Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography.

In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch®), or mixtures of H2O2 and H2SO4, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the tubing wall and the stable anchorage of monolith to the wall, respectively. Special emphasis was also put on the reduction of the unwanted effects of shrinking of monolith during polymerization, by using an external proper mold and by selecting the adequate monomers in order to increase the flexibility of the polymer. Poly(glycidyl methacrylate-co-divinylbenzene) monoliths were in situ synthesized by thermal polymerization within the confines of surface-vinylized PTFE tubes. The modified PTFE tubing tightly held the monolith, and the monolithic column exhibited good pressure resistance up to 20 MPa. The column performance was also evaluated via the isocratic separation of a series of alkylbenzenes in the reversed-phase mode. The optimized monolithic columns gave plate heights ranged between 70 and 80 µm. The resulting monoliths were also satisfactorily applied to the separation of proteins.

FI on-line chemiluminescence reaction for determination of MCPA in water samples.

This paper reports an economic, simple, and rapid FI-CL method for the determination of MCPA. This method requires simple instrumentation and it is fast enough to be used in routine analyses. A chemiluminescence signal is generated by reaction between photodegraded MCPA and ferricyanide solution in alkaline medium. All physical and chemical parameters in the flow injection chemiluminescence system were optimized in the experimental setting. To eliminate interference, a solid-phase extraction stage with SDB-1 cartridges and ethanol elution is applied. The signal-MCPA concentration relation is linear in concentration intervals between 0.0015 and 0.6 µg·mL(-1). The calibration lines are statistically similar in different working conditions: standards with ethanol without extraction and standards with ethanol and extraction, allowing standards to be excluded from the extraction step, which simplifies the process. The detection limit (DL) is 0.5 ng·mL(-1), which is the same order as the maximum limit established in legislation regarding pesticide limits in water destined for human consumption. A DL of 0.13 ng·mL(-1) can be reached if a sample of 100 mL is preconcentrated. The interday variance coefficient is 3% and the sample throughput is 90 h(-1). The water analysis method is efficient with relative error percentages lower than 5% with respect to the added concentration.

Flow-injection analysis-spectrophotometric determination of nitrite and nitrate in water samples by reaction with proflavin.

A flow-injection manifold is proposed for determination of nitrite based on the reaction with 3,6-diamino acridine (proflavin sulfate) in hydrochloride acid medium. The assembly is adapted for nitrate determination by including a reductive column filled with copperized cadmium. The influence of foreign substances is also studied. The method gives a linear calibration graph over the range 0.06-4 mg 1(-1) nitrite, with an RSD <0.5%. The method was applied to nitrite and nitrate determinations in either waste water or coastal marine water samples.

FIA-fluorimetric determination of thiamine.

A flow injection-fluorimetric determination of thiamine is reported. The procedure is based on the oxidation of the analyte with potassium hexacyanoferrate(III) immobilized on an anionic exchange resin; the fluorescence is monitored in aqueous basic solution. Concentrations of the vitamin of 0.1-4 ppm have been determined; the relative standard deviation was 1.8%. The injection rate was 28 samples/h. The influence of other substances and the determination of the drug in a pharmaceutical formulation are also reported.