Evaluation of Monomer Leaching from a Resin Cement Through Dentin.

The aim of the study was to evaluate the elution of Triethylene glycol dimethacrylate (TEGDMA), Urethane dimethacrylate (UDMA), Bisphenol A glycerolate dimethacrylate (BisGMA), and Bisphenol A (BPA), from a dual-cured resin cement through human dentin, under constant positive pulpal pressure. Ten human dentin disks were adjusted into a custom made testing device and transparent glass slabs were luted with Variolink II cement, under a steady pressure. The device was filled with Ringer's solution and a pressure of 14.1 cm H2O was applied. Eluates were retrieved from each one of the ten specimens at 9 time interval. All the samples were analyzed by High Performance Liquid Chromatography (HPLC). TEGDMA was detected from the second and UDMA was detected from the fourth time interval and then. The highest average concentration of TEGDMA and UDMA was detected in the 3 day time interval. Time had a significant effect on their elution. BPA and BisGMA were not detected in any sample of any time interval. The clinical relevance of the present study is that the concentration of the eluted monomers, under the conditions that were chosen, did not reach toxic levels for the pulp.

Solid-phase extraction for purification of alkannin/shikonin samples and isolation of monomeric and dimeric fractions.

Isohexenylnaphthazarins (IHN), commonly known as alkannins and shikonins (A/S), are potent pharmaceutical substances with a wide spectrum of wound healing, antimicrobial, anti-inflammatory, and antitumor activity. Purification of A/S is crucial for their use in pharmaceuticals and for biological experimentation. Dimeric and oligomeric A/S derivatives co-exist with the active monomeric ones in most of the samples produced either by (semi)-synthesis or biotechnologically or isolated from natural products. Oligomeric A/S derivatives have not been studied for biological activity hitherto and a method to isolate them is essential.In the present study, solid-phase extraction (SPE) was applied for purification of commercial samples and isolation of monomeric and oligomeric A/S fractions, testing several stationary phases. Sephadex LH-20 cartridges achieved efficient purification for commercial samples containing both monomeric and dimeric A/S derivatives and also separation and isolation of both pure monomeric and dimeric A/S fractions for biological experiments. A high-performance liquid chromatography-diode array detection method was applied for detection, identification and quantification of monomeric and oligomeric shikonin fractions.

HPLC as a tool in medicinal chemistry for the monitoring of tricyclic antidepressants in biofluids.

HPLC is discussed as an essential tool in medicinal chemistry for the monitoring of tricyclic antidepressants in biofluids, providing clinicians with efficient fast and reliable methods to define individual optimum therapeutic concentrations in treatment of depressions. Additional information on mechanism of action, structure activity relationship and metabolism is provided.

Adsorption of fluoride, chloride, bromide, and bromate ions on a novel ion exchanger.

A novel ion exchanger based on double hydrous oxide (Fe2O3Al2O3xH2O) was obtained by the original sol-gel method from easily available and cheap raw materials and employed for adsorption of F-, Cl-, Br-, and BrO-3 from simultaneous solutions. Adsorbent was characterized by potentiometric titration, zeta-potential, and poremetrical characteristics. A technologically attractive pH effect of F-, Br-, and BrO-3 sorption on the investigated double hydroxide of Fe and Al, which is capable of working in the pH range 3 to 8.5, was observed. Kinetic data on fluoride and bromide sorption fit well the pseudo-second-order model. Isotherms of fluoride, bromide, chlorine, and bromate ion sorption on Fe2O3Al2O3xH2O were obtained at pH 4. The isotherm of F- sorption fit well the Langmuir model; sorption affinity (K=0.52 L/mg) and sorption capacity (90 mg F/g) were high. In the competitive adsorption of bromide and bromate, bromide dominated at equilibrium concentrations of the ions >40 mg/L. The mechanism of fluoride adsorption to the surface of the model cluster of the sorbent synthesized and the geometry of the cluster itself were modeled with the HyperChem7 program using the PM3 method.

