Influence of the nozzle type on particle size and its consequence for flowability of spray-dried protein powders

J. Schfer1, G. Lee2
1,2 Friedrich-Alexander-University

Erlangen-Nrnberg, Division of Pharmaceutics, Cauerstrae 4 (Haus 6), 91058 Erlangen, Germany; telefon: +49 9131 8529 559; mail: schaefer@pharmtech.uni-erlangen.de

Purpose This work shall investigate the influence of different nozzle types on the particle morphology of spray dried protein powders. The flowability is to be characterized. Materials and methods For the drying experiments a lab-scale spray dryer from Pro-C-ept (Zelzate, Belgium) is used. Its special design is able to produce large droplets in spite of a small sample volume and liquid feed. A two-part spray tower with an overall length of 140 cm was assembled. A standard two-fluid nozzle (cap-orifice diameter 1.2 mm, atomizing air pressure 20.0 kPa) and two ultrasonic nozzles (25 kHz; 60 kHz; Sono-Tek Corp., Milton, USA) were used to generate an atomized spray containing droplets as large and consistent as possible. For the liquid feed a peristaltic pump with 10 compression rolls was used. Catalase from Bovine liver and Trizma hydrochloride were purchased from Sigma-Aldrich, Germany and used as obtained. In order to characterize flowability a vibrating spatula (Gro-Mor Inc., Massachusetts, USA) was applied. The device was connected to an analytical balance (Sartorius LA 120S; accuracy: 0.1 mg) [1]. Results A solution of Catalase (0.1 g/ml) in 0.5M Trizma-buffer was atomized and dried with an inlet temperature of 130C. With the two-fluid nozzle particle sizes range from 1 to 20 m with an irregular gauged particle surface (fig. 1). The 60 kHz ultrasonic nozzle generates particles with a similar size but less fines (fig. 2). Particles dried with the 25 kHz nozzle are larger with sizes ranging from 15 to 60 m. The surface seems a little bit smoother (fig. 3). For flowability measurement the vibrating spatula was loaded with 160.0 mg of each spray dried powder and turned on for 3 minutes. The mass flow was recorded so that it can be expressed as a function of time. Figure 4 shows the difference in flowing behaviour. Mass flow can be observed with both ultrasonic nozzles, whereas the 25 kHz nozzle shows the best result.

figure 1 Catalase, spray dried from a 10% aqueous solution, 2-fluid nozzle (SEM, 500x)

figure 3 Catalase, spray dried from a 10% aqueous solution, ultrasonic nozzle 25 kHz (SEM, 500x)
25 kHz nozzle 60 kHz nozzle two fluid nozzle
160 140 120

weight [mg]

100 80 60 40 20 0 00:00

01:26

02:53

time [mm:ss]

figure 2 Catalase, spray dried from a 10% aqueous solution, ultrasonic nozzle 60 kHz (SEM, 500x)

figure 4 Mass flow of spray-dried powders from a vibrating spatula

Conclusion Atomizing nozzle types have an influence on the size and the morphology of the resulting dried particles. Flowability of the powder differs from each other. Ultrasonic atomization and spray drying could lead to flowable powders. It seems that atomization with the 25 kHz nozzle results in the largest particles and the best flowability.
References: 1. A. Hickey: Flow Properties of Selected Pharmaceutical Powders from a vibrating spatula (1994), Particle & Particle Systems Characterization, 11(6), 457-62, Weinheim