DoE Screening and Optimization of Liquid Chromatographic Determination of Nicotinic Acid and Six Statins: Application to Pharmaceutical Preparations and Counterfeit Detection

Abstract

An isocratic reversed-phase high performance liquid chromatographic method has been developed and validated to simultaneously determine nicotinic acid, pravastatin sodium, rosuvastatin calcium, atorvastatin calcium, pitavastatin calcium, lovastatin sodium and simvastatin sodium in focus on counterfeit drug detection. Thin-layer chromatography, nuclear magnetic resonance and mass spectrometry have been additionally performed to verify the identification of adulterants of counterfeit herbal medicines. Chromatographic separation was carried out on Inertsil® ODS-3 C18 (4.6 × 150 mm, 5 μm) with isocratic mobile phase elution containing a mixture of acetonitrile: methanol: 25 mM potassium dihydrogen phosphate buffer, pH 2.86 adjusted with 0.1 M o-phosphoric acid (48: 30: 22, v/v/v), at a flow rate of 1 mL/min and with UV detection at 238 nm. The design of experiment methodology, Plackett–Burman and Box–Behnken designs, was used to screen and optimize the mobile phase composition. The validation of the method was also carried out under the International Conference on Harmonization guidelines. The developed method was sensitive, accurate, simple, economical and highly robust, in addition to the comprehensiveness and novelty of this method for separating the seven drugs. The results were statistically compared with the reference methods used Student’s t-test and variance ratio F-test at P < 0.05.

Utilizing experimental design and desirability function in optimizing RP-HPLC method for simultaneous determination of some skeletal muscle relaxants and analgesics

“…Many analytical methods, such as colorimetry 24 , IR-spectroscopy 25 , 26 , Raman- spectroscopy 27 , NMR 28 , GC–MS 29 – 31 , TLC 32 – 35 , HPTLC 36 , RP-HPLC 37 – 41 , and LC–MS 42 – 44 , have been reported in the literature for the detection and determination of pharmaceutical and herbal counterfeit items.…”