The use of a monolithic column to improve the simultaneous determination of four cephalosporin antibiotics in pharmaceuticals and body fluids by HPLC after solid phase extraction--a comparison with a conventional reversed-phase silica-based column.

The use of a monolithic column (Chromolith, SpeedROD RP-18e, by Merck) was studied on the determination of cephalosporin antibiotics. Results were compared with those from a previously developed analytical method using conventional silica-based analytical column. A rapid, accurate and sensitive method has been developed and validated for the quantitative simultaneous determination of four cephalosporins: Cephalexine and Cephadroxil (first generation), Cefaclor (second generation) and Cefotaxim (third generation) in pharmaceuticals as well as in human blood serum and urine. Hydroflumethiazide (HFM) (3,4-dihydro-6(trifluoromethyl)-2H-1,2,4-benzothiadiazine-7-sulfonamide-1,1-dioxide) was used as an internal standard at a concentration of 1.5 ng/microL. A rectilinear relationship was observed up to 5 ng/microL for the four compounds. Analysis time was less than 4 min. The statistical evaluation of the method was examined by means of within-day repeatability (n=8) and day-to-day precision (n=8) and was found to be satisfactory with high accuracy and precision results. The method was applied to the determination of the cephalosporins in commercial pharmaceuticals and in biological fluids: human blood serum after solid phase extraction and urine simply after filtration and dilution. Recovery of analytes in spiked serum samples was in the range from 88.7 to 107.8%, while for urine samples recovery was from 98.0 to 105.6%. By comparing the figures of merit for the monolithic column and the silica-based one, regarding the determination of the four cephalosporins investigated in the present study, the outstanding efficiency of the monolithic column can be noticed.

Rapid and sensitive high-performance liquid chromatographic determination of four cephalosporin antibiotics in pharmaceuticals and body fluids.

A rapid, accurate and sensitive method has been developed and validated for the quantitative simultaneous determination of four cephalosporins, cephalexin and cefadroxil (first-generation), cefaclor (second-generation) and cefataxim (third-generation), in pharmaceuticals as well as in human blood serum and urine. A Spherisorb ODS-2 250 x 4-mm, 5-microm analytical column was used with an eluting system consisting of a mixture of acetate buffer (pH 4.0)-CH(3)OH 78-22% (v/v) at a flow-rate 1.2 ml/min. Detection was performed with a variable wavelength UV-Vis detector at 265 nm resulting in limit of detection of 0.2 ng for cefadroxil and cephalexin, but only 0.1 ng for cefotaxime and cefaclor per 20-microl injection. Hydrochlorothiazide (HCT) (6-chloro-3,4-dihydro-7 sulfanyl-2H-1,2,4-benzothiadiazine-1-1-dioxide) was used as internal standard at a concentration of 2 ng/microl. A rectilinear relationship was observed up to 8, 5, 12 and 35 ng/microl for cefadroxil, cefotaxime, cefaclor, cephalexin, respectively. Analysis time was less than 7 min. The statistical evaluation of the method was examined by means of within-day repeatability (n=8) and day-to-day precision (n=9) and was found to be satisfactory with high accuracy and precision. The method was applied to the determination of the cephalosporins in commercial pharmaceuticals and in biological fluids: human blood serum after solid-phase extraction and urine simply after filtration and dilution. Recovery of analytes in spiked samples was in the range from 76.3 to 112.0%, over the range of 1-8 ng/microl.

Direct determination of four fluoroquinolones, enoxacin, norfloxacin, ofloxacin, and ciprofloxacin, in pharmaceuticals and blood serum by HPLC.

