HPLC method for identification and quantification of three active substances in a dermatological preparation--Viosept ointment.

The study was aimed at developing a HPLC method to identify and quantify domiphen bromide, tripelennamine hydrochloride and clioquinol in Viosept ointment. The tested substances were successfully separated using Inertsil ODS-3 (250 x 4.6 mm, 5 µm) as a stationary phase and a gradient elution. Detection at 310 nm wavelength was applied for tripelennamine hydrochloride and clioquinol, and at 215 nm wavelength for domiphen bromide. Methods of extraction of the tested substances were developed: domiphen bromide and clioquinol were extracted with acetone from heated solutions, and tripelennamine hydrochloride was extracted in a hexane-water system. Validation procedure confirmed the method to be sufficiently selective, precise and accurate. Correlation coefficients of calibration curves pointed out that they were linear within the examined concentration range.

Determination of antihistamines based on the formation of mixed aggregates with surfactants.

The determination of antihistamines based on the measurement of the critical micelle concentration (c.m.c.) of mixed sodium dodecyl sulfate (SDS)-antihistamine aggregates is proposed. The dye Coomassie Brilliant Blue G (CBBG) was used as a photometric probe for the rapid determination of c.m.c.s. The micellar properties of these drugs permitted the determination of diphenhydramine, antazoline, tripelennamine, diphenylpyraline and clemizole at the micron level with detection limits ranging between 0.1 and 0.7 microns. Hence the proposed method surpassed existing alternative photometric methods used routinely in the quality control of these drugs in sensitivity and featured similar detection limits to fluorimetric methods. The relative standard deviation for 6 micron diphenhydramine was 3.7%. The method was applied to the determination of these drugs in pharmaceutical preparations (solutions, capsules, creams and pills). which were analyzed directly after dissolution of the samples in distilled water.

Construction and evaluation of PVC conventional and tubular tripelennamine-selective electrodes: their application in pharmaceutical preparations.

The construction and evaluation of tripelennamine conventionally-shaped ion-selective electrodes and tubular detectors for the determination of this compound in pharmaceutical formulations are described. Electrodes with conventional configuration have been constructed without an internal reference solution, using several types of immobilized ionic sensors in PVC. The different electrode membranes were prepared by using tripelennamine tetraphenylborate as ionic-exchanger, dissolved in 2-nitrophenyl octyl ether (type A), dibutylphthalate (type B) and bis-(2-ethylhexyl)sebacate (type C) as plasticizer solvents. The general working characteristics of the different types of conventional electrodes were evaluated in tripelennamine solutions, with adjusted ionic strength, showing a linear response in the concentration range of about 4 x 10(-5) - 1 x 10(-1) M and a slope near the theoretical value. The electrodes presented a fast response (> 20 s) and a high reproducibility (> or = 0.2 mV per day). The electrode selectivity in the presence of some interferents, such as sodium, potassium, lithium, ammonium, chlorpheniramine, diphenydramine, promethazine, meclizine and pentazocine, was good, particularly for those whose sensor membrane was prepared with tripelennamine tetraphenylborate dissolved in 2-nitrophenyl octyl ether (type A). Tubular detectors were also prepared using the same sensor membrane and were evaluated in a low-dispersion flow-injection manifold. Under these conditions the detectors presented response characteristics similar to those of the corresponding conventionally-shaped electrodes. The analysis of different pharmaceutical forms (creams, syrups and gels) gave good results with mean recoveries of 99.8-100.6% when the experiments were conducted by direct potentiometry and 99.9-100.4% where the same determinations were conducted by flow-injection analysis with tubular detectors.

Direct analysis of microbial extracts containing metabolites of ethylenediamine-type antihistamines via high-performance liquid chromatography-thermospray mass spectrometry.

The utility of high-performance liquid chromatography-thermospray mass spectrometry (HPLC-TSMS) for the characterization of the ethylenediamine-type antihistamines, pyrilamine, methapyrilene, tripelennamine, and thenyldiamine, and their methylene chloride-extractable microbial metabolites from a biological matrix is demonstrated. Typically, the [M + H]+ ion was detected as the base peak in the TS mass spectra of these compounds. The ethylenediamine-type antihistamine metabolites were detected in an extract of a fungal culture grown in the presence of 5 mg of the antihistamine. A detection limit of 200 ng was observed for the HPLC-TSMS analysis of pyrilamine.

Characterization of the antihistamines tripelennamine, methapyrilene, and thenyldiamine and their N-oxides by thermospray mass spectrometry.

This study describes an investigation of the thermospray (TS) mass spectrometric analysis of tripelennamine, methapyrilene, thenyldiamine, and their N-oxide derivatives. These compounds were analyzed by direct injection TS mass spectrometry in the column bypass mode and with 0.1M ammonium acetate/methanol (80:20, v/v) as the mobile phase. Typically, the parent antihistamines produced only [MH]s ions under these conditions. The N-oxides provided strong [MH]s ions and multiple fragment ions. A scheme to explain the fragmentation patterns is proposed.

Spontaneous live birth with a maternal history of intravenous use of pentazocine and tripelennamine (T's and blues).

A 24-year-old black female presented a live birth of six-months gestation. The 700-g neonate survived for 11 h. After toxicology revealed the presence of pentazocine and tripelennamine (T's and Blues), the mother admitted to using this combination intravenously 9 h previous to admission. Concentrations of pentazocine and tripelennamine were simultaneously determined by gas-liquid chromatography (GLC) combined with nitrogen selective detection. Analyses were performed on a 3% OV-101 column, with the added internal standard, dexbrompheniramine. Both pentazocine and tripelennamine were qualitatively confirmed by their electron impact mass spectra. Concentrations of pentazocine and tripelennamine in various fluids and tissues were determined.

Report of a fatal, acute tripelennamine intoxication.

A death resulting from tripelennamine overdose in a 19-year-old male Caucasian is reported. The patient died 7 h after ingesting approximately twenty 50-mg tripelennamine tablets. A concentration of 1.0 mg/100 ml was found in the blood. All tissue concentrations were measured by ultraviolet spectroscopy and verified by gas-liquid chromatography. Significant findings included pulmonary edema and multiple small petechial hemorrhages in the soft tissue of the scalp.