Complementary use of flow and sedimentation field-flow fractionation techniques for size characterizing biodegradable poly(lactic acid) nanospheres

Poly(lactic acid) (PLA) nanoparticles were synthesized using a modified evaporation method, testing two different surfactants (sodium cholateand Pluronic F68) for the process. During their formulation the prodrug 5-octanoyl-CPA (Oct-CPA) of the anti-ischemic N6-cyclopentyladenosine(CPA) was encapsulated. Three different purification methods were compared with respect to the influence of surfactant on the size characteristicsof the final nanoparticle product. Flow and sedimentation field-flow fractionation techniques (FlFFF and SdFFF, respectively) were used to sizecharacterize the five poly(lactic acid) particle samples. Two different combinations of carrier solution (mobile phase) were employed in the FlFFFanalyses, while a solution of poly(vinyl alcohol) was used as mobile phase for the SdFFF runs. The separation performances of the two techniqueswere compared and the particle size distributions (PSDs), derived from the fractograms, were interpreted with the support of observations byscanning electron microscopy. Some critical aspects, such as the carrier choice and the channel thickness determination for the FlFFF, have beeninvestigated. This is the first comprehensive comparison of the two FFF techniques for characterizing non-standard particulate materials. The twoFFF techniques proved to be complementary and gave good, congruent and very useful information on the size distributions of the five poly(lacticacid) particle samples.