A rapid, accurate and sensitive method has been developed for the quantitative determination of four fluoroquinolone antimicrobial agents, enoxacin, norfloxacin, ofloxacin and ciprofloxacin, with high in-vitro activity against a wide range of Gram-negative and Gram-positive organisms.A Kromasil 100 C(8) 250 mm x 4 mm, 5 microm analytical column was used with an eluting system consisting of a mixture of CH(3)CN-CH(3)OH-citric acid 0.4 mol L(-1) (7:15:78 %, v/v). Detection was performed with a variable wavelength UV-visible detector at 275 nm resulting in limits of detection: 0.02 ng per 20 microL injection for enoxacin and 0.01 ng for ofloxacin, norfloxacin and ciprofloxacin. Hydrochlorothiazide (HCT) was used as internal standard at a concentration of 2 ng microL(-1). A rectilinear relationship was observed up to 2 ng microL(-1) for enoxacin, 12 ng microL(-1) for ofloxacin, 3 ng microL(-1) for norfloxacin, and 5 ng microL(-1) for ciprofloxacin. Separation was achieved within 10 min. The statistical evaluation of the method was examined by performing intra-day (n=8) and inter-day precision assays (n=8) and was found to be satisfactory with high accuracy and precision. The method was applied to the direct determination of the four fluoroquinolones in human blood serum. Sample pretreatment involved only protein precipitation with acetonitrile. Recovery of analytes in spiked samples was 97+/-6% over the range 0.1-0.5 ng microL(-1).

Use of novel solid-phase extraction sorbent materials for high-performance liquid chromatography quantitation of caffeine metabolism products methylxanthines and methyluric acids in samples of biological origin.

An automated reversed-phase high-performance liquid chromatographic (RP-HPLC) method, using a linear gradient elution, is described for the simultaneous analysis of caffeine and metabolites according to their elution order: 7-methyluric acid, 1-methyluric acid, 7-methylxanthine, 3-methylxanthine, 1-methylxanthine, 1,3-dimethyluric acid, theobromine, 1,7-dimethyluric acid, paraxanthine and theophylline. The analytical column, an MZ Kromasil C4, 250 x 4 mm, 5 microm, was operated at ambient temperature with back pressure values of 80-110 kg/cm2. The mobile phase consisted of an acetate buffer (pH 3.5)-methanol (97:3, v/v) changing to 80:20 v/v in 20 min time, delivered at a flow-rate of 1 ml/min. Paracetamol was used as internal standard at a concentration of 6.18 ng/microl. Detection was performed with a variable wavelength UV-visible detector at 275 nm, resulting in detection limits of 0.3 ng per 10-microl injection, while linearity held up to 8 ng/microl for most of analytes, except for paraxanthine and theophylline, for which it was 12 ng/microl and for caffeine for which it was 20 ng/microl. The statistical evaluation of the method was examined performing intra-day (n=6) and inter-day calibration (n=7) and was found to be satisfactory, with high accuracy and precision results. High extraction recoveries from biological matrices: blood serum and urine ranging from 84.6 to 103.0%, were achieved using Nexus SPE cartridges with hydrophilic and lipophilic properties and methanol-acetate buffer (pH 3.5) (50:50, v/v) as eluent, requiring small volumes, 40 microl of blood serum and 100 microl of urine.

A rapid high performance liquid chromatographic (HPLC) assay for the determination of oxytetracycline in commercial pharmaceuticals.

In the present study, a simple, sensitive and rapid reversed-phase high performance liquid chromatographic (HPLC) method with ultraviolet detection for the analysis of oxytetracycline (OTC) is developed and applied to the determination of the antibiotic in commercial pharmaceutical preparations (powder, capsules, vaginal tablets and ointment). The isocratic elution is performed with methanol-0.01 M oxalic acid, pH 3.0 (30:70, v/v) at a flow rate of 0.95 ml min, using a Silasorb C8 analytical column, 250 x 4 mm, 10 microm. Codeine is used as internal standard. Absorbance is monitored at 250 nm where both analyte of interest and internal standard have significant absorption. Total analysis time was approximately 7 min. Data with respect to precision and accuracy and limits of detection are reported and discussed. The described method can be readily utilised for analysis of pharmaceutical products and pharmacokinetic studies as well.