Resumo (PT):
In this work an automated multicommutated flow methodology was implemented for the spectrophotometric determination of trimipramine in pharmaceutical preparations by oxidation with ammonium monovanadate in acidic medium. The developed procedure exploits a new approach for sample/reagent intermixing by combining binary sampling with flow-reversal. Rather than inserting the sample as a single continuous volume the intercalation of multiple small sample and reagent aliquots, under a time-based control, created multiple reaction interfaces that promoted reaction zone homogenisation even in limited dispersion conditions. Additionally, the reaction interfaces were reversed, increasing mutual zone penetration, which contributed to a faster reaction development while assuring a low dispersion pattern. A linear range of determination was verified for trimipramine concentrations between 1.0 and 18.0 μg ml−1 with a relative standard deviation (n=10) lower than 1.69% and a sample throughput of about 26 samples per hour. The results were in agreement with those obtained by the reference procedure with relative deviations lower then 2.37%.
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Keywords: Trimipramine; Multicommutated flow system; Reversed flow; Binary sampling; Spectrophotometry
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<a target="_blank" href="http://www.sciencedirect.com/science?_ob=ArticleURL&_udi=B6TGX-496NRVX-2&_user=2460038&_coverDate=12%2F05%2F2003&_rdoc=6&_fmt=high&_orig=browse&_srch=doc-info(%23toc%235266%232003%23999669994%23473113%23FLA%23display%23Volume)&_cdi=5266&_sort=d&_docanchor=&_ct=39&_acct=C000057398&_version=1&_urlVersion=0&_userid=2460038&md5=738eb85bc5c3fc1b52e8c9db33d71141"> Texto integral</a>
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Abstract (EN):
In this work an automated multicommutated flow methodology was implemented for the spectrophotometric determination of trimipramine in pharmaceutical preparations by oxidation with ammonium monovanadate in acidic medium. The developed procedure exploits a new approach for sample/reagent intermixing by combining binary sampling with flow-reversal. Rather than inserting the sample as a single continuous volume the intercalation of multiple small sample and reagent aliquots, under a time-based control, created multiple reaction interfaces that promoted reaction zone homogenisation even in limited dispersion conditions. Additionally, the reaction interfaces were reversed, increasing mutual zone penetration, which contributed to a faster reaction development while assuring a low dispersion pattern. A linear range of determination was verified for trimipramine concentrations between 1.0 and 18.0 mug ml(-1) with a relative standard deviation (n = 10) lower than 1.69% and a sample throughput of about 26 samples per hour. The results were in agreement with those obtained by the reference procedure with relative deviations lower then 2.37%.
Language:
English
Type (Professor's evaluation):
Scientific
No. of pages:
8