Flow Methods in Pharmaceutical Analysis

Chemiluminometric determination of the pesticide 3-indolyl acetic acid by a flow injection analysis assembly

Abstract A new method is proposed for the chemiluminescent determination of the pesticide 3-indolyl acetic acid by means of an flow injection analysis system. The chemiluminescence emission is obtained by oxidation of the analyte with Ce (IV) in nitric acid and presence of β-cyclodextrine. The continuous-flow method allows the determination of 159 samples h−1 of 3-indolyl acetic acid in an interval of concentrations over the range 0.5–15.0 mg l−1. The limit of detection was 0.1 μg l−1 and the R.S.D. (n, 17) at 2.0 mg l−1 of the pesticide level was 2.7%. The method was applied to water samples.

Determination of the herbicide benfuresate by its photo-induced chemiluminescence using flow multicommutation methodology.

The present paper deals with an analytical strategy based on coupling photo-induced chemiluminescence in a multicommutation continuous-flow methodology for the determination of the herbicide benfuresate. The solenoid valve inserted as small segments of the analyte solution was sequentially alternated with segments of the NaOH solution for adjusting the medium for the photodegradation. Both flow rates (sample and medium) were adjusted to required time for photodegradation, 90 s; and then, the resulting solution was also sequentially inserted as segments alternated with segments of the oxidizing solution system, hexacyanoferrate (III) in alkaline medium. The calibration range from 1 microg L(…

Photo‐Induced Chemiluminometric Determination of Acrolein in a Multicommutation Flow Assembly

Abstract This paper deals with the determination of acrolein based on a strategy provided with a sensitive detection, the chemiluminescence; a “clean chemical” analyte treatment, the on‐line UV‐irradiation; and, a simple and quick automated system, the emergent multicommutation continuous‐flow methodology. The pesticide solution is irradiated (stopped‐flow) for 30 s; then, the resulting solution is introduced to the flow‐cell after being alternated with segments of the stream formed by potassium permanganate in strong acid solution and ethanol segments. The calibration range, from 1 to 1 mg l−1, resulted in a linear behavior over the range 5–100 µg l−1 and fitting the linear equation: I=75.…

Analytical strategy photodegradation/chemiluminescence/continuous-flow multicommutation methodology for the determination of the herbicide Propanil

The present paper is dealing with an analytical strategy based on coupling photodegradation, chemiluminescence and multicommutation continuous-flow methodology for the determination of the pesticide Propanil, a common herbicide. The pesticide solution is inserted as small segments sequentially alternated with segments of the solution for adjusting the suitable medium for the photodegradation. Both flow-rates (sample and medium) are adjusted to required time for photodegradation, 2.0 min; and then, the resulting solution is also sequentially inserted as segments alternated with segments of the oxidizing solutions system, 1.00 x 10(-4) mol 1(-1) potassium permanganate in 2.00 mol 1(-1) sulphu…

Chemiluminometric photo-induced determination of Strychnine in a Multicommutation flow assembly

This paper deals on the determination of Strychnine, a potent and dangerous pesticide and the analytical procedure is based on the photo-induced chemiluminescence of the pesticide by means of the Multicommutation continuous-flow methodology. Small segments of the pesticide solution were sequentially alternated with segments of the solution for adjusting the suitable medium for the photodegradation. The required time of UV irradiation was obtained by stopped-flow during 150 s; then, the resulting solution formed alternated segments with the oxidizing solution containing 5 × 10−3 mol l−1 Ce(IV) in 0.6 mol l−1 nitric acid. The calibration range, from 2 μg l−1 to 50 mg l−1, resulted in a linear…

Theoretical prediction of the native fluorescence of pharmaceuticals

At present, to search fluorescent compounds or to increase the native fluorescence is an active research line specially and not only with analytical purposes. On some analytical areas and from the early times of applications of fluorescence (mid-fifties) the fluorimeter was defined as the suitable detector for determination of pharmaceuticals and subsequently, this detection mode has been widely applied. Therefore, it is mandatory to develop new strategies to discover or to enhance in a simple way the native fluorescence of organic compounds to increase the number of analytes to be determined by direct fluorescence. In the present paper are studied further applications of a new tool suitabl…

Photo-induced chemiluminometric determination of Karbutilate in a continuous-flow Multicommutation assembly

The present paper deals with the chemiluminescent determination of the herbicide Karbutilate on the basis of its previous photodegradation by using a low-pressure Hg lamp as UV source in a continuous-flow multicommutation assembly (a solenoid valves set). The pesticide solution was segmented by a solenoid valve and sequentially alternated with segments of the 0.001 mol l(-1) of NaOH solution, the suitable media for the formation of photo-fragments; then it passes through the photo-reactor and was lead to the flow-cell after being divided in small segments which were sequentially alternated with the oxidizing system; 2 x 10(-5) mol l(-1) of potassium permanganate in 0.2% pyrophosphoric acid.…

Photo-induced fluorescence of magnesium derivatives of tetracycline antibiotics in wastewater samples

Abstract An analytical strategy, for the determination of tetracyclines (TCs), based on a HPLC system coupled with a photo-reactor followed by post-column derivatization was developed. Higher fluorescence emission after coupling the resulting photo-fragments with magnesium ions was observed for the determination of minocycline (MC), epitetracycline (ETC), tetracycline (TC) and doxycycline (DC). The manifold included a HPLC system with a photo-reactor (PTFE tubing helically coiled around a low-pressure mercury lamp), a mixing T-piece and a fluorescence detector. The derivatization reagent was delivered at 0.5 mL min −1 by a pump. After HPLC separation using a gradient system with a mobile ph…