31Dec 2015

Simultaneous LC determination of two co-prescribed analgesics with anti-hypercholesterolemic agent in bulk drug, dosage formulations and in human serum with programmed UV detection

  • Department of Chemistry, University of Karachi, Karachi-75270.
  • Research Institute of Pharmaceutical Sciences, University of Karachi, Karachi-75270.
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A simple, accurate and sensitive High-Performance Liquid Chromatography-UV detection method was developed for simultaneous determination of rosuvastatin with co-administered NSAIDs (piroxicam and diclofenac) in bulk drug, dosage formulations and human serum. Isocratic separation was employed on pre-packed Purospher STAR® C18 (5 µm, 25 x 0.46 cm) column at ambient temperature. Mobile phase consisted of methanol, water and acetonitrile (80:17.5:2.5 v/v), pH adjusted to 3.0 with o-phosphoric acid at 1 mLmin-1. Drugs in eluent were monitored at isosbestic point of drugs 230 nm for their similar absorptivity and under wavelength-program to provide their maximum absorbance. Linear behavior was observed between 0.33-16.66 ?gmL-1 for rosuvastatin and piroxicam and 0.25-12.5 ?gmL-1 for diclofenac with r2 ? 0.998. %RSD for intra-day and inter-day precision was less than 2 in all bulk, formulations and human serum samples. % recoveries for all drugs were 98.18-101.46% in API, pharmaceutical formulations and in human serum at isosbestic point. Wavelength-programmed analysis made the method more sensitive where 11-38 ngmL-1 LOQs and 3-12 ngmL-1 LODs for bulk, 11-21 ngmL-1 LOQs and 4-7 ngmL-1 LODs for formulations; and 8-14 ngmL-1 LOQs and 3-4 ngmL-1 LODs for samples in human serum shifted to 4-11 ngmL-1 LOQs and 1-3 ngmL-1 LODs for API, 9-13 ngmL-1 LOQs and 3-5 ngmL-1 LODs for pharmaceutical formulations; and 3-14 ngmL-1 LOQs and 1-5 ngmL-1 LODs for samples in human serum recorded at isosbestic point respectively for rosuvastatin, piroxicam and diclofenac. Recovery of drugs was 97.26-102.46% in API, 97.23-102.65% in formulations and 97.68-102.71% in serum samples at %RSD less than 2 for all. Both methods are equally applicable for implementation in industries for QC analyses, forensic, clinical and research work due to the high throughput of methods within 5 minutes with non-toxic and non-corrosive solvents and conventional detector for quantities present in little amounts.


[Arman Tabassum, Muhammad Saeed Arayne and Najma Sultana (2015); Simultaneous LC determination of two co-prescribed analgesics with anti-hypercholesterolemic agent in bulk drug, dosage formulations and in human serum with programmed UV detection Int. J. of Adv. Res. 3 (Dec). 1724-1733] (ISSN 2320-5407). www.journalijar.com


Arman Tabassum