Resumo (PT):
In this contribution, a new separation method for simultaneous determination of paracetamol, caffeine, acetylsalicylic acid, and internal standard benzoic acid was developed based on a novel reversed-phase sequential injection chromatography (SIC) technique with UV detection. A Chromolith® Flash RP-18e, 25-4.6 mm column (Merck, Germany) and a FIAlab® 3000 system (USA) with an 8-port selection valve and a 5 mL syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-(0.01 M) phosphate buffer (10 : 90, v/v) pH 4.05, flow rate 0.6 mL min-1. UV detection was at 210 and 230 nm. The validation parameters showed good results: linearity (r >0.999) for all compounds, detection limits in the range 0.3-0.8 g mL-1, repeatability (RSD) of peak heights between runs in the range 1.10-4.30% at three concentration levels and intra-day repeatability of the retention times in the range 0.28-0.43%. The analysis time was < 6 min. The method was found to be applicable for the routine analysis of the active compounds paracetamol, caffeine, and acetylsalicylic acid in pharmaceutical tablets.
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Keywords
Sequential injection analysis (SIA) • Sequential injection chromatography (SIC) • Monolithic columns • Paracetamol • Caffeine • Acetylsalicylic acid
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<a target="_blank" href="http://www3.interscience.wiley.com/journal/107642973/abstract"> texto integral</a>
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Abstract (EN):
In this contribution, a new separation method for simultaneous determination of paracetamol, caffeine, acetylsalicylic acid, and internal standard benzoic acid was developed based on a novel reversed-phase sequential injection chromatography (SIC) technique with UV detection. A Chromolith(R) Flash RP-18e, 25-4.6 mm column (Merck, Germany) and a FIAlab(R) 3000 system (USA) with an 8-port selection valve and a 5 mL syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-(0.01 M) phosphate buffer (10: 90, v/v) pH 4.05, flow rate 0.6 mL min(-1). UV detection was at 210 and 230 nm. The validation parameters showed good results: linearity (r>0.999) for all compounds, detection limits in the range 0.3-0.8 mug mL(-1), repeatability (RSD) of peak heights between runs in the range 1.10-4.30% at three concentration levels and intra-day repeatability of the retention times in the range 0.28-0.43%. The analysis time was <6 min. The method was found to be applicable for the routine analysis of the active compounds paracetamol, caffeine, and acetylsalicylic acid in pharmaceutical tablets.
Language:
English
Type (Professor's evaluation):
Scientific
No. of pages:
8