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J Claramunt

Publications and source records attributed to J Claramunt.

5 recordsLinked to original sources
PubMed2004

Development and validation of a fully automated method for the chromatographic determination of content uniformity of drug tablets.

A fully automated method for the content uniformity analysis of LAS 34475 25mg tablets has been developed by using an automated procedure. This automated method has been validated within the requirements of ICH guidelines Q2A-Q2B. Standard and sample solutions are processed by an automated benchtop system. The operations automated include the phases of disintegration of the dosage form, filtration of the resultant homogenate and injection of the clear sample into the chromatographic system. Although a manual method validated according to ICH guidelines already existed for this compound, the benefits of applying appropriate automation should provide continuous operation, increased precision, an affordable electronic audit trail and significantly reduced time consumption as well as reducing the exposure of the analyst to the drug substance. The objective of this work was to adapt the manual method to an automated workstation. Considerable effort went into developing and validating an automated method. The results obtained in the validation of this automated method were equivalent to the manual method in terms of system precision, linearity, accuracy, robustness and sensitivity (limits of detection, LOD and limits of quantification, LOQ), and carry-over.

Automation↗
PubMed2004

Development and validation of a capillary electrophoresis method with ultraviolet detection for the determination of the related substances in a pharmaceutical compound.

A capillary electrophoresis (CE) method was successfully developed to quantify the impurity profile of a new substance of pharmacological interest: LAS 35917. CE method was developed in order to separate the chloromethylated, monomethylated and hydroxylated impurities (molecules with very similar chemical structures) having the three coelution in the reversed-phase LC method initially established. Taking into account the structure of the impurities of LAS 35917, separation by conventional liquid chromatography (LC) methods would be longer and tedious than separation by CE, which is an appropriate and versatile technique giving easier and quicker methods. Among the three potential impurities mentioned of LAS 35917, two are due to the synthesis route of this drug, and the third arises from degradation. These drug-related impurities were separated using a capillary of 56 cm of effective length and 50 microm I.D., a 60 mM tetraborate buffer, at pH 9.2, and a positive voltage of 20 kV. The optimised CE method was preliminary validated with regard to specificity, linearity, limits of detection and quantitation, repeatability and solution stability. The method allows the detection and quantitation of impurities above 0.04 and 0.08% level, respectively. All three related substances were separated, detected and quantified from their parent drug in the analysis of real samples of LAS 35917, stressed or not stressed, with this simple and fast CE method.

Electrophoresis, Capillary↗
PubMed1995

Degradation profile and identification of the major degradation products of dobupride under several conditions by GC/MS and HPLC-particle beam/MS.

The effect of pH, light, temperature and oxygen on the stability of dobupride (1), a novel gastroprokinetic drug, has been studied, storing the sample in the solid state and as a solution in methanol-water. The main forced degradation products have been identified by means of techniques such as GC/MS and HPLC-particle beam/MS, and two major degradation pathways have been characterized. One degradation route involves the loss of chlorine, yielding 4-amino-2-butoxy-N-[1-(1,3-dioxolan-2-ylmethyl)piperid -4-yl]benzamide (4) as the major degradation product. The second pathway results from cleavage of the piperidine-amide bond, producing 4-amino-2-butoxy-5-chlorobenzamide (2) as the major degradation product. Under the studied conditions, except when exposed to direct light in solution, dobupride has been shown to be very stable: after 5 months storage, the benzamide 2 (second pathway) was the only product identified (less than 0.5%). However, when dobupride in solution is exposed to natural or artificial sunlight, degradation is very fast, and after 7 days only 5% of the unchanged product remains. Under these circumstances, the main degradation route is the first one, with compound 4 being the most abundant degradation product, and compound 2 only being detectable in small amounts.

Benzamides↗
PubMed1972

[The cheiroceps].

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Adolescent↗