Encapsulation of Liquids Via Extrusion--A Review.

Various encapsulation techniques are known for pharmaceutical applications. Extrusion is of minor importance. However, extrusion is used to obtain granules with encapsulate liquid active ingredients (AI) like essential oils and flavours for food applications since decades. Many of these AIs can be used for agrochemical, home care, and pharmaceutical products, too. Thus, the focus of this review is on the interdisciplinary presentation and evaluation of the available knowledge about the encapsulation process via extrusion. The desired microcapsule structure is discussed at the outset. The microcapsule is compared to the alternative glassy solid solution system, before an overview of suitable excipients is given. In the next section the development of the extrusion technique, used for encapsulation processes, is presented. Thereby, the focus is on encapsulation using twin-screw extruders. Additionally, the influence of the downstream processes on the products is discussed, too. The understanding of the physical processes during extrusion is essential for specifically adjustment of the desired product properties and thus, highlighted in this paper. Unfortunately not all processes, especially the mixing process, are well studied. Suggestions for further studies, to improve process understanding and product quality, are given, too. The last part of this review focuses on the characterization of the obtained granules, especially AI content, encapsulation efficiency, and storage stability. In conclusion, extrusion is a standard technique for flavour encapsulation, but future studies, may lead to more (pharmaceutical) applications and new products.

Encapsulation of orange terpenes investigating a plasticisation extrusion process.

Extrusion is widely used for flavour encapsulation. However, there is a lack of process understanding. This study is aimed at improving the understanding of a counter rotating twin screw extrusion process. Orange terpenes as model flavour, maltodextrin and sucrose as matrix materials, and a water feed rate between 4.0% and 5.7% were applied. Product temperatures < 80 °C and specific mechanical energy inputs <260 Wh/kg resulted. Amorphous and partly crystalline samples were obtained. The loss of crystalline sucrose was linked to a dissolution process of the sugar in the available water amount. Melting of the excipients did not arise, resulting in a plasticisation extrusion process. Maximally 67% of the flavour was retained (corresponding to a 4.1% product flavour load). The flavour loss correlated with insufficient mixing during the process and flavour evaporation after extrusion. Based on these results, recommendations for an improved encapsulation process are given.

Encapsulation of liquids using a counter rotating twin screw extruder.

Until now extrusion is not applied for pharmaceutical encapsulation processes, whereas extrusion is widely used for encapsulation of flavours within food applications. Based on previous mixing studies, a hot melt counter-rotating extrusion process for encapsulation of liquid active pharmaceutical ingredients (APIs) was investigated. The mixing ratio of maltodextrin to sucrose as matrix material was adapted in first extrusion trials. Then the number of die holes was investigated to decrease expansion and agglutination of extrudates to a minimum. At a screw speed of 180 min(-1) the product temperature was decreased below 142 °C, resulting in extrudates of cylindrical shape with a crystalline content of 9-16%. Volatile orange terpenes and the nonvolatile α-tocopherol were chosen as model APIs. Design of experiments were performed to investigate the influences of barrel temperature, powder feed rate, and API content on the API retentions. A maximum of 9.2% α-tocopherol was encapsulated, while the orange terpene encapsulation rate decreased to 6.0% due to evaporation after leaving the die. During 12 weeks of storage re-crystallization of sucrose occurred; however, the encapsulated orange terpene amount remained unchanged.

Mechanistic study of carvacrol processing and stabilization as glassy solid solution and microcapsule.

Essential oils and other liquid active pharmaceutical ingredients (APIs) are frequently microencapsulated to improve shelf life, handling, and for tailoring release. A glassy solid solution (GSS), a single-phase system, where the excipient is plasticized by the API, could be an alternative formulation system. Thus this study focuses on the investigation of two formulation strategies using carvacrol as a model compound, namely a microcapsule (MC) and a glassy solid solution (GSS). Applying the solubility parameter approach, polyvinylpyrrolidone (PVP) was chosen as a suitable matrix material for a GSS system, whereas maltodextrin and sucrose served as excipients for a microcapsule (MC) system. Differential scanning calorimetry (DSC) measurements of the excipients' glass transition temperatures and the melting point of carvacrol verified plasticizing properties of carvacrol on PVP. Batch mixing processes, as preliminary experiments for future extrusion processes, were performed to prepare GSSs and MCs with various amounts of carvacrol, followed by crushing and sieving. Maximally 4.5% carvacrol was encapsulated in the carbohydrate material, whereas up to 16.3% were stabilized as GSS, which is an outstanding amount. However, grinding of the samples led to a loss of up to 30% of carvacrol.