Analysis of piroxicam in pharmaceutical formulation and human urine by dispersive liquid-liquid microextraction...

Piroxicam, is non-steroidal anti-inflammatory and analgesic agent, which is widely used in the treatment of patients with rheumatologic disorders. A new analytical approach based on the dispersive liquid-liquid microextraction (DLLME) has been developed for the extraction and determination of PX in pharmaceutical preparation and human urine.

From the PX standard solution or solutions prepared from real samples, aliquot volumes were pipetted into centrifuge tubes and mixed with acetate buffer at pH 3.0 and NaCl solution. The contents were subjected to the DLLME, so 700 µL of methanol containing 70 µL of chloroform was injected rapidly into a sample solution. A cloudy solution was rapidly produced and the PX extracted into dispersed fine droplets. The mixture was centrifuged, thus these fine droplets of chloroform were settled. The supernatant aqueous phase was readily decanted, then the remained organic phase was diluted with ethanol and the absorbance measured at 355 ± 3 nm against a reagent blank.

The main factors affecting the extraction efficiency such as pH, extraction and disperser solvent types and etc. were studied and optimized systematically. Under optimized conditions, the calibration graphs were linear over the range of 0.2 to 4.8 µg/mL. The limit of detection and relative standard deviation were found to be 0.058 µg/mL and 2.83%, respectively. Relative recoveries in the spiked samples ranged from 97 to 110%.

Using the developed method PX can be analyzed in pharmaceutical formulation and human urine sample in a simpler, cheaper and more rapid manner.