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On-line coupling of sequential injection extraction with restricted-access materials and post-column derivatization for sample clean-up and determination of propranolol in human plasma
D Satinsky, HS Serralheiro, P Solich, AN Araujo, MC Montenegro
Jazyk angličtina Země Nizozemsko
- MeSH
- financování organizované MeSH
- kalibrace MeSH
- koncentrace vodíkových iontů MeSH
- lidé MeSH
- molekulární struktura MeSH
- on-line systémy přístrojové vybavení MeSH
- propranolol chemie krev MeSH
- průtoková injekční analýza metody přístrojové vybavení MeSH
- senzitivita a specificita MeSH
- Check Tag
- lidé MeSH
The presented paper deals with a new methodology for direct determination of propranolol in human plasma. The methodology described is based on sequential injection analysis technique (SIA) coupled with solid phase extraction (SPE) column based on restricted access materials (RAM). Special RAM column containing 30 microm polymeric material-N-vinylacetamide copolymer was integrated into the sequential injection manifold. SIA-RAM system was used for selective retention of propranolol, while the plasma matrix components were eluted with two weak organic solutions to waste. Due to the acid-basic and polarity properties of propranolol molecule and principles of reversed-phase chromatography, it was possible to retain propranolol on the N-vinylacetamide copolymer sorbent (Shodex MSpak PK-2A 30 microm (2 mm x 10 mm)). Centrifuged plasma samples were aspirated into the system and loaded onto the column using acetonitrile-water (5:95, v/v), pH 11.00, adjusted by triethylamine. The analyte was retained on the column while proteins contained in the sample were removed to waste. Interfering endogenous substances complicating detection were washed out by acetonitrile-water (15:85), pH 11.00 in the next step. The extracted analyte was eluted by means of tetrahydrofuran-water (25:75), pH 11.00 to the fluorescence detector (emission filter 385 nm). The whole procedure comprising sample pre-treatment, analyte detection and column reconditioning took about 15 min. The recoveries of propranolol from undiluted plasma were in the range 96.2-97.8% for three concentration levels of analyte. The proposed SIA-RAM method has been applied for direct determination of propranolol in human plasma.
Citace poskytuje Crossref.org
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- $a Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovskeho 1203, Hradec Kralove 500 05, Czech Republic.
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- $a The presented paper deals with a new methodology for direct determination of propranolol in human plasma. The methodology described is based on sequential injection analysis technique (SIA) coupled with solid phase extraction (SPE) column based on restricted access materials (RAM). Special RAM column containing 30 microm polymeric material-N-vinylacetamide copolymer was integrated into the sequential injection manifold. SIA-RAM system was used for selective retention of propranolol, while the plasma matrix components were eluted with two weak organic solutions to waste. Due to the acid-basic and polarity properties of propranolol molecule and principles of reversed-phase chromatography, it was possible to retain propranolol on the N-vinylacetamide copolymer sorbent (Shodex MSpak PK-2A 30 microm (2 mm x 10 mm)). Centrifuged plasma samples were aspirated into the system and loaded onto the column using acetonitrile-water (5:95, v/v), pH 11.00, adjusted by triethylamine. The analyte was retained on the column while proteins contained in the sample were removed to waste. Interfering endogenous substances complicating detection were washed out by acetonitrile-water (15:85), pH 11.00 in the next step. The extracted analyte was eluted by means of tetrahydrofuran-water (25:75), pH 11.00 to the fluorescence detector (emission filter 385 nm). The whole procedure comprising sample pre-treatment, analyte detection and column reconditioning took about 15 min. The recoveries of propranolol from undiluted plasma were in the range 96.2-97.8% for three concentration levels of analyte. The proposed SIA-RAM method has been applied for direct determination of propranolol in human plasma.
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