[Rapid detection of alkaloids in Ipecac by direct analysis in real time tandem mass spectrometry (DART-MS/MS)].

OBJECTIVE: To detect alkaloids in Ipecac by direct analysis in real time tandem mass spectrometry (DART-MS) without pre-treatment and chromatographic separation. METHOD: Under the optimum conditions, DART-MS characteristic spectra were collected for tablet of Ipecac powder, Ipecac stems and leaves by full scanning, and secondary spectra were adopted for identifying alkaloids. The multiple reaction monitoring mode was adopted to determine the mass spectrum peak intensity of determinands on the surface of determined samples, in order to calculate their average content in samples. RESULT: Spectra of tablet of Ipecac powder and Ipecac stems showed remarkable ionized ion peaks of emetine and cephaeline at m/z 481 and 467, while spectra of leaves showed ionized ion peaks of other alkaloids at m/z 479 and 465. Furthermore, the quantitative analysis was also demonstrated with good reproducibility and linear relationship. CONCLUSION: The mode can play a role in rapid determination of medicinal materials and prepared herbal medicines and real-time rapid quantitative analysis on intermediates and preparations.

Determination of chlorpheniramine maleate and tincture ipecac in dosage form by liquid chromatography with ultraviolet detection.

A procedure was developed and validated for measuring chlorpheniramine maleate and tincture ipecac (as emetine hydrochloride) by reversed-phase liquid chromatography with methanol-10 mM sodium heptanesulfonate (20 + 30) as the mobile phase; the pH was adjusted to 4 with acetic acid, and the flow rate was at 1.5 mL/min, with ultraviolet detection at 254 nm. Propyl paraben was used as the internal standard. The standard curves were linear (r = 0.998 and 0.9998) for both chlorpheniramine maleate and emetine hydrochloride over the ranges of 5-100 and 0.1-40 microg/mL, respectively. The mean recoveries +/- standard deviation were 101.37 +/- 2.77% for chlorpheniramine maleate and 98.8 +/- 1.47% for emetine hydrochloride. The proposed method was applied to the determination of chlorpheniramine maleate alone in tablet and syrup dosage forms. The method also was applied to the determination of the emetine content of ipecac liquid extract and tincture ipecac; the results were compared with those of the method of the British Pharmacopoeia. The proposed method was applied successfully to the simultaneous determination of chlorpheniramine maleate and tincture ipecac, as emetine hydrochloride, in syrup dosage form. Both drugs and the internal standard were separated from all interfering components in < 5 min. The proposed method is simple, specific, and economical, when compared with other published methods that determine each component alone.

Colorimetric and spectrophotometric determination of total and non-phenolic alkaloids in ipeca and its formulations.

A simple method, requiring no chromatographic separation, is presented for the determination of the total and non-phenolic alkaloids in ipeca and its preparations. The complex formed between the alkaloid and methyl orange at pH 5.0 is extracted with chloroform and treated with 0.1N NaOH. The liberated dye, determined at 460 nm, is a measure of the total alkaloids. The chloroform phase remaining is treated with 0.1N H2SO4, and the acid extract is measured at 283 nm for the non-phenolic alkaloids, calculated as emetine. The proposed method was successfully applied to samples of ipeca powder, ipeca tincture, and 3 British Pharmaceutical Codex mixtures containing ipeca tincture, namely, ipecacuanha mixture, pediatric; ipecacuanha and ammonia mixture, pediatric; and belladonna and ipecacuanha mixture, pediatric. The proposed method compares favorably with the Egyptian Pharmacopoeia, British Pharmacopoeia, and USP methods and has a relative standard deviation of 1.54%. The present procedure is less time-consuming and requires about 45 and 90 min for the assay of ipeca tincture and powder, respectively. Only a small sample (0.2 mL tincture of 1.0 g powder) is required.

Structure and fragmentation mechanisms of some ions in the mass spectrum of ephedrine.

This paper describes the use of gas chromatography mass spectrometry for the confirmation of ephedrine in adulterated powdered ipecac and ipecac fluid extract. Deuteration studies of ephedrine hydrochloride and some related compounds were also performed in an attempt to postulate structures for some of the fragment ions appearing in the spectrum of ephedrine.

Are consumers provided with adequate information on the actions and uses of ipecacuanha syrup?

The results of a study to assess the level of consumer information about the action and uses of Ipecacuanha Syrup (Emetic) Australian Pharmaceutical Formulary (APF) are reported. Of 40 community pharmacies selected at random from the 321 pharmacies in the Perth metropolitan area, four were unable to supply the syrup. Dosage information provided on the labels of branded products was, for the most part, comprehensive and in line with APF recommendations. Syrup samples dispensed under pharmacy labels provided much less detailed dose information and no information on contraindications on the labels. Counselling by pharmacists was mostly adequate, but information provided by pharmacy assistants was much less detailed. The active alkaloid content of about 77% of the samples of ipecacuanha syrup was within +/- 12% of the target concentration; the remainder had only 56%-58% of the required alkaloid concentration, which indicates a need for more stringent quality control.

Absorption of ipecac alkaloids in emergency patients.

Syrup of ipecac contains the nauseant alkaloids emetine and cephaeline. Although thousands of doses are given yearly, no data exist on the absorption of these alkaloids in man. We gave 30 mL of USP Syrup to ten adult patients. Blood and urine samples were obtained at approximately one-half and two hours after administration, and the entire volume of vomitus was saved. The samples were then analyzed for cephaeline and emetine by a high-performance liquid chromatographic (HPLC) assay developed in our laboratory. All patients vomited within 30 minutes, but the amounts of alkaloid regurgitated varied from 22 +/- 14% in six patients to 80 +/- 16% in the remaining four. Only six patients had emetine or cephaeline in their blood by two hours (range, 5 to 73 ng/mL), although ten patients had detectable concentrations of the alkaloids in their urine. Measured over two hours, no patient eliminated more than 0.5% of the dose by the urinary route. In our study ipecac was absorbed by all who received it; the extent of absorption varied widely, and elimination by the renal route was small.