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Needleless Electrospinning of Nanofibers for Pharmaceutical And processes Review A Mini-Review: Needleless Electrospinning of Nanofibers for Pharmaceutical and Biomedical Applications Ioannis Partheniadis 1 , Ioannis Nikolakakis 1 , Ivo Laidmäe 2 and Jyrki Heinämäki 2,* 1 Department of Pharmaceutical Technology, School of Pharmacy, Faculty of Health Sciences, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece; [email protected] (I.P.); [email protected] (I.N.) 2 Institute of Pharmacy, Faculty of Medicine, University of Tartu, 50411 Tartu, Estonia; [email protected] * Correspondence: [email protected]; Tel.: +372-7375281 Received: 30 April 2020; Accepted: 4 June 2020; Published: 6 June 2020 Abstract: Electrospinning (ES) is a convenient and versatile method for the fabrication of nanofibers and has been utilized in many fields including pharmaceutical and biomedical applications. Conventional ES uses a needle spinneret for the generation of nanofibers and is associated with many limitations and drawbacks (i.e., needle clogging, limited production capacity, and low yield). Needleless electrospinning (NLES) has been proposed to overcome these problems. Within the last two decades (2004–2020), many research articles have been published reporting the use of NLES for the fabrication of polymeric nanofibers intended for drug delivery and biomedical tissue engineering applications. The objective of the present mini-review article is to elucidate the potential of NLES for designing such novel nanofibrous drug delivery systems and tissue engineering constructs. This paper also gives an overview of the key NLES approaches, including the most recently introduced NLES method: ultrasound-enhanced electrospinning (USES). The technologies underlying NLES systems and an evaluation of electrospun nanofibers are presented. Even though NLES is a promising approach for the industrial production of nanofibers, it is a multivariate process, and more research work is needed to elucidate its full potential and limitations. Keywords: needleless electrospinning; nanofibers; drug delivery; tissue engineering; ultrasound- enhanced electrospinning; process limitations; alternatives 1. Introduction Nanofiber technology involves the manufacturing and processing of fibers with nanoscale dimensions; the properties of such fibers are greatly dependent on their size (diameter). Nanofibers exhibit unique structural, chemical and mechanical properties such as high specific area, porosity and significant tensile strength and are therefore used in a range of applications [1]. Electrospinning (ES) is the most common method used in the fabrication of nanofibers and has found uses in both scientific research work and industrial applications [2,3]. Although ES is a simple and versatile process, some challenges associated with its low production rate and the utilization of needles as spinnerets have limited its full potential in fabricating nanofibers [3]. In recent years, some progress has been made to increase the production rate of ES by exploiting multi-needle spinnerets [4]. However, multi-needle spinnerets also present challenges and do not resolve the problem of needle clogging [1,3]. For this reason, needleless electrospinning (NLES) systems have been developed to increase nanofiber production rates and overcome the needle-associated challenges of the conventional ES process [5]. The present mini-review article was conducted by using the Scopus® (Elsevier) and the PubMed® (NLM: United States National Library of Medicine) databases. Its aim was to elucidate the Processes 2020, 8, 673; doi:10.3390/pr8060673 www.mdpi.com/journal/processes Processes 2020, 8, x FOR PEER REVIEW 2 of 20 Processes 2020, 8, 673 2 of 20 The present mini-review article was conducted by using the Scopus® (Elsevier) and the PubMed® (NLM: United States National Library of Medicine) databases. Its aim was to elucidate the potential ofpotential NLES in of NLESthe fabrication in the fabrication of nanofibers of nanofibers for pharmaceutical for pharmaceutical and biomedical and biomedical applications. applications. NLES technologiesNLES technologies are reviewed are reviewed in an at intempt an attempt to provide, to provide, for the for first the time, first time, a systematic a systematic overview overview of the of featuresthe features of NLES. of NLES. Novel Novel NLES NLES approaches approaches such such as ultrasound as ultrasound-enhanced-enhanced electrospinning electrospinning (USES) (USES) are alsoare alsodiscussed. discussed. 