Direct mixing of alginate and divalent cations such as Ca 2+ generally produces heterogeneous gels that form almost instantaneously. Therefore, is particularly difficult to measure the rheological properties of this gelation event due to the rapid gelation kinetics. In this study, the gelation of alginate when exposed to a solution of CaCl 2 was measured by using a modified rheometer. This modification involved attaching a petri dish to the lower plate of the rheometer into which, filter paper impregnated with CaCl 2 solution was added. A semipermeable membrane was then placed above the filter paper as a barrier to prevent the filter paper imbibing the gel. Samples of 4%w/w alginate were loaded onto the semi-permeable membrane and measurements were taken using 55mm parallel plate geometry. Measurements of G′ and Gʺ were determined as a function of time to monitor gelation. Once gelation was complete the filter paper was removed and replaced with filter paper impregnated with calcium chelators (EDTA, sodium citrate) to assess the degradation of the gel. The results showed that this technique was suitable for analysing the external gelation of alginate with a sharp increase in G′ in the first three minutes which then plateaued over the remainder of the test. It was also shown that gel stiffness reduced to a greater extent on exposure to EDTA compared with sodium citrate. This method is not only suitable for measuring rapid gelation kinetics on exposure to cross-linkers, but has potential applications in modelling the in situ gelation behaviour in simulated physiological environments. Graphical AbstractHighlights: A novel method for the rheological measurements of the gelation of alginate from an external source of calcium ions Simple modification of a commercial rheometer Can be used to measure the degradation of alginate gel on exposure to calcium chelators Potential model for measurements of in situ gelation
The impact of different physiological fluids on the rheological properties of gellan gum is investigated using a commercially available rheometer with a modified lower plate. The power of this method is demonstrated by measuring in real time, the rapid gelation kinetics, and gel strength of gellan gum exposed to simulated gastric fluid, lacrimal fluid, saliva, and wound fluid (all having a different ionic composition), highlighting potential use in the intelligent design of in situ gelling delivery systems. Changes in rheological behavior are examined in situ, gelation kinetics are modeled, and microstructure analyzed in the different simulated physiological environments.
There is great potential to improve drug delivery through the use of in-situ gelling delivery systems. Here we demonstrate a technique capable of measuring changes in rheology (gelation and/or dissolution) of in-situ gelling delivery systems on contact with physiological fluid, while simultaneously analysing drug release. An ocular in-situ gelling formulation (gellan and timolol maleate) and an in-situ gelling oral liquid (alginate and metronidazole) were used as exemplar formulations. The method allowed profiling of increasing gellan concentration resulting in a reduction of timolol maleate released into simulated lacrimal fluid. When alginate was used as an in-situ gelling oral formulation there was a rapid increase in Gʹ on contact with simulated gastric fluid. When this was changed to simulated intestinal fluid, drug release rate increased rapidly, coinciding with alginate gel dissolution. This work highlights the potential of this technology as a tool in development and optimisation of these increasingly popular delivery systems.
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