 column using methanol and 0.5% formic acid as the mobile phase, eluting in a gradient system. Detection was achieved with selected reaction monitoring using the electrospray ionization technique. The method was validated by evaluation of selectivity, linearity, precision, accuracy and limit of quantification. Its applicability was demonstrated through the quantification of oroxylin A and oroxylin A-7-O-glucuronide in plasma after intravenous administration of oroxylin A at a dose of 20mgkg−1 to rats. The developed quantification method can now be used for pharmacokinetic studies after intravenous infusion of oroxylin A injection in rats. KeywordsLiquid chromatography–Tandem mass spectrometry–Pharmacokinetic study–Oroxylin A–Oroxylin A-7-O-glucuronide
  Chromatographia 05/2012; 74(1):75-81.
• Article: LC–MS–MS Quantitative Determination of Gefitinib in Human Serum and Cerebrospinal Fluid

  Xin Zheng, Pei Hu, Jian Liu, Qian Zhao, Mengzhao Wang, Ji Jiang, Wei Zhong
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  ABSTRACT: A specific, sensitive, and rapid method based on high-performance liquid chromatography coupled to tandem mass spectrometry (LC–MS–MS) was developed for determination of gefitinib in human serum and cerebrospinal fluid (CSF). The analyte was detected by tandem mass spectrometry operating in positive electrospray ionization mode with multiple reaction monitoring (MRM). Gefitinib was extracted from serum or CSF samples with ethyl acetate using icotinib as internal standard. The method was validated over the concentration range of 1.00–1,000ngmL−1 in human serum and 0.05–50.0ngmL−1 in CSF. For both matrices, inter- and intraday precision (CV%) were less than 15% and accuracy was within 85–115%. Average extraction recoveries were 78.9 and 61.8% in human serum and CSF, respectively. Linearity, recovery, matrix effects, and stability were validated in the two matrices. The method was successfully used for analysis of clinical samples from lung cancer patients with brain metastases treated with gefitinib in the dosage range of 250–500mgday−1. KeywordsLC–MS–MS–Gefitinib–Human serum–CSF–Brain metastases
  Chromatographia 05/2012; 74(1):41-49.
• Article: 60th Birthday of Professor Boguslaw Buszewski

  Renata Gadzała-Kopciuch
  Chromatographia 05/2012; 74(5):365-366.
• Article: Determination of Trace Chloroanilines in Environmental Water Samples Using Hollow Fiber-Based Liquid Phase Microextraction

  Anna Young, Guida Lai, Brian Hung, Amy Yuen, Yi He
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  ABSTRACT: A liquid phase microextraction method using hollow fiber to support extraction solvent was developed for enrichment of trace level chloroanilines in environmental water samples. Target analytes, 2-chloroaniline, 3-chloroaniline, 2,3-dichloroaniline, 2,4-dichloroaniline, 3,4-dichloroaniline, and 3,5-dichloroaniline were determined using gas chromatography-flame ionization detector after extraction. Experimental conditions that affect extraction efficiency were investigated and optimized. The proposed method showed a wide linear range from lower μgL−1 to 1,000μgL−1, low detection limits (≤5.1μgL−1), and reasonable relative standard deviations (RSDs<13%). Feasibility of the method was evaluated by analyzing river water samples collected from the Hudson River and the East River in New York City. KeywordsHollow fiber-based liquid phase microextraction–Chloroanilines–River water
  Chromatographia 05/2012; 74(1):83-88.
• Article: GC–MS Coupled with Hollow-Fiber Drop-to-Drop Solvent Microextraction for Determination of Antidepressants Drugs in Human Blood Sample

  Kavita Tapadia, Kamlesh Shrivas, Lata Sheo Bachan Upadhyay
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  ABSTRACT: A simple, rapid and sensitive hollow-fiber with drop-to-drop solvent microextraction (HF-DDSME) combined with gas chromatography–mass spectrometry (GC–MS) has been successfully developed for extraction and determination of antidepressants drugs (AD) in blood sample. The parameters that affect the separation and preconcentration of AD from sample solution were investigated. Calibration curve obtained for three AD were in the range of 100–1,000; 150–1,200; and 80–1,200ngmL−1 for amitriptyline, imipramine, and promethazine, respectively, with correlation coefficient (R 2 ) between 0.990 and 0.997. The limit of detection (LOD) obtained for amitriptyline, imipramine and promethazine was 25, 30 and 18ngmL−1, respectively. The developed method has been successfully applied for the determination of AD concentration in blood sample, and the recoveries for the spiked samples were in the range of 92.3–97.6%. The sample preparation procedure is very simple, effective and virtually solvent-free, and indicated to be a good alternative for the traditional liquid–liquid extraction. Finally, the proposed method was successfully applied for the determination of drug concentration of AD in human blood sample. KeywordsGas chromatography–mass spectrometry–Hollow-fiber–Drop-to-drop solvent microextraction–Antidepressants drugs–Blood
  Chromatographia 05/2012; 74(5):437-442.
• Article: Qualitative and Quantitative Analysis of 17 Different Types of Tetra- and Pentacyclic Triterpenic Acids in Boswellia papyrifera by a Semi-Automatic Homomodal 2D HPLC method

  Michael Paul, Gerit Brüning, Joachim Weihrather, Johann Jauch
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  ABSTRACT: A semi-automatic two dimensional high-performance liquid chromatography (HPLC) gradient method with photo diode array detection was developed, capable of separating and quantifying up to 17 different triterpenic acids in the gum resin of the frankincense species Boswellia papyrifera. The here reported quantitation of 14 of the possible 17 compounds contains boswellic, tirucallic and lupeolic acids. All compounds were isolated from B. papyrifera and used as external standards. Quantitation of these compounds was performed after minimizing the matrix by liquid–liquid separation, using alkaline, acidic and organic media to separate the acids from interfering matrix compounds. Therefore, two different extraction procedures were tested, giving two different extraction profiles. Within the first run (1st dimension) 13 compounds could be quantified. Quantitation of β-boswellic acid, which was proved to elute as inhomogeneous peak, was achieved by introduction of a second dimension, leading to a fully validated semi-automatic homomodal 2D chromatography. The method is applicable for determination of compounds occurring in different types of frankincense and their pharmaceutical products. It also can be applied to distinguish between different kinds of frankincense. Moreover, it is the first published method feasible of separating and quantifying five different types of tirucallic acids. KeywordsColumn liquid chromatography–Tirucallic acids–Tetra- and pentacyclic triterpenic acids– Boswellia papyrifera (Del.) Hochst.–Frankincense gum resins
  Chromatographia 05/2012; 74(1):29-40.