1.1. Nano Nanofibersfibers A fiber fiber is is a a substrate substrate of of natural natural or or synthetic synthetic origin origin that that is issignificantly significantly longer longer than than it is it wide is wide (a length/diameter(a length/diameter L/D L/ Dratio ratio of of more more than than 1:200 1:200).). Nano Nanofibersfibers are are solid solid-state-state linear linear nanomaterials nanomaterials with with a diameter below 100 nm, though from the aspect of industry and engineering, submicron diameter fiberfiberss are often calledcalled nanofibersnanofibers [[1].1]. Nano Nanofibersfibers are are expected expected to to exhibit significantly significantly improved properties due due to to the the characteristics characteristics associated associated with with their their small small size, size, large large specific specific surface surface area, high area, numberhigh number of tiny of tinyvoid void spaces spaces (fibrous (fibrous mesh), mesh), significant significant mechanical mechanical streng strengthth and and flexibility flexibility in functionalizationfunctionalization.. They They are are used used in in a a range range of of applications, applications, mainly mainly due due to to their their extremely extremely large large surface area to volume ratio. The The high high number number of of small small void void spaces spaces combined combined with with a a void space size distribution in in the the micro/nano micro/nano range a andnd their light weight and and flexibility flexibility also also play play a a key key role role in the rangerange of their applications [6]. [6]. The The a aforementionedforementioned unique characteristics of of nano nanofibersfibers make them suitable candidates forfor pharmaceutical pharmaceutical and and biomedical biomedical applications. applications. They They can can be usedbe used e.g., e.g. in water, in water and andair filtration air filtration systems, systems, membranes membranes and environmental and environmental science asscience well asas for well manufacturing as for manufacturing protective protectiveclothing [7 clothing]. [7]. 1.2. Classification Classification of of Nano Nanofibersfibers FibFibersers are mainly categorized based on their length and in particular their LL/D/D ratio. On this basis, nano nanofibersfibers are categorized as continuous or discontinuous (short) fib fibers,ers, where continuous nanonanofibersfibers have an L/D L/D ratio value above 200 [8]. [8]. Moreover, Moreover, nano nanofibersfibers can be categorized ba basedsed on thethe organization of their collections. A A collection collection of of nano nanofibersfibers is is usually usually referred referred to to as as a a mat mat or or a a mesh. A A mesh mesh of of nano nanofibersfibers can can be be categorized as as either either a a woven or non non-woven-woven mesh based on the arrangement of the fiber fiberss in the mesh. A A woven woven mesh mesh consists consists of of fiber fiberss orientated orientated in patterns of high regularityregularity and a non non-woven-woven mesh is composed of continuous layers of randomly aligned nano nanofibersfibers with a large porepore size,size, usuallyusually comparable comparable to to the the diameter diameter of of the the fibers fiber [s3 ,[3,9].9]. Schematic Schematic illustrations illustrations of ofthe th twoe two types types of of fiber fibe meshr mesh are are presented presented in Figurein Figure1. 1. Void spaces (a) (b) Figure 1. SchematicSchematic illustrations illustrations of of ( (aa)) a a woven and (b) a non-wovennon-woven fiberfiber mesh.mesh. Adapted with permission (CC BY 4.0) from [[3]3].. 1.3. Characterization of Nanofibers The characterisation of nanofibers is considered from three perspectives: (i) physicochemical characterisation, (ii) mechanical properties and (iii) bioactivity and interactions. The physicochemical characterisation of nanofibers involves the evaluation of the fiber size (diameter and diameter distribution) and the structure of the mat (orientation/alignment/arrangement) by scanning electron microscopy (SEM), transmission electron microscopy (TEM), field emission scanning electron Processes 2020, 8, 673 3 of 20 microscopy (FESEM) and atomic force microscopy (AFM) [10]. The crystallinity of the fibers and their surface properties (i.e., wettability) are also part of the physicochemical characterisation and can be examined using X-ray diffraction (XRD) and contact angle measurements, respectively. The mechanical characterisation of nanofibers is usually carried out with instruments such as a texture analyser and an optical tensiometer. The properties of the nanofibers measured as part of their mechanical characterisation include: the tensile strength, elongation at break, toughness, stiffness and Young’s modulus [11]. The mechanical properties of nanofibers are influenced by the polymer type and concentration, process parameters and process conditions. For example, the concentration of the polymer and its molecular weight (Mw) can influence the solution viscosity. The solution viscosity can further affect the diameter of